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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 469 records · Page 26
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Origins of Electrostriction in Poly(vinylidene fluoride)-Based Ferroelectric Polymers

Although electrostriction is ubiquitous for dielectric polymers, giant electrostriction has not been observed until relaxor ferroelectric (RFE) poly(vinylidene fluoride) (PVDF)-based polymers are achieved. However, the exact origin for giant electrostriction in these polymers has not been fully understood. By studying the electrostriction in the uniaxially stretched films of a ferroelectric poly(VDF-co-trifluoroethylene) [P(VDF-TrFE)] random copolymer and an RFE poly(VDF-co-TrFE-co-chlorotrifluoroethylene) [P(VDF-TrFE-CTFE)] random terpolymer in this work, we confirmed that ferroelectric switching with large hysteresis, such as in the case of P(VDF-TrFE), was not genuine electrostriction. By decreasing large ferroelectric domains to the nanometer scale (i.e., 2–3 nm), such as in the case of the P(VDF-TrFE-CTFE) terpolymer, electrostriction with low hysteresis could be achieved. Here, two origins of the large electrostriction in these polymers were identified. The first was the mechano-electrostriction due to the poling field-induced conformation transformation of oriented polymer chains. The second was the electric repulsion of electrically aligned nanodomains. These effects could occur in both crystals and the oriented amorphous fraction, which links between the nanocrystals and the isotropic amorphous fraction. When the poling field was relatively low (e.g., <40 MV/m), the mechano-electrostriction was the major contribution and the electric repulsion effect was a minor contribution to electrostriction. Meanwhile, a strong temperature dependence of the low-field electrostriction coefficient was observed. Finally, we found an empirical inverse relationship between the electrostriction coefficient and the product of Young’s modulus and dielectric constant. The knowledge obtained from this study provides an insightful understanding of the electrostriction mechanism in PVDF-based electroactive polymers, which will find potential applications in sensors and actuators for wearable electronics and soft robotics.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Exchangeable Liquid Crystalline Elastomers: Enabling Rapid Processing and Enhanced Actuation Stability through On-Demand Deactivation

Exchangeable liquid crystalline elastomers (xLCEs) bearing dynamic covalent bonds are promising candidates for soft actuators due to their unique capability to adjust both network structure and liquid crystalline (LC) alignment after polymerization. While current xLCEs with low exchange temperatures are convenient for processing, they suffer from issues such as creep and loss of LC alignment during repeated thermal actuation. Herein, we present an effective solution using dynamic anhydride chemistry within a thiol-ene-based xLCE. This approach enables a catalyst-free, low-temperature bond exchange of the xLCE after polymerization, allowing for the adjustment of LC orientation under mild conditions. More importantly, it enables on-demand deactivation of the bond exchange via anhydride hydrolysis, effectively eliminating creep and enhancing actuation stability for over 100 cycles. Furthermore, the hydrolysis process results in the formation of carboxylic acid groups, which can be converted into carboxylates via alkali treatment, thereby providing the xLCE with humidity responsiveness. Finally, these findings highlight the use of dynamic anhydride bonds in the fabrication and optimization of xLCEs with enhanced durability and functionality, which is expected to facilitate significant advancements in their applications in soft actuators and robotics.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The Buckling Spectra of Nanoparticle Surfactant Assemblies

Fine control over the mechanical properties of thin sheets underpins transcytosis, cell shape, and morphogenesis. Applying these principles to artificial, liquid-based systems has led to reconfigurable materials for soft robotics, actuation, and chemical synthesis. However, progress is limited by a lack of synthetic two-dimensional membranes that exhibit tunable mechanical properties over a comparable range to that seen in nature. In this study, we show that the bending modulus, B , of thin assemblies of nanoparticle surfactants (NPSs) at the oil–water interface can be varied continuously from sub- k B T to 10 6 k B T , by varying the ligands and particles that comprise the NPS. We find extensive departure from continuum behavior, including enormous mechanical anisotropy and a power law relation between B and the buckling spectrum width. Our findings provide a platform for shape-changing liquid devices and motivate new theories for the description of thin-film wrinkling.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2026

Reversible Polymer–Metal Mechanical Transitions Enabled by Electrochemical Modulation

