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Mechanochemistry Meets Biomolecules: Continuous Production of Metal-Organic Framework Biocomposites
(2026)
Mechanochemistry provides a solvent-minimized route to metal–organic framework (MOF) biocomposites, materials that combine the protective and porous features of MOFs with the functionality of biomolecules, and show great promise for drug delivery, biocatalysis, and biosensing. However, their broader application has been limited by batch-type ball-milling synthesis and the associated challenges in reproducibility and upscaling under mild conditions.
In this work,[1] we achieve rapid formation of protein-, carbohydrate-, enzyme-, lipid-, and DNA-containing zeolitic imidazolate framework (ZIF-8) composites using simple hand-mixing reactions,[2] while maintaining high encapsulation efficiencies and retention of enzymatic activity (Figure 1, 1st step). Guided by mechanistic understanding obtained from in situ extrusion studies,[3, 4] this hand-mixing approach is translated to continuous twin-screw extrusion (Figure 1, 2nd step). Using bovine serum albumin (BSA)@ZIF-8 as a model system, we demonstrate stable continuous operation, yielding highly crystalline and porous biocomposites with tunable biomolecule loading, achieving BSA contents of up to 26 wt% and encapsulation efficiencies of up to 96% (Figure 2). The process delivers biocomposites at a production rate of 1.30 kg d⁻¹ with a space-time yield of 2.96 × 10⁴ kg m⁻³ d⁻¹.
The approach is further extended to therapeutic biomolecules, including hyaluronic acid (HA). Shaped HA@ZIF-8 extrudates are produced in a single step directly from reagent powders without external binders. The molecular integrity of encapsulated HA is preserved upon release and during long-term storage (Figure 3). Overall, this study establishes reactive extrusion as a robust mechanochemical approach for the scalable synthesis and shaping of MOF biocomposites for biomedical and biocatalytic applications.
New methods that are suitable for the rapid screening of energetic material (EM) impact sensitivity are needed for the high-throughput discovery of EMs. We here demonstrate a proof-of-concept experimental vibrational spectroscopy (inelastic neutron scattering spectroscopy and low-frequency THz-Raman spectroscopy) study that has promise in this regard. Specifically, we show that a modified version of the vibrational up-pumping model can be applied to experimental vibrational spectroscopy data, to provide a screening tool to rank the impact sensitivities of EMs. We demonstrate the potential of this method on a preliminary set of EMs – CL-20, HMX, FOX-7, NTO, and TATB – with our findings indicating that portable spectroscopic probes could become suitable for the contactless and non-destructive evaluation of miligram quantities of EMs, expediting the design and discovery of new EMs. We expect such analyses could become useful for ensuring novel EMs are safe to handle before performing larger scale sensitivity tests.
Herein, we report the charge storage and plastic properties of the redox-active, bimetallic metal phosphonate framework of [Cu(2,2′-bpy)VO(O3PC6H5)2]. The flexible crystals of [Cu(2,2′-bpy)VO(O3PC6H5)2] combine high energy storage with mechanical flexibility on the same platform, which is an unusual and significant property that is not observed in traditional rigid layered electrode materials. In contrast to RuO2, graphene, or MXenes, which prefer concentrated acidic or basic electrolytes to operate effectively as electrodes, [Cu(2,2′-bpy)VO(O3PC6H5)2] operates between pH values of 4 and 10 while reaching a specific capacitance of about 140 F/g in H3PO4 at pH 4 and in NaOH at pH 10 at 1 mV/s. It also demonstrates high chemical and electrochemical stability between pH 2 and 12 and in lithium hexafluorophosphate for extended periods. The use of [Cu(2,2′-bpy)VO(O3PC6H5)2] as electrodes eliminates the need for harsh chemical environments, generating more sustainable and environmentally friendly energy storage solutions, and [Cu(2,2′-bpy)VO(O3PC6H5)2] can be synthesized in water at mild temperatures. The combination of chemical stability, mechanical flexibility of [Cu(2,2′-bpy)VO(O3PC6H5)2], and compatibility with mild electrolytes makes [Cu(2,2′-bpy)VO(O3PC6H5)2] a more sustainable alternative to conventional metal oxides, MXenes, and carbon-based electrodes in next-generation supercapacitors and battery technologies.
We studied the three-component mechanochemical cycloruthenation of benzo[h]quinoline (1) using the halide-bridged dimer complex [(p-cymene)RuCl2]2 (4) in the presence of NaOAc. Rigorous monitoring of the C–H activation reaction by ex situ powder X-ray diffraction and in situ synchrotron powder X-ray diffraction enabled detection of a crystalline phase during the ball milling reaction between 1 and 4 as well as [(p-cymene)RuCl(OAc)] (5) during the milling of 4 and NaOAc. Notably, complex 5 was also detected as an intermediate in both the one-pot and the sequential reactions of 1, 4 and NaOAc that led to the formation of the cycloruthenated product [(p-cymene)Ru(BHQ)Cl] (7). Our results shed light on the mechanochemical cycloruthenation pathway in the absence of solvent and complement recent findings on mechanochemical cyclometalation with other metals (e.g., Rh and Ir).
Additive manufacturing (AM) has expanded in dentistry, yet the color and translucency stability of 3-dimensional-printed resin-based materials remain insufficiently understood. This study investigated the main and interaction effects of printing orientation, specimen thickness, and surface treatments on the color and translucency stability of a 3-dimensional printed resin–ceramic hybrid material. Ninety AM specimens were fabricated using a factorial design combining 3 printing orientations, 3 specimen thicknesses, and 2 surface treatments (3 × 3 × 2, n = 5 per condition) and compared with 30 subtractively manufactured control specimens (Vita Enamic). Aging was simulated by thermocycling (5000 cycles, 5–55 °C). Color coordinates were measured via the Commission Internationale de l’Éclairage L*a*b* color system, and color change and translucency change were calculated. Degree of conversion, water sorption, and surface roughness were also evaluated. Printing orientation and specimen thickness significantly affected color change and translucency change (P < 0.05), with the 90° orientation showing lower changes than 0° and 45°. Surface treatment had a limited influence on color and translucency stability, although glazing resulted in higher water sorption as compared with polishing (P < 0.05). No significant effects of printing orientation were observed for degree of conversion or surface roughness, whereas surface treatment significantly influenced surface roughness (P < 0.05). Despite these variations, all groups remained within clinically acceptable thresholds for color and translucency changes. Overall, the findings suggest that AM resin–ceramic restorations have potential for use in definitive restorations. Optimizing printing orientation and material thickness may enhance the color and translucency stability of AM resin–ceramic restorations, supporting their clinical applicability.
The newly developed “wire‐print” method is a fast, repeatable and flexible sample preparation procedure aimed at depositing isolated particles or flakes on a substrate for morphological/dimensional analysis, but also for the analysis of the chemical composition. The method was successfully tested on graphene‐related 2D materials (GR2M) and a set of representative reference particles with sizes in nano‐ and micrometer range. Due to their complex morphology and chemistry, the accurate characterization of GR2M is challenging and no standard sample preparation procedure is available. In terms of deposited volume (down to well below 1 nL) and area (down to tens of µm), wire‐print is similar to the piezoelectrical‐driven inkjet printing, but without applying shearing forces to the suspension. It allows for high‐throughput and repeatable deposition of most particulate materials from liquid dispersion as isolated objects onto a substrate. For chemical analysis with Energy‐Dispersive X‐Ray Spectroscopy (EDS) or X‐Ray Photoelectron Spectroscopy (XPS), wire‐printing of µm‐thick and compact spots is also demonstrated. The very short drying times of tiny volumes of suspension imposed by wire‐printing lead to the significant reduction or even disappearance of the typical coffee‐ring effect and thus, to a more homogeneous deposition.
The synthesis and characterisation of ACF-Si-teflate (teflate: pen tafluoroorthotellurate, [OTeF5]−) is reported, which is a solid super Lewis acid generated by incorporating teflate-functionalised silicon containing entities into an aluminium chlorofluoride (ACF) matrix. ATR IR analysis confirmed its super acidic nature, with a blueshift Δν(CN) of 69 cm−1 for ACF-Si-teflate·CD3CN, adduct exceeding that of SbF5·CD3CN. This material catalytically degrades the persistent fluorinated ether bis(difluoromethyl) ether (CF2H)2O into CF3H, with Et3SiH serving as an HF scavenger. More than 95% conversion to generate CF3H was achieved within 24 h. The scavenger is crucial to ensure continuous catalytic activity, preventing HF from blocking the active sites at the catalyst. This hetero geneous catalysis approach provides a strategy for remediating stable fluorinated pollutants
A sustainable mechanochemical process for the generation of sodium aluminium fluorides by conversion of polyvinylidene fluoride (PVDF) waste on using ball milling in the presence of a Lewis acid was developed. The generated fluorides can be key materials for the aluminium production process. The Lewis acid AlCl3 initiates dehydrofluorination steps at PVDF, releasing HF for further fluorination of both NaCl and AlCl3 to yield chiolite under ball milling conditions. Further calcination of chiolite generates cryolite with an overall yield of 62% with respect to AlCl3. The procedure avoids the use of solvents and minimises energy consumption. The identity and phase purity of the products was confirmed by XRD, NMR, IR, and Raman analyses. It was also demonstrated that powdered PVDF, real-life PVDF membrane waste orPVDFextracted from Li-ion batteries can be upcycled into industrially relevant fluoride materials. The presented method offers a sustainable approach for resource recovery and environmental remediation.
Mechanochemistry — the use of mechanical force to drive chemical transformations — is emerging as a powerful, sustainable alternative to conventional, solution-based synthesis.[1,2] By minimising or eliminating the use of solvents, reducing energy consumption and enabling access to novel reaction pathways, mechanochemistry addresses key challenges in green chemistry and the circular economy.[3] This presentation will demonstrate how time-resolved in situ synchrotron X-ray diffraction and Raman spectroscopy have revolutionised our understanding of mechanochemical reactions by enabling us to observe bond-breaking and bond-forming events during milling in real time.
Examples will be presented spanning coordination polymers, metal-organic frameworks, and functional materials for catalysis and environmental remediation.[4] These examples will demonstrate how mechanochemical approaches can enable precise control over the structure and properties of complex solid systems. There will be a particular focus on the mechanochemical deconstruction and valorisation of polymeric materials, including recent advances in converting waste polymers into valuable chemical feedstocks.[5,6] Finally, I will discuss how these mechanochemical strategies can be applied to bio-based and lignocellulosic systems to open new pathways for sustainable materials design in the bioeconomy.[7] By combining fundamental mechanistic insight with practical applications, mechanochemistry provides a flexible toolkit for converting abundant, renewable resources into the next generation of functional materials.
