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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Sustainable Synthesis of NiMo Alloy Nanoparticles for Hydrogen Evolution Catalysis Using a Recyclable Ionic Liquid Solvent

Advancing the sustainability of nanoparticle electrocatalyst synthesis requires reducing solvent waste without compromising catalytic performance. Here, we report a rapid, microwave‐assisted colloidal synthesis of NiMo alloy nanoparticles in the ionic liquid 1‐butyl‐3‐methylimidazolium bis(trifluoromethylsulfonyl)imide (BMIM‐NTf 2 ), which serves as both reaction medium and recyclable solvent. NiMo nanoparticles with tunable compositions were obtained within 1 min at 230 °C, with Ni 0.86 Mo 0.14 giving the highest activity toward the hydrogen evolution reaction (HER), achieving an onset potential of −129 mV, an overpotential at 10 mA cm −2 of −290 mV versus RHE in acidic electrolyte, and >99% Faradaic efficiency. The ionic liquid was recovered and purified via aqueous NH 4 OH extraction, removing over 99% of residual Mo species, and reused for up to five successive syntheses. Nanoparticles prepared in recycled BMIM‐NTf 2 retained comparable crystallinity, morphology, and catalytic activity, with stable HER performance over 45 h of electrolysis. These results demonstrate that ionic liquid recycling can improve the sustainability of the preparation of NiMo nanoparticle electrocatalysts while preserving performance and material integrity.

bimetallic alloy↗
DOE OSTI2021

Solvation Structure and Dynamics of Mg(TFSI) 2 Aqueous Electrolyte

Using ab initio molecular dynamics (AIMD) simulations, classical molecular dynamics (CMD) simulations, small-angle X-ray scattering (SAXS), and pulsed-field gradient nuclear magnetic resonance (PFG-NMR), the solvation structure and ion dynamics of magnesium bis(trifluoromethanesulfonyl)imide (Mg(TFSI) 2 ) aqueous electrolyte at 1, 2, and 3 m concentrations are investigated. From AIMD and CMD simulations, the first solvation shell of an Mg 2+ ion is found to be composed of six water molecules in an octahedral configuration and the solvation shell is rather rigid. The TFSI - ions prefer to stay in the second solvation shell and beyond. Meanwhile, the comparable diffusion coefficients of positive and negative ions in Mg(TFSI) 2 aqueous electrolytes have been observed, which is mainly due to the formation of the stable [Mg(H 2 O) 6 ] 2+ complex, and, as a result, the increased effective Mg ion size. Finally, the calculated correlated transference numbers are lower than the uncorrelated ones even at the low concentration of 2 and 3 m, suggesting the enhanced correlations between ions in the multivalent electrolytes. This work provides a molecular-level understanding of how the solvation structure and multivalency of the ion affect the dynamics and transport properties of the multivalent electrolyte, providing insight for rational designs of electrolytes for improved ion transport properties.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Multi‐electron Oxidation of Ce(III) Complexes Facilitated by Redox‐Active Ligands

A family of cerium complexes featuring a redox-active ligand in different oxidation states has been synthesized, including the the iminosemiquinone (isq) 1− compound, Ce( dipp isq) 3 (1-Ceisq), and the amidophenolate (ap) 2− species Ce III ( dipp ap) 3 K 3 (2-Ceap), [Ce III ( dipp ap) 3 K][K(18-c-6)] 2 (2-Ceap 18c6), and [Ce III ( dipp ap) 3 K][K(15-c-5) 2 ] 2 (2-Ceap 15c5). Treating 2-Ceap 15c5 with dioxogen furnishes the cerium(IV) derivative [Ce IV ( dipp ap) 3 ][K(15-c-5) 2 ] 2 (3-Ceap 15c5), and an analogous synthesis can be used to generate [Ce IV ( dipp ap) 3 ][K(crypt)] 2 (3-Ceap crypt). Similarly, addition of hexamethyldisiloxane produces an interesting bis(amidophenolate) species, [(Me 3 SiO) 2 Ce IV ( dipp ap) 2 ][K(15-c-5) 2 ] 2 (4-CeOSiMe 3 ). In conclusion, full spectroscopic and structural characterization of each derivative was performed to establish the oxidation states of both the ligands and the cerium ions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Lithium-Ion Battery Testing Capable of Simulating “Ultralow” Lunar Temperatures