The mechanical properties of materials, e.g., elastic modulus and hardness, are important for many engineering applications. Here, we introduce a hierarchically ordered structure (HOS) polymer system that exhibits exceptionally large, reversible changes in mechanical behavior upon electrochemical lithiation and delithiation. Full lithiation of the HOS polymer induces a substantial mechanical transition from polymer-like to metal-like attributes, yielding a 10-fold increase in elastic modulus and a 3-fold increase in hardness, with values comparable to those of aluminum. Upon removal of Li+ ions, the elastic modulus and hardness return to nearly pristine polymer levels, and this transformation remains highly repeatable over many electrochemical cycles. Reversible transitions between polymer-like and metal-like mechanical behaviors offer a new pathway for engineering materials for applications that require tunable mechanical properties, such as soft robotics and stimuli-responsive systems.

Thapa, Santosh↗
DOE OSTI2021

Performance of Spherical Quantum Well Down Converters in Solid State Lighting

We report the color conversion performance of amber and red emitting quantum dots (QDs) on InGaN solid-state lighting (SSL) light emitting diode (LED) packages. Spherical quantum well (SQW) architectures (CdS/CdSe 1- x S x /CdS) were prepared using a library of thio- and selenourea synthesis reagents and high throughput synthesis robotics. CdS/CdSe 1- x S x QDs with narrow luminescence bands were coated with thick CdS shells (thickness = 1.6-7.5 nm) to achieve photoluminescence quantum yields (PLQY) up to 88% at amber and red emission wavelengths (λ max = 600-642 nm, FWHM < 45 nm). The photoluminescence from SQWs encapsulated in silicone and deposited on LED packages was monitored under accelerated aging conditions (oven temperature = 85 °C, relative humidity = 5-85%, blue optical power density = 3-45 W/cm 2 ) by monitoring the red photon output over several hundred hours of continuous operation. The growth of a ZnS shell on the SQW surface increases the stability under long-term operation but also reduces the PLQY, especially of SQWs with thick CdS shells. The results illustrate that the outer ZnS shell layer is key to optimizing the PLQY and the long-term stability of QDs during operation on SSL packages.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Adhesion of Self-Complementary, Sinusoidal Surfaces Fabricated Using Two-Photon Polymerization

Microscale, pick-and-place assembly is a non-lithographic assembly method poised to impact diverse fields including flexible electronics, microfluidics and robotics. However, a major technological challenge is the need to deterministically control adhesion between parts. Here, switchable adhesion involving 3D-printed, self-complementary surfaces is demonstrated. Mechanical properties of metasurfaces pressed against flat, rigid substrates are modeled using finite element methods. A series of flat slabs and metastructured slabs with 2D sinusoidal surfaces are printed using two-photon polymerization (2PP) of a shape-memory resin. The surface frequency of featured slabs was varied between $3.\bar3$ mm −1 and $26.\bar6$ mm −1 with similar amplitudes. Adhesion between printed metasurfaces and glass and between printed, self-complementary metasurfaces is studied above and below the cured resin’s glass transition temperature (∼45 °C). Simple heating of adhering surfaces to above 60 °C lowers adhesion, and compression of surfaces while above the glass transition temperature followed by cooling to room temperature elevates adhesion. The nominal adhesive strength between printed, self-complementary surfaces, as determined by the maximum observable pull-off stress, exceeds 3 MPa. Further tailoring complementary surfaces for adhesion control may facilitate microscale disassembly for recovery of components or precious metals.

amorphous materials↗
DOE OSTI2025

Data-Driven Discovery of Bimetallic Nanoparticles Catalysts for the Hydrogenolysis of Polyethylene

Supported platinum nanoparticles are known to convert polyolefins to high-quality liquid hydrocarbons with hydrogen under relatively mild conditions. However, no systematic study has been undertaken using bimetallic catalysts for polyethylene upcycling. Specifically, a total of 98 monometallic and bimetallic combinations (Ag, Cr, Co, Cu, Fe, Ga, In, Mn, Ni, Pd, Pt, Rh, Ru, Zr) on alumina were synthesized utilizing surface organometallic chemistry (SOMC) technique via robotic platform. These were investigated at a small scale (10 mg of catalyst and 50 mg of polyethylene) for their activity for the hydrogenolysis of polyethylene in a high-throughput batch reactor. Combinations of Ni and Co were selected as candidates with high activity toward conversion into paraffin oils. Reaction conditions were optimized with Ni/Co/Al 2 O 3 catalyst at a larger scale (300 mg catalyst and 3 g polyethylene) to obtain a high yield (93.1%) of paraffin wax with desired properties (M n = 380 Da) and low polydispersity (Đ = 1.2). Ni/Co/Al 2 O 3 was compared against Co/Ni/Al 2 O 3 to understand the role of the deposition sequence. When Co is deposited before Ni, a layer of cobalt aluminate is formed upon reduction, stabilizing the deposition of 5 nm metallic Ni particles. When nickel is deposited before Co, particles are larger (average >20 nm) and more oxidized (Ni δ+ in NiAl 2 O 4 ), decreasing the availability of the catalytically active metallic Ni. In conclusion, the difference in electronic environments was also described by DFT calculations, which revealed that smaller 3D clusters of Ni are preferred on CoAl2O4 over the 3D clusters on NiAl 2 O 4 and that these smaller clusters are more reducible, as confirmed experimentally.

Polymer↗
DOE OSTI2022

Ambient Aerosol Is Physically Larger on Cloudy Days in Bondville, Illinois

Particle chemical composition affects aerosol optical and physical properties in ways important for the fate, transport, and impact of atmospheric particulate matter. For example, hygroscopic constituents take up water to increase the physical size of a particle, which can alter the extinction properties and atmospheric lifetime. At the collocated AERosol RObotic NETwork (AERONET) and Interagency Monitoring of PROtected Visual Environments (IMPROVE) network monitoring stations in rural Bondville, Illinois, we employ a novel cloudiness determination method to compare measured aerosol physicochemical properties on predominantly cloudy and clear sky days from 2010 to 2019. On cloudy days, aerosol optical depth (AOD) is significantly higher than on clear sky days in all seasons. Measured angstrom ngstro''m exponents are significantly smaller on cloudy days, indicating physically larger average particle size for the sampled populations in all seasons except winter. Mass concentrations of fine particulate matter that include estimates of aerosol liquid water (ALW) are higher on cloudy days in all seasons but winter. More ALW on cloudy days is consistent with larger particle sizes inferred from angstrom ngstro''m exponent measurements. Aerosol chemical composition that affects hygroscopicity plays a determining impact on cloudy versus clear sky differences in AOD, angstrom ngstro''m exponents, and ALW. This work highlights the need for simultaneous collocated, high-time-resolution measurements of both aerosol chemical and physical properties, in particular at cloudy times when quantitative understanding of tropospheric composition is most uncertain.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2026

Synergistic Evolution of Segmental Motion and Cooperative Relaxation within the Amorphous Phase of Organic Mixed Ionic-Electronic Conductors

Organic mixed ionic-electronic conductors (OMIECs) facilitate a variety of electrochemical processes and feature a heterogeneous microstructure composed of both crystalline and amorphous phases. However, structural evolution in amorphous regions during electrochemical doping remains poorly understood, limiting our understanding of mixed conduction mechanisms. Here, in this work, we develop operando chip calorimetry to probe amorphous phase evolution in poly­(3,4-ethylenedioxythiophene):poly­(styrenesulfonate) (PEDOT:PSS) under swelling and electrochemical (de)­doping. Our results reveal that amorphous regions providing ionic transport pathways and those within electronic transport channels undergo heterogeneous, yet synergistic, evolution during electrochemical modulation. The cooperative interplay between segmental motion and relaxation maintains ionic conductivity and intergrain electronic transport upon electrowetting and doping, while facilitating efficient ion hopping and adaptable chain conformations during dedoping. Such synergies are more pronounced in loose structures featuring a fibrillar morphology, which exhibit lower glass transition temperatures (T g ) and higher fragility (m). High-throughput robotic screening further establishes a strong correlation between elevated m/T g ratios and enhanced mixed conduction. These findings elucidate the role of the amorphous phase in the synthesis of OMIECs and underscore the potential of operando chip calorimetry in uncovering structure–property relationships in electroactive polymers.

amorphous phase↗
DOE OSTI2026

Dynamic Interfacial Design in Adaptive Hybrid Materials Enables Reversible and Tunable Mechano-Optic Smart Responses

Next-generation polymeric materials are shifting toward adaptive and interactive behaviors of living systems; however, designing materials that can reversibly modulate optical properties under mechanical deformation while maintaining mechanical robustness remains a key challenge. Here, we report a mechanically robust vitrimer-based adaptive hybrid material (AHM) that exhibits a stretch-induced reversible transparency-to-opacity transition, enabled by the integration of dynamic interactions at the polymer–silica nanoparticle interface and controlled nanoparticle self-assembly. The AHM combines boronic ester–functionalized polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene (S-Bpin) with diol-functionalized silica nanoparticles (diol-SiNPs) to form a hybrid network hosting both dynamic boronic ester and hydrogen-bonding interactions. These reversible linkages facilitate controlled nanoparticle self-assembly and enable strain-induced nanoparticle alignment/aggregation. Upon stretching, SiNP-rich domains align and aggregate within the polymer matrix, while local modulus mismatch between stiff aggregated SiNP/borylated-styrene-rich regions and the softer elastomeric midblock induces surface microwrinkle formation. These internal aggregates and surface wrinkles cooperatively enhance light scattering, producing the opaque state under strain. Furthermore, the tailored AHM exhibits high toughness, thermomechanical stability, reprocessability, and programmable shape-memory behavior. This work presents a dynamic interfacial design strategy for mechanically robust, optically reconfigurable, and reusable soft materials for adaptive optics, smart windows, sensing, soft robotics, and circular smart-material platforms.

adaptive hybrid materials↗
DOE OSTI2026

Production and Evaluation of Fluorophore-Doped Polymer Substrates to Screen for Plastic-Degrading Enzymes

Fast and sensitive analytical methods are the key to efficient screening of plastic-degrading enzymes. Here, we present a streamlined and affordable approach to assess the enzymatic deconstruction of insoluble synthetic polymers by blending them with a fluorescent dye, rhodamine 6G, and we evaluate this screening method using poly(ethylene terephthalate) (PET) as a model material. Our results indicate that enzymatic depolymerization of the rhodamine-doped PET can be observed in a high-throughput fashion by following release of the fluorophore. The fluorescence data obtained during the hydrolysis of rhodamine-doped PET by 14 PET hydrolases, produced with a robotic platform, correlated with the quantitative chromatographic analysis of PET degradation products. Remarkably, the use of the rhodamine-loaded PET substrate resulted in negligibly low background signals even when detecting PETase activity in crude cell lysates, suggesting suitability for screening of a wide variety of samples. Encouraged by these results, we next produced a selection of polyethylene- and nylon-based materials loaded with rhodamine 6G. While rapid leaching of fluorophore observed with nylon substrates limits the utility of the method for detecting nylonase activity, the rhodamine-loaded polyethylene showed promising performance in passive diffusion tests, indicating that this latter substrate may be used to screen for polyolefin-degrading enzymes.

09 BIOMASS FUELS↗
DOE OSTI2020

Light-Driven Expansion of Spiropyran Hydrogels

The incorporation of molecular switches in organic structures is of great interest in the chemical design of stimuli-responsive materials that mimic the complex functions of living systems. Merocyanine dyes that convert to spiropyran moieties upon exposure to visible light have been extensively studied as they can be incorporated in hydrated covalent networks that will expel water when this conversion occurs and induce a volumetric shrinkage. We report here on a sulfonatebased water soluble photoswitch that in contrast to the well-known system triggers a volumetric expansion in hydrogels upon exposure to photons. Contraction is in turn observed under dark conditions in a highly reversible manner. The novel behavior of the photoswitch incorporated in the covalent network was also predicted by coarse grain simulations of the system’s chemical structure. Using pH control and polymeric structures that differ in lower critical solution temperature we were able to develop hydrogels with highly tunable volumetric expansion. Furthermore, the novel molecular function of the systems developed here led to materials with the negative phototaxis observed in plants, and can expand the potential use of hydrogels as sensors, soft robots, and actuators.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

High-Throughput Discovery Illuminates Design Principles and Limits for Long-Lived Charged Species in Organic Electrolytes

The chemical stability of charged molecules in all-organic redox flow batteries (RFBs) is required for the prolonged operation of these devices. Molecular engineering and electrolyte optimization are used to mitigate parasitic reactions and extend the lifetimes of the charge carriers. However, how much can structural variation extend the lifetime? To probe this query, we designed a high-throughput kinetic study of the radical cation of N-methylphenothiazinium, guided by statistical sampling and learning algorithms. Using Argonne’s autonomous discovery facility, we conducted over 6,000 kinetic experiments with robotic sample preparation, parallel kinetic measurements, and machine learning inputs, testing 188 solvent molecules selected from a space of over 540 candidates from 11 chemical classes. Algorithmic selections guided us to stable solvent candidates, which were further tested in high concentration with and without supporting electrolyte. Our findings reveal the inherent difficulty of exceeding the current state of the art through solvent variation. The desired stability is statistically rare and poorly predictable. Among the many tested, only three solvents significantly outperformed our baseline, acetonitrile─and none by more than a factor of 3─suggesting a general challenge in achieving the necessary techno-economic targets. Furthermore, we suggest that self-discharge through solvent homolysis is the cause of the observed limitations. Several structural motifs contribute to >1,000 h half-life stability including molecular simplicity, symmetry, oxidation complement, and strategic fluorination. Importantly, this workflow establishes effective assays for diagnosing and predicting oxidative stress for highly stable liquid electrolytes in all batteries.

Batteries↗
DOE OSTI2026

Automated and High-Throughput Phase Separation Control for Supramolecular Polymer Blends Enabled by Machine Learning

Supramolecular polymer blends (SPBs) offer tunable morphologies that dictate their macroscopic properties, yet their rational design is limited by the absence of predictive structure−morphology models. Here, we introduce a data-driven highthroughput workflow that integrates modular polymer synthesis, robotic formulation, automated morphology characterization, and machine learning (ML) for accelerated SPB discovery. Using a plug-and-play synthetic strategy, 33 hydrogen-bonding endfunctional homopolymers were prepared and orthogonally combined to generate 260 SPBs in 1 day. A fully automated atomic force microscopy (AFM) pipeline enabled systematic imaging, producing 2340 morphology data sets with minimal human intervention. Domain spacings were extracted through complementary imageprocessing methods and used to train ML models. A support vector regression (SVR) model accurately predicted target phase-separation sizes (50, 100, and 150 nm), which were experimentally validated. This work demonstrates the power of coupling high-throughput experimentation with ML to accelerate morphology discovery and provides one of the first large-scale experimental data sets for supramolecular polymer systems.

ML-guided polymer design↗
DOE OSTI2021

Pyrolysis Vacuum-Assisted Plasma Ionization Ion Mobility–Mass Spectrometry for Insoluble Polymer Analysis

Wire-based metal additive manufacturing utilizes the ability of additive manufacturing to fabricate complex geometries with high deposition rates (above 7 kg/h), thus finding applications in the fabrication of large-scale components, such as stamping dies. Traditionally, the workhorse materials for stamping dies have been martensitic steels. However, the complex thermal gyrations induced during additive manufacturing can cause the evolution of an inhomogeneous microstructure, which leads to a significant scatter in the mechanical properties, especially the toughness. Therefore, to understand these phenomena, arc-based additive AISI 410 samples were fabricated using robotic gas metal arc welding (GMAW) and were subjected to a detailed characterization campaign. The results show significant scatter in the tensile properties as well as Charpy V-notch impact toughness data, which was then correlated to the microstructural heterogeneity and delta (δ) ferrite formation. Post-processing (austenitizing and tempering) treatments were developed and an ~70% reduction in the scatter of tensile data and a four-times improvement in the toughness were obtained. The changes in mechanical properties were rationalized based on the microstructure evolution during additive manufacturing. Based on these, an outline to tailor the composition of “printable” steels for tooling with isotropic and uniform mechanical properties is presented and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

High-Throughput Characterization and Optimization of Polyamide Hydrolase Activity Using Open Port Sampling Interface Mass Spectrometry

Enzymatic biodegradation of polymers, such as polyamides (PA), has the potential to cost-effectively reduce plastic waste, but enhancements in degradation efficiency are needed. Engineering enzymes through directed evolution is one pathway toward identification of critical domains needed for improving activity. However, screening such enzymatic libraries (100s-to-1000s of samples) is time-consuming. Here we demonstrate the use of robotic autosampler (PAL) and immediate drop on demand technology (I.DOT) liquid handling systems coupled with open-port sampling interface-mass spectrometry (OPSI-MS) to screen for PA6 and PA66 hydrolysis by 6-aminohexanoