Aerogel Catalysts Research Articles

Atomically dispersed nickel in CeO2 aerogel catalysts completely suppresses methanation in the water-gas shift reaction.

Nickel-based catalysts are widely studied for water-gas shift (WGS), a key intermediate step in hydrogen production from carbon-based feedstocks. Their viability under practical conditions is limited at high temperatures when Ni aggregates and converts CO to methane, an undesirable side product. Because experimental and computational studies identify undercoordinated Ni step sites as most active toward CH4 formation, we eliminate Ni step sites by atomically dispersing Ni into networked, nanoparticulate CeO2 aerogels. The mesoporous catalyst with 2.5 atomic % Ni in CeO2 is highly active for WGS, converting near-equilibrium levels of CO at 350°C, while no CH4 is detected at the limit of detection (<2 parts per million). In contrast, supporting low weight percentages of Ni clusters or nanoparticles on CeO2 aerogels leads to methanation. The CH4 yield produced by the atomically dispersed Ni-substituted CeO2 aerogel is over an order of magnitude lower than previously reported Ni-based catalysts claiming methane suppression, marking an important advance in the development of WGS catalysts.

Preparation of sulfonated lignin-based carbon aerogel catalyst for biodiesel production from waste vegetable oil

ABSTRACT Using effective green heterogeneous catalysts to produce biodiesel from inexpensive non-food oils is vital for reducing reliance on fossil fuels, meeting increasing global energy demands, and supporting carbon neutrality. This study explores the use of a sulfonated lignin-based carbon aerogel catalyst for biodiesel production from waste vegetable oil (WVO). The catalyst, prepared via a sol–gel method followed by carbonization and sulfonation exhibited a specific surface area of 78.16 m2/g and a -SO₃H group density of 2.81 ± 0.14 mmol/g, which served as the primary active sites. Under optimal conditions; 10 wt% catalyst loading, a 45:1 methanol-to-WVO molar ratio, 65°C reaction temperature, and 5-hr reaction time, the catalyst achieved a maximum biodiesel conversion of 93.3% and a biodiesel yield of 88.51%. However, a decline in performance was observed over repeated cycles, with conversion dropping to 51.68% by the fourth cycle, attributed to the leaching of -SO₃H groups and a reduction in surface area to 44.13 m2/g. The decrease in the sulfonic group density from 2.81 ± 0.14 to 1.03 ± 0.11 mmol SO₃H g− 1 indicated a loss of active sites, highlighting the need to improve the active sites’ stability and the catalyst’s structural integrity. The produced biodiesel met ASTM D6751 and EN 14,214 standards, demonstrating the catalyst’s effectiveness for sustainable biodiesel production.

Aerogels for sustainable CO2 electroreduction to value-added chemicals

Carbon dioxide electrochemical reduction (CO2ER) affords an appealing pathway for transforming discarded CO2 to fuels and economic chemicals. Various nanocatalysts have been used for CO2ER, of which porous catalysts have attracted widespread attentions because of their large electrochemically active surface area, large number of pores for molecule transportation, and high local pH. Aerogels (including carbon-based aerogels and metallic aerogels), as a new class of porous catalysts, have been applied to CO2ER in recent years because of their high electrical conductivity (to reduce overpotential), three-dimensional porous structure and intrinsic hydrophobicity (to inhibit parasitic hydrogen evolution reaction, HER). In this article, we reviewed latest progresses toward aerogels for CO2ER, including (1) synthesis strategies of carbon-based aerogels and metallic aerogels; (2) innovations in aerogels design, such as heteroatom doping and metal incorporation in carbon-based aerogel, creating grain boundaries, regulating Cu0–Cu+ interfaces, and optimizing synergistic effect in metal aerogels; and (3) structural properties of aerogel catalysts to enhance CO2ER performance. Finally, we discuss the challenges, possible solutions and future directions for further development of aerogels in CO2ER.