The first-ever lithium-ion battery cycler capable of testing the coin and pouch cells under ultralow (≤40 °C) temperatures down to -175 °C to simulate extreme climates found in the lunar and space missions, high-altitude air vehicles, polar regions of Earth, and military expeditionary missions is enthusiastically reported. The extremely cold temperatures are achieved through a tailored extreme low-temperature system (ELTS) with liquid nitrogen flow and the ability to reach temperatures between -175 and 25 °C, using 1 kΩ and 1 MΩ resistors at varying currents of 1–4 mA and 1–4 μA, respectively, is validated. Employing the ELTS, Li 4 Ti 5 O 12 (LTO)||Li cells with 1 m lithium bis(fluorosulfonyl)imide in cyclopentyl methyl ether as an electrolyte developed in this research group are charged and discharged at room temperature (cycling rate C/5), -20 (C/10), -40 (C/40), and -60 °C (C/50), which exhibited discharge capacities of 159.04, 119.12, 101.79, and 33.06 mAh g -1 , respectively. Moreover, the LTO||Li cell produced a reversible capacity of 7.12 mAh g -1 tested at -100 °C for the first time.

25 ENERGY STORAGE↗
DOE OSTI2024

Ionic Thermoelectric Generators in Vertical and Planar Topologies Based on Fluorinated Polymer Hybrid Materials with Ionic Liquids

Abstract Ionic thermoelectrics (TEs), in which voltage generation is based on ion migration, are suitable for applications based on their low cost, high flexibility, high ionic conductivity, and wide range of Seebeck coefficients. This work reports on the development of ionic TE materials based on the poly(vinylidene fluoride‐trifluoroethylene), Poly(VDF‐co‐TrFE), as host polymer blended with different contents of the ionic liquid, IL, 1‐ethyl‐3‐methylimidazolium bis(trifluoromethylsulfonyl)imide, [EMIM][TFSI]. The morphology, physico‐chemical, thermal, mechanical, and electrical properties of the samples are evaluated together with the TE response. It is demonstrated that the IL acts as a nucleating agent for polymer crystallization. The mechanical properties and ionic conductivity values are dependent on the IL content. A high room temperature ionic conductivity of 0.008 S cm −1 is obtained for the sample with 60 wt% of [EMIM][TFSI] IL. The TE properties depend on both IL content and device topology‐vertical or planar‐the largest generated voltage range being obtained for the planar topology and the sample with 10 wt% of IL content, characterized by a Seebeck coefficient of 1.2 mV K −1 . Based on the obtained maximum power density of 4.9 µW m −2 , these materials are suitable for a new generation of TE devices.

Pereira, Nelson↗
DOE OSTI2026

In-Process Melt Separation of Depolymerized PET in PET/PE Blends for Upcycling via Twin-Screw Extrusion

Our previous work focused on depolymerizing polyethylene terephthalate (PET) in twin-screw extrusion, as part of a broader project to continuously separate PET from polyolefins in the melt. This study focused on linear low-density polyethylene (LLDPE) and PET films and the use of ethylene glycol (EG), diethylene glycol (DEG), triethylene glycol (TEG), and bis(2-hydroxyethyl) terephthalate (BHET) to depolymerize the PET in the extruder to levels above 90% Mw. In this work, the focus will shift to achieving separation of the two polymers in the twin-screw extruder, which is made possible due to a 90% reduction in the Mw of the PET, which caused a decrease of its viscosity by several orders of magnitude. Owing to the viscosity difference and pressure buildup in the die, the low-viscosity PET preferentially exited a degassing vent instead of going through the die. This is because the flow of the PET would travel through a non-pressure vent rather than through a high-pressure die. However, owing to the higher viscosity of the LLDPE, the pressure was too high to pass through such a small diameter vent hole. Supercritical CO 2 (SCCO 2 ) was used to assist in this extraction, but SCCO 2 negatively impacted the overall degree of separation. Through analysis of the separated materials, it was concluded that a high separation of the two materials was achieved. TGA and FTIR confirmed that the material separated from the vent was 100% PET. The material removed from the die was composed of 95% LLDPE and 5% PET.

36 MATERIALS SCIENCE↗
DOE OSTI2026

In‐Process Melt Separation of PE/PET Blends for Upcycling via Twin‐Screw Extrusion. Impact of Catalyst Reagents on PET Depolymerization

Part 1 of this work focused on depolymerizing polyethylene terephthalate (PET) in twin-screw extrusion, as part of a broader project to continuously separate PET from polyolefins in the melt. This study focused on linear low-density polyethylene (LLDPE) and PET films and the use of ethylene glycol (EG), diethylene glycol (DEG), triethylene glycol (TEG), and bis(2-hydroxyethyl) terephthalate (BHET) to depolymerize the PET in the extruder to levels above 90% Mw. In part 2, the focus will shift to achieving separation of the two polymers in the twin-screw extruder, which is made possible due to a 90% reduction in the Mw of the PET, which caused a decrease of its viscosity by several orders of magnitude. Owing to the viscosity difference and pressure buildup in the die, the low-viscosity PET preferentially exited a degassing vent instead of going through the die. This is because the flow of the PET would travel through a non-pressure vent rather than through a high-pressure die. However, owing to the higher viscosity of the LLDPE, the pressure was too high to pass through such a small diameter vent hole. Supercritical CO₂ (SCCO₂) was used to assist in this extraction, but SCCO₂ negatively impacted the overall degree of separation. Through analysis of the separated materials, it was concluded that a very high separation of the two materials was achieved. TGA and FTIR confirmed that the material separated from the vent was 100% PET. The material removed from the die was composed of 90% LLDPE and 10% PET.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Identification of Blue Discoloration in PBX 9404 using Ultrahigh Pressure Liquid Chromatography with Quadrupole Time-of-Flight Mass Spectrometry

PBX 9404, composed of 94 wt% HMX (1,3,5,7-Tetranitro-1,3,5,7-tetrazoctane), 3 wt% NC (nitrocellulose), 2.9 wt% CEF (tris(beta-chloroethyl) phosphate) and 0.1 wt% DPA (diphenylamine), has often been observed with a slight to entire blue discoloration of the manufactured prills. This blue discoloration has been observed since the formulation development of PBX 9404 in the late 1950s. In order to determine the source of the blue discoloration in PBX 9404, ultraviolet/visible (UV/Vis) absorbance of PBX 9404 and two potential candidates for the discoloration, p-nitrosodiphenylamine (p-NDPA) and N-nitrosodiphenylamine (N-NDPA) were evaluated. An absorbance band at 590 nm in PBX 9404 sample was attributed to the blue discoloration while p-NDPA and N-NPDA had different absorbance bands. Using the knowledge gained from the UV/Vis analysis, a semi-targeted approach using ultrahigh pressure liquid chromatography coupled to UV/Vis detector and quadrupole time of flight mass spectrometry (UHPLC-UV/Vis-QTOF) was implemented. Investigating the UHPLC-UV/Vis-QTOF chromatograms at a wavelength of 590 nm, a single compound was tentatively identified as being the source of the blue discoloration. Targeted tandem mass spectrometry (MS/MS) on the compound and subsequent analysis indicated that 4,4 -{[4-(Phenylimino)-2,5-cyclohexadien-1-ylidene]methylene}bis(N-phenylaniline), also known as Spirit Blue Base, was the source of the blue discoloration, which was confirmed using a standard. Here, a theory on the formation of Spirit Blue Base in PBX 9404 involving DPA, nitric acid (HNO 3 ) / nitrogen oxide(s) NO x , and formaldehyde is proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Characterization of NBCMA—A DAPO Precursor

As part of our investigation into the process optimization of 2,6-diaminopyrazine-1-oxide (DAPO), small-scale sensitivity testing (impact, friction, and ESD) was conducted on the precursor, N-nitroso-bis(cyanomethyl)amine (NBCMA). NBCMA exhibited moderate sensitivity to friction, whereas no sensitivity to impact or spark was observed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Position-specific carbon isotope analysis of serine by gas chromatography/Orbitrap mass spectrometry, and an application to plant metabolism

Position-specific 13 C/ 12 C ratios within amino acids remain largely unexplored in environmental samples due to methodological limitations. We hypothesized that natural-abundance isotope patterns in serine may serve as a proxy for plant metabolic fluxes including photorespiration. Here we describe an Orbitrap method optimized for the position-specific carbon isotope analysis of serine to test our hypothesis and discuss the generalizability of this method to other amino acids. Position-specific carbon isotope ratios of serine were measured using a Thermo Scientific™ Q Exactive™ GC Orbitrap™. Amino acids were hydrolyzed from Arabidopsis biomass, purified from potential matrix interferences, and derivatized alongside standards. Derivatized serine (N,O-bis(trifluoroacetyl)methyl ester) was isolated using gas chromatography, trapped in a reservoir, and purged into the electron ionization source over tens of minutes, producing fragment ions containing different combinations of atoms from the serine-derivative molecule. The 13 C/ 12 C ratios of fragments with monoisotopic masses of 110.0217, 138.0166, and 165.0037 Da were monitored in the mass analyzer and used to calculate position-specific δ 13 C values relative to a working standard. This methodology constrains position-specific δ 13 C values for nanomole amounts of serine isolated from chemically complex mixtures. The δ 13 C values of fragment ions of serine were characterized with ≤1‰ precisions, leading to propagated standard errors of 0.7–5‰ for each carbon position. Position-specific δ 13 C values differed by up to ca 28 ± 5‰ between serine molecules hydrolyzed from plants grown under contrasting pCO 2 , selected to promote different fluxes through photosynthesis and photorespiration. The method was validated using pure serine standards characterized offline. Here this study presents the first Orbitrap-based measurements of natural-abundance, position-specific carbon isotope variation in an amino acid isolated from a biological matrix. We present a method for the precise characterization of isotope ratios in serine and propose applications probing metabolism in plants. We discuss the potential for extending these approaches to other amino acids, paving the way for novel applications.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Metal-Free, Oxidative Condensation of Heteroaryl- and Aryl Carbaldehydes towards Functionalized Carbonitriles

Functionalization of pyridines with the carbonitrile group for advanced cyclization reactions routinely incorporates metals, toxic oxidants, and cyanide reagents, often in linear synthetic sequences. Here, motivated by the strategic need of a heteroaryl carbonitrile synthon for further elaboration, we disclose an efficient, metal-free, one-pot reaction sequence that uses ammonium acetate as the nitrogen source and bis-acetoxyiodobenzene as the oxidant with low loadings. The developed method tolerates a diverse substrate scope including heteroaryl, aryl, and alkyl substrates with similar efficiency and expands the practitioner's reaction. Method development, optimization, substrate scope, preliminary mechanistic observations, competition experiments, and a scale up reaction are delineated herein.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Multi–Modular Design of Stable Pore–Space–Partitioned Metal–Organic Frameworks for Gas Separation Applications

Pore space partition (PSP) is an effective materials design method for developing high-performance small-pore materials for storage and separation of gas molecules. The continued success of PSP depends on broad availability and judicious choice of pore-partition ligands and better understanding of each structural module on stability and sorption properties. Here, by using substructural bioisosteric strategy (sub-BIS), a dramatic expansion of pore-partitioned materials is targeted by using ditopic dipyridyl ligands with non-aromatic cores or extenders, as well as by expanding heterometallic clusters to uncommon nickel–vanadium and nickel–indium clusters rarely known before in porous materials. The dual-module iterative refinement of pore-partition ligands and trimers leads to remarkable enhancement of chemical stability and porosity. Here a family of 23 pore-partitioned materials synthesized from five pore-partition ligands and seven types of trimeric clusters is reported. New materials with such compositionally and structurally diverse framework modules reveal key factors that dictate stability, porosity, and gas separation properties. Among these, materials based on heterometallic vanadium–nickel trimeric clusters give rise to the highest long-term hydrolytic stability and remarkable uptake capacity for CO 2 , C 2 H 2 /C 2 H 4 /C 2 H 6 , and C 3 H 6 /C 3 H 8 hydrocarbon gases. Here, the breakthrough experiment shows the potential application of new materials for separating gas mixtures such as C 2 H 2 /CO 2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Polycarbonate‐Based Solid‐Polymer Electrolytes for Solid‐State Sodium Batteries

Solid-polymer electrolytes comprised of polypropylene carbonate (PPC) and varied sodium bis(fluorosulfonyl)imide (NaFSI) salt concentrations are investigated for implementation as a conductive solid polymer electrolyte into solid-state cathode composites utilizing a sodium-layered oxide active material. The ionic conductivity generally increases with NaFSI salt content, reaching ≈1 mS cm −1 at 80 °C at the highest salt concentration (PPC:NaFSI = 0.5:1). Through an all-in-one slurry casting method, Na 2/3 Ni 1/3 Mn 2/3 O 2 cathode composites are fabricated in which the dispersed PPC electrolyte acts as the primary binder. Enabled by a bilayer polymer electrolyte system, cycling performance with the PPC cathode electrolyte is optimized with respect to salt concentration and anode material. The best cyclability is achieved with a moderate salt concentration electrolyte (PPC:NaFSI = 5:1), showcasing an initial capacity of 83 mA h g −1 with a remarkable 80% capacity retention after 150 cycles at C/5 rate and 60 °C. The superior performance of the lower salt concentration electrolyte is attributed to better electrochemical stability, as confirmed by linear sweep voltammetry and online electrochemical mass spectrometry measurements. In conclusion, these results underscore the potential of carbonate-based polymer electrolytes and the importance of balancing electrolyte conductivity and stability in cell design.

25 ENERGY STORAGE↗
DOE OSTI2023

Microwave‐Assisted Synthesis of SrTiO 3 Nanocuboids without TiCl 4

Strontium titanate (STO) nanocuboids are a novel support for Pt nanoparticle catalysts (Pt/STO). The first of many steps in commercializing Pt/STO will be developing a scalable, environmentally sustainable, and cost‐effective STO nanocuboid synthesis. Herein, Sr–Ti–OH mixtures are synthesized from various Sr 2+ and Ti 4+ reagents and treated by convection‐ and microwave‐assisted heating to obtain STO nanoparticles. These experiments clarify how phase composition of the prehydrothermal Sr–Ti–OH mixture and choice of heating method affect final nanoparticle morphology. In Sr–Ti–OH mixtures synthesized with TiCl 4 , STO is the most stable phase and precipitates prior to heating, while titania sol–gels are the most stable phase when other Ti 4+ sources are used. STO nanocrystals always form when Sr–Ti–OH mixtures are treated by convection heating, though nanocuboids are only observed if STO precipitates from the Sr–Ti–OH mixture. Microwave‐assisted hydrothermal treatment more rapidly heats the precursor solution, and thus, STO nanocuboids can form from a variety of Sr–Ti–OH mixtures regardless of mixture composition. Two microwave syntheses of STO nanocuboids are reported: one which uses TiCl 4 as a Ti 4+ source, and another that uses titanium(IV) bis(ammonium lactato) dihydroxide ([NH 4 CH 3 CH(O)CO 2 ] 2 Ti(OH) 2 ), a water‐stable Ti 4+ complex.

Peczak, Ian L.↗
DOE OSTI2025

Tunable Crosslinked Ether Polymer Network Electrolytes for High‐Performance All‐Solid‐State Sodium Batteries

All-solid-state batteries (ASSBs) are critical for achieving high energy density and enhanced safety. Solid polymer electrolytes (SPEs) offer key advantages over other electrolytes, including improved safety, flexibility, and interfacial contact. Among the SPEs, ether-based polymers are widely studied due to their ease of processing and high ionic conductivity (σi) in the amorphous state. In this work, the introduction of poly(ethylene glycol) methyl ether methacrylate (PEGMEMA) into an SPE matrix composed of poly(ethylene glycol) diacrylate (PEGDA), poly(ethylene glycol) (PEG2k), and sodium bis(fluorosulfonyl)imide (NaFSI) salt is investigated to facilitate the formation of amorphous, high σ i SPEs through end-group engineering and polymer ratio optimization. PEGMEMA enhances structural integrity via crosslinking with PEGDA through its methacrylate group, while its methyl end group aids ion conduction. A 2:1:7 ratio of PEGDA:PEGMEMA:PEG2k exhibits a σi of 1.16 x 10 -4 S cm -1 and oxidative stability up to 4.4 V at 60 °C. A solid-state cell incorporating this SPE, a Na 2/3 Ni 1/3 Mn 2/3 O 2 (NM12) cathode, and a sodium-metal anode demonstrates excellent cycling stability, retaining over 80 % of its initial capacity for 150 cycles at 60 °C. The findings highlight the potential of end-group engineering in improving the electrochemical performance of SPEs.

25 ENERGY STORAGE↗
DOE OSTI2021

Super Flexible Transparent Conducting Oxide-Free Organic–Inorganic Hybrid Perovskite Solar Cells with 19.01% Efficiency (Active Area=1 cm 2 )

Highly efficient organic-inorganic hybrid perovskite solar cells (OIHP-SCs) are often fabricated on a transparent conducting oxide (TCO) substrate such as indium tin oxide (ITO). However, the presence of TCOs is disadvantageous to the development of flexible OIHP-SCs due to the brittle nature of ITO which is easily breakable during bending. Herein, a flexible TCO-free OIHP-SC is demonstrated by using lithium bis(trifluoromethane)sulfonimide (Li-TFSI) as a codopant for the single-layer graphene transparent conducting electrode and poly(triarylamine) hole-transporting material (HTM) on a flexible polydimethylsiloxane substrate. The optical and electrical properties of the Li-TFSI-doped graphene substrate are measured by controlling the doping amount and the best conditions for charge extraction are established at a doping concentration of 20 mm Li-TFSI, thus optimizing the device photovoltaic performance. As a result, a highest power conversion efficiency of 19.01% is demonstrated by the flexible TCO-free OIHP-SC devices with an active area of 1 cm 2 . In addition, the flexible TCO-free OIHP-SCs exhibit good bending stability after 5000 bending cycles at radii of 6, 4, and 2 mm and excellent light soaking stability under 1 Sun light intensity over 1000 h as opposed to the poor stability when using poly(3,4-ethylenedioxythiophene) polystyrene sulfonate as the HTM.

14 SOLAR ENERGY↗
DOE OSTI2023

Archeological wood conservation with selected organosilicon compounds studied by XFM and nanoindentation

Waterlogged wood conservation is a complex and challenging task. Detailed knowledge about the interactions between the applied chemicals and wood is necessary to ensure the effective and safe conservation of wooden artifacts. The present research aims to determine the mechanism of dimensional stabilization of archeological wood by organosilicon compounds using the combination of synchrotron-based X-ray fluorescence microscopy (XFM) and nanoindentation. Archeological oak wood was treated with methyltrimethoxysilane, (3-mercaptopropyl)trimethoxysilane, or 1,3-bis-[(diethylamino)-3-(propoxy)propan-2-ol]-1,1,3,3-tetramethyldisiloxane, which in previous studies were found to be more effective than other organosilicons in stabilizing wood dimensions. The XFM and nanoindentation results showed that all three organosilicons infiltrated wood cell walls and enhanced their mechanical properties. The XFM also showed that part of the chemicals filled some void spaces like cell lumina. Based on the results obtained here and in our previous research, it is determined that the mechanism of archeological wood dimensional stabilization by organosilicon treatment is complex and likely involves both filling cell lumina and infiltration into cell walls where organosilicons interact with wood polymers.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Conservation of model degraded pine wood with selected organosilicons studied by XFM and nanoindentation

Previous research found that some organosilicon treatments proved effective in stabilizing waterlogged wood dimensions during drying. The present research aimed to determine the mechanism of wood stabilization by these chemicals to understand their mode of action. Here, the study used chemically (ChP) and biologically degraded (BP) model Scots pine wood treated with Methyltrimethoxysilane (MTMS), (3-Mercaptopropyl) trimethoxysilane (MPTMS), or 1,3-Bis(diethylamino)-3-propoxypropanol)-1,1,3,3-tetramethyldisiloxane (DEAPTMDS). Synchrotron-based X-ray fluorescence microscopy (XFM) was used to investigate the penetration of organosilicons into the wood cellular structure and cell walls, and nanoindentation was used to study the mechanical properties of the treated wood cell walls. All treatments resulted in high volumetric anti-shrink efficiency (ASE V ) values of 74-82%, except for MTMS-treated ChP with an ASE V of 52%. The multiscale XFM results revealed that all applied organosilicons penetrated throughout the whole wooden blocks and deposited in both cell lumina and cell walls. The retention of all applied organosilicons was highest in BP wood, and so was the dimensional stabilization effect. MTMS-treated ChP had the lowest measured cell wall infiltration, which likely contributed to its lower ASE v . DEAPTMDS treatments plasticized the cell walls and resulted in lowered nanoindentation elastic modulus (E s NI ) and hardness (H) for all types of wood. MTMS and MPTMS had modest effects on cell wall mechanical properties, and the effect depended on the type of wood. The final effect of organosilicon treatment on the dimensional wood stabilization and mechanical properties of wood cell walls depended not only on the type of the applied organosilicon but also the type of wood degradation. This means that the treatment cannot be considered universal, and specific approaches are needed for the conservation of individual wooden objects. Although some mechanisms are now better understood, such as the need for organosilicons to infiltrate the cell walls and the plasticizing effect of DEAPTMDS, other aspects will benefit from a more detailed analysis of the molecular interactions between organosilicons and wood polymers.

59 BASIC BIOLOGICAL SCIENCES↗