Nano-Pd/SiO2 aerogel catalyst prepared via ambient pressure drying process using perlite powder in hydrogenation and cross-coupling reactions

Perlite, a cheap silica source with abundant reserves in countries such as Türkiye, China, and Greece, was used to produce nano Pd-doped silica aerogel powder for the first time in this study. The microstructure and morphology of the prepared silica aerogel powder were examined using SEM, FE-SEM, and TEM. The phases of the silica aerogel powders were analyzed via XRD (X-ray Diffraction) technique. The chemical bonding of the surface modifier with aerogels was analyzed by Fourier transform infrared spectroscopy (FTIR, Spectrum RX-1, Perkin Elmer). Surface areas, pore volumes, distributions, and particle sizes of the alumina-silica-based aerogel powders with a porous structure were measured using a Micromeritics/ASAP 2020 brand BET (Brunauer, Emmet, and Teller) device in a liquid nitrogen gas environment at 77K.The efficiency of this nano Pd-doped silica aerogel powder was investigated as a heterogeneous catalyst for well-known transformations in organic synthesis, such as alkene hydrogenation and cross-linking reactions. The results indicated that the developed method is chemoselective, reducing only carbon-carbon multiple bonds without affecting C-N or C-O multiple bonds, such as carbonyl and nitrile. The effectiveness of the newly developed catalyst was also investigated in Heck and Suzuki-Miyaura reactions, yielding the targeted products with high efficiency.Thus, an inexpensive, economical, and environmentally friendly method has been developed that is potentially applicable in the hydrogenation and cross-coupling reactions of alkenes.

Enhancement strategies for NH3-SCR performance of MnCeOx nanowire aerogel catalyst: Synergistic modulation of phosphotungstic acid and structure

Improving the low-temperature SO2 and H2O resistance and N2 selectivity of manganese oxide（MnOx） catalysts is a major challenge in achieving industrial applications. This issue can be effectively addressed by using phosphotungstic acid (HPW) modified MnCeOx-N aerogel catalysts. The HPW-MnCeOx-N catalysts demonstrated excellent NOx conversion (∼100 % at 150–400 °C) and N2 selectivity (>90 % at 50–400 °C). Notably, even under challenging conditions such as 250 ppm SO2 at 250 °C, the catalytic activity of HPW-MnCeOx-N remained largely intact. The NOx conversion was still able to be maintained at 95 % even under the influence of 10 vol% H2O. This represents a significant improvement of 14 % and 5 % compared to the unmodified MnOx-N and MnCeOx-N catalysts, respectively. The integration of HPW within the lattice structure of the HPW-MnCeOx-N catalyst results in an increased number of oxygen vacancies and stronger surface acidity. The interaction between HPW and CeO2 promotes the formation of Ce4+-O-W species, which in turn modifies the redox properties of the MnCeOx-N catalyst. This modification leads to a suppression of NH species formation, thereby improving the selectivity towards N2 production. Physicochemical analyses have shown that the presence of HPW alters the reaction pathway of the MnCeOx-N catalyst, increasing the adsorption of NH3 species and significantly enhancing the generation of bidentate nitrate species, thereby facilitating the reaction through the L-H mechanism. On the HPW-MnCeOx-N catalyst, SO2 mainly inhibits the generation of monodentate nitrate and bridged nitrate species, while having little effect on the major active bidentate nitrates.

Exploring the performance of ammonia microfluidic fuel cell using PdNiCo aerogel

In this manuscript, PdNiCo and NiCo aerogel catalysts are prepared by an ultrafast sol-gel method combining microwave heating and freeze-drying. These new aerogels are synthesized to explore the transition metal content compared to a Pd aerogel in order to minimize the dependence on noble metals and improve their electrocatalytic properties in the presence of ammonia. The textural properties of the aerogels were characterized by the N2 adsorption/desorption isotherms. The crystal structures were measured by X-ray diffraction and X-ray photoelectron spectroscopy was used to analyze the electronic structures of the elements. The electrocatalytic activity of the aerogels towards the ammonia oxidation reaction was tested by cyclic voltammetry in a 1 M KOH + 1 M NH4OH solution. The combination of these properties in the PdNiCo and NiCo aerogels enhances the electrocatalytic activity of ammonium electro-oxidation compared to that of the Pd aerogel alone, and the multimetallic aerogels are more stable when used in a microfluidic device such as an ammonia fuel cell.

Operando X-Ray Scattering for Electrocatalysis and Beyond

The energy transition stands as one of the greatest challenges of today’s society. In this context, electrocatalyst materials at the heart of electrochemical energy conversion devices such as fuel cells and water electrolyzers are expected to play an increasing crucial role in the near future. The urgent bottleneck to be overcome in electrocatalyst materials development to allow the widespread deployment of electrochemical systems is thus reaching combined high activity and long-term stability at low cost. Despite the diversity in electrocatalyst materials, the latter being largely imposed by the various types of electrochemical systems (noble vs. non-noble metals in acidic vs. alkaline media for example) and the prerequisites of the different electrochemical processes (oxidation or reduction reactions of various species at different electrode potential ranges), most activity and stability properties of electrocatalysts directly derive from their (surface) chemistry and structure [1]. Such properties (and their temporal evolution) can thus be directly investigated by means of in situ or operando high energy X-ray scattering (XRD) technique [2].In this presentation, the versatility of in situ and operando XRD technique in addressing key bottlenecks in electrocatalyst materials development, notably by probing adsorption and oxidation trends [3], will be showcased. After an overview of previous contributions from the literature, the talk will focus on our ongoing works which encompass the study of Pt-based nanocatalysts for the oxygen reduction reaction (ORR) at proton-exchange membrane fuel cells (PEMFCs) anode, carbon-capped Ni@C catalyst for the hydrogen oxidation reaction (HOR) at anion-exchange membrane fuel cells (AEMFCs) anode and IrCu unsupported aerogel catalyst for the oxygen evolution reaction (OER) at proton-exchange membrane water electrolyzers (PEMWEs) anode.Finally, the ability of operando XRD to provide device-relevant insights at the macroscale (such as ionomer hydration in PEMFCs or water distribution in AEMFCs) beyond electrocatalysts microstructural properties will be presented.

Construction of a gelatin aerogel catalyst functionalized with LaCoO3 and g-C3N5 for efficient ciprofloxacin degradation via adsorption and peroxymonosulfate activation

Three-dimensional porous gelatin-based aerogels functionalized with LaCoO3 and nitrogen-rich graphitic carbon nitride (g-C3N5) were successfully fabricated via a freeze-drying approach. Herein, the gelatin-based aerogels served as excellent adsorbents and catalysts activating peroxymonosulfate (PMS) to efficiently degrade ciprofloxacin (CIP) from aqueous solutions. In comparison to the pristine gelatin aerogel (GA), the optimized functionalized aerogel (GA–LCCN-1.5) demonstrated a 17.0% superior CIP adsorption performance. Remarkably, GA–LCCN-1.5 exhibited 95.7% removal efficiency for CIP, attributed to the effective generation of •OH, SO4•−, and 1O2 via PMS activation. In addition, high degradation efficiencies over 84.1% were maintained throughout a broad pH range of 3–9. Notably, GA–LCCN-1.5 demonstrated outstanding stability and reusability, with 93.2% CIP removal efficiency even after five reuse cycles indicating significant promise in real applications. Radical quenching and electron spin resonance (ESR) analysis suggest that CIP degradation was dominated by radical and non-radical routes through GA–LCCN-1.5 catalyzed PMS decomposition. Besides, the plausible CIP degradation mechanisms were systemically analyzed and proposed. The toxicities of CIP and the intermediate by-products were evaluated and reported. The findings of this study and insights demonstrate a facile construction of a biopolymer-based aerogel catalyst for synergistic and efficient PMS activation for the removal of antibiotics in water.

Interfacial effects in Ni(OH)2/MnO@Ni aerogel heterostructures promote highly efficient electrooxidation of ethylene glycol to formate and hydrogen

The sluggish oxygen evolution reaction (OER: 4OH− → O2 + 2H2O + 4e−, E = 1.23 V vs RHE) retards the large-scale hydrogen production. Replacing OER with low-potential ethylene glycol oxidation reaction (EGOR) to drive water splitting is a promising approach to solve the high energy consumption in hydrogen production. Herein, we report an energy-efficient electrocatalytic water splitting system by using a heterostructure Ni(OH)2/MnO aerogel catalyst (NiMn AG) that replaces OER with ethylene glycol oxidation reaction (EGOR), resulting in the co-production of value-added formate and green hydrogen. Owing to the optimized electron distribution on the heterostructure interface, the NiMn AG catalyst exhibits excellent EGOR catalytic performance, with an overpotential of only 290 mV at 100 mA cm−2. The open-circuit potential of the reaction is reduced to 0.86 V for EGOR, rendering an earlier occurrence of electron transfer. The ion chromatography (IC) result demonstrates a highly selectivity (96%) for formate in EGOR. The density functional theory (DFT) calculations show that the interfacial effects between Ni(OH)2 and MnO optimizes the surface energy states of NiMn AG, improving the adsorption efficiency of the reaction intermediates for EGOR and further promoting the efficient cleavage of C–C to form formate. Additionally, the incorporation of MnO stabilizes the overall energy state during violent bond-breaking processes. This work sheds light on a new methodology to design bimetallic catalysts assisted by EGOR for decoupled green hydrogen production.

Nickel-doped magnetic carbon aerogel derived from xanthan gum: a competent catalyst for the degradation of single and binary dye-based water pollutants.

Toxic organic dyes (colorants) are one of the main causes of water pollution that releases destructive effluents in the environment. To overcome this issue, a fundamental need to produce a novel, efficient catalyst for the degradation and mineralization of dye mixtures has arisen. The objective of this research is to develop an eminent Ni-doped magnetic carbon aerogel (Ni-MCA) catalyst using graft co-polymerization method having xanthan gum as backbone doped with Ni-magnetic nanoparticles (Ni-MNPs), that do not show agglomeration and easy to separate. The examination revealed that Ni-MCA provided exceptional magnetic characteristics (Ms = 52.75emu/g) and potent catalytic activity for the degradation of mono- as well as binary-dye solutions of Congo red (CR) and methyl green (MG) dyes. The formation was verified by various characterization techniques such as FTIR, VSM, XRD, XPS, SEM, TEM, and EDX mapping. Interestingly, Ni-MCA shows faster result on anionic dye CR up to 97% with degradation rate of 5.647 × 10-1min-1, and MG dye shows degradation of 95.7% with the degradation rate of 2.169 × 10-1min-1, while dye mixture is showing 90% degradation with rate of 2.159 × 10-1min-1.

Anchored silver-palladium aerogel on carbon cloth via diazonium chemistry for electrochemical reduction of CO2

Electrochemical CO2 reduction reaction (eCO2RR) is a promising route for removal of CO2 from the atmosphere and transforming it into value-added products. The development of new and efficient catalysts plays a vital role in this regard. Here a combination of carbon grafting and bimetallic metal aerogel is presented as a catalyst for eCO2RR. The grafted surface plays an essential function in assembling the catalyst on the carbon cloth (CC) surface as a supported catalyst. Herein, we describe the use of para-aminothiophenol (p-TP) as a grafting agent combined with diazonium chemistry to fix a metallic aerogel catalyst on CC as support. The silver, palladium and bi-metallic silver-palladium aerogels (Ag-p-TP, Pd-p-TP, and AgPd-p-TP) anchored onto the surface of CC yielding the corresponding surface-bound materials were used for testing the electrochemical reduction of CO2. The mono-metallic Ag carbon cloth (Ag-p-TP/CC) exhibited the ability in reducing CO2 to CO with moderate Faradaic efficiency (FE) of 74 % in 0.1 M, NaHCO3 electrolyte at pH = 7.5. The bimetallic AgPd-p-TP-CC further enhanced the Faradaic efficiency for CO formation to 88.7 %, with an unexpectedly low onset potential of −0.09 V vs. RHE. Surprisingly, formate was identified to be the liquid product when Pd-p-TP-CC and AgPd-p-TP-CC were used, with maximal FEformate of 19.0 % and 25.7 % at −1.0 V vs. RHE, respectively. In contrast, CC lacking the chemical grafting that allows immobilization of the metal aerogel (Ag-Pd/CC) exhibits lower FEco% for eCO2RR, highlighting the importance of this chemical modification of the carbon cloth surface. Diazonium chemistry coupled with metal aerogels is a new approach to generating surface-bound catalysts for the effective reduction of CO2.

Microwave assisted biomass derived carbon aerogel for highly efficient oxytetracycline hydrochloride degradation: Singlet oxygen mechanism and C vacancies accelerated electron transfer

With plant biomass α-cellulose and sodium lignosulfonate as starting materials, biochar aerogel catalysts were prepared with facile microwave assisted pyrolysis in 5 min; and the as-prepared biochars were utilized for efficient peroxymonosulfate (PMS) activation and oxytetracycline hydrochloride (OTC) degradation under transition metal free conditions. It was found that microwave treatment and sodium lignosulfonate were beneficial for thiophene S introduction, C = O groups and C vacancies enrichment, as well as specific surface area increase. The optimal α-cellulose and sodium lignosulfonate derived metal free biochar aerogel catalyst C3S2 displayed excellent ability to promote PMS activation for 99.9 % OTC degradation during 15 min with rate constant up to 0.818 min−1. Through correlation analysis, quenching tests as well as EPR characterization, C = O groups and thiophene S were considered as main sites for PMS activation to produce nonradicals singlet oxygen (1O2) in OTC degradation. Meanwhile, C vacancies enrichment further improved the pollutants degradation by means of electron transfer acceleration. This research demonstrated new insight in metal-free biochar catalyst design for highly efficient contaminants degradation with 1O2 pathway.

Effect of ceria–silica-based synthesized catalyst in a CI engine exhaust system operating with plastic oil blend

This study investigates the impact of ceria–silica (Ce–Si)-based catalyst integrated in the catalytic converter (CC) on the compression ignition (CI) engine's exhaust manifold. The synthesis catalyst, Ce–Si was developed with the solvothermal method and aged for 4 h at 55°C. Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscope, thermogravimetric analysis, energy dispersive X-ray spectroscopy and transmission electron microscopy analyses were carried out to conclude the synthesis of the catalyst. The catalyst performance of the CC was tested for the emission behavior of nitrogen oxides (NOx), carbon monoxide (CO), hydrocarbon (HC) and smoke. A custom-built CC was installed on the test engine's exhaust manifold. The synthesis catalyst was installed in the engine exhaust route of the stationary single-cylinder diesel engine to conduct the study. To determine the effect of the synthesis catalyst on the exhaust manifold to test both diesel and DPB (B50) fuel with and without CC. Under maximum load conditions, the presence of CC reduced oxide of nitrogen and carbon monoxide emissions by 23% and 17%, respectively, compared to diesel. The synthesized aerogel catalyst has a low density and a high surface area relative to its volume. Ce–Si aerogel catalyst can be used to improve the conversion efficiency of nitric oxide (NO), unburned hydrocarbon and CO in the three-way CC.

A Hierarchical Metal-Organic Framework Composite Aerogel Catalyst Containing Integrated Acid, Base, and Metal Sites for the One-Pot Catalytic Synthesis of Cyclic Carbonates.

Catalysis has played a decisive role in the development of unique chemical reactions to produce important chemicals. However, conventional stepwise synthetic routes that rely on individual catalysts to promote each step often suffer from ponderous processes for the isolation of intermediates that result in massive material losses and large economic expenditures. In addition, traditional powder forms of these catalysts suffer from poor processability and recoverability. Herein, we designed and prepared a hierarchical metal-organic framework (MOF) composite monolithic catalyst IL-Au@UiO-66-NH2/CMC that contains integrated acid (Zr4+), base (ionic liquid (IL)), and metal sites (Au nanoparticles (NPs)) to promote the one-pot preparation of cyclic carbonates from styrene derivatives and CO2. Highly dispersed Au NPs, IL 1-aminoethyl-3-methylimidazolium bromide ([C2NH2 MIM] [Br]), and MOF-positioned Lewis acid sites within this composite aerogel are separately responsible for catalyzing selective epoxidation of the styrene derivatives and the subsequent cycloaddition reaction of CO2 with intermediate styrene oxides. Importantly, inclusion of the imidazolium-based IL effectively modulates the size and chemical microenvironment of the Au NPs via electrostatic protection, leading to catalyst stability and its selective oxidation of styrene. Benefiting from the rapid mass transfer and high exposure of active sites within the pore-rich hierarchical nanostructure, IL-Au@UiO-66-NH2/CMC promotes high conversion (90.5%) of the styrene and selectivity (80.5%) for styrene carbonate (SC) formation in the one-pot process, a performance level that far exceeds those of related catalysts containing only Au NPs or IL (the selectivity of SC < 42%). Furthermore, the composite aerogel catalyst can be readily separated and recycled at least five times without a remarkable loss of activity and selectivity. The controllable integration of various active components in the hierarchical MOF composite aerogel herein should serve as the foundation for the design of multifunctional monolithic catalysts for other valuable tandem processes.

Hierarchically porous cellulose-based carbon aerogels with N-doped skeletons and encapsulated iron-based catalysts for efficient tetracycline catalytic degradation

Three-dimensional interpenetrating and hierarchically porous carbon material is an efficient catalyst support in water remediation and it is still a daunting challenge to establish the relationship between hierarchically porous structure and catalytic degradation performance. Herein, a highly porous silica (SiO2)/cellulose-based carbon aerogel with iron-based catalyst (FexOy) was fabricated by in-situ synthesis, freeze-drying and pyrolysis, where the addition of SiO2 induced the hierarchically porous morphology and three-dimensional interpenetrating sheet-like network with nitrogen doping. The destruction of cellulose crystalline structure by SiO2 and the iron-catalyzed breakdown of glycosidic bonds synergistically facilitated the formation of electron-rich graphite-like carbon skeleton. The unique microstructure is confirmed to be favorable for the diffusion of reactants and electron transport during catalytic process, thus boosting the catalytic degradation performance of carbon aerogels. As a result, the catalytic degradation efficiency of tetracycline under light irradiation by adding only 5 mg of FexOy/SiO2 cellulose carbon aerogels was as high as 90 % within 60 min, demonstrating the synergistic effect of photocatalysis and Fenton reaction. This ingenious structure design provides new insight into the relationship between hierarchically porous structure of carbon aerogels and their catalytic degradation performance, and opens a new avenue to develop cellulose-based carbon aerogel catalysts with efficient catalytic performance.

Up-Scaled Preparation of Pt–Ni Aerogel Catalyst Layers for Polymer Electrolyte Fuel Cell Cathodes

Up-Scaled Preparation of Pt–Ni Aerogel Catalyst Layers for Polymer Electrolyte Fuel Cell Cathodes

Developing an FexCoyLaz-based amorphous aerogel catalyst for the oxygen evolution reaction via high throughput synthesis

High-throughput synthesis was used to fabricate ternary FexCoyLaz-based aerogel electrocatalysts for stoichiometric assessment. This work suggests a feasible way to find water-splitting non-precious metal electrocatalysts.

Sol–Gel Synthesized Nickel‐Doped Ruthenium Oxide Aerogel for Highly Efficient Acidic Hydrogen Evolution Reaction

Solar and wind energy for water electrolysis are gaining interest in contemporary times. In this context, platinum catalysts are commonly recognized as the standard for the hydrogen evolution reaction (HER), yet their effectiveness is constrained by their high cost and inadequate stability. Combining Ru and Ni lowers the material expense and greatly improves the electrocatalytic performance. Therefore, in the present study, a 3D nanostructured amorphous RuO2 aerogel is doped with various concentrations of Ni for enhanced HER activity. The results indicate that the 4% Ni‐RuO2 aerogel exhibits a 0D colloidal network featuring interconnected mesopores, with a high specific surface area of 241.5 m2·g−1. In addition, the 4% Ni‐RuO2 aerogel catalyst exhibits the lowest overpotentials of 63 and 122 mV at current densities of 10 and 50 mA·cm−2, respectively, along with enhanced hydrogen adsorption activity for the HER due to the 3D porous structure of the aerogel. However, a further increase in Ni doping leads to a decrease in HER activity due to a reduction in the number of catalytic Ru sites. The study found that doping with the optimum amount of Ni causes a redistribution of charges on the sample surface, thereby uncovering more reaction sites and enhancing the electrocatalytic performance.

Preparation of reusable copper-based biomass-carbon aerogel catalysts and their application in highly selective reduction of maleimides to succinimides with hydrosilane as a hydrogen source

A novel copper-based biomass-carbon aerogel catalyst was prepared as a highly efficient and selective catalyst for maleimides reduction for the first time with excellent catalytic activity, chemo-selectivity, and recyclability.

Electrothermal Transformations within Graphene-Based Aerogels through High-Temperature Flash Joule Heating.

Flash Joule heating of highly porous graphene oxide (GO) aerogel monoliths to ultrahigh temperatures is exploited as a low carbon footprint technology to engineer functional aerogel materials. Aerogel Joule heating to up to 3000 K is demonstrated for the first time, with fast heating kinetics (∼300 K·min-1), enabling rapid and energy-efficient flash heating treatments. The wide applicability of ultrahigh-temperature flash Joule heating is exploited in a range of material fabrication challenges. Ultrahigh-temperature Joule heating is used for rapid graphitic annealing of hydrothermal GO aerogels at fast time scales (30-300 s) and substantially reduced energy costs. Flash aerogel heating to ultrahigh temperatures is exploited for the in situ synthesis of ultrafine nanoparticles (Pt, Cu, and MoO2) embedded within the hybrid aerogel structure. The shockwave heating approach enables high through-volume uniformity of the formed nanoparticles, while nanoparticle size can be readily tuned through controlling Joule-heating durations between 1 and 10 s. As such, the ultrahigh-temperature Joule-heating approach introduced here has important implications for a wide variety of applications for graphene-based aerogels, including 3D thermoelectric materials, extreme temperature sensors, and aerogel catalysts in flow (electro)chemistry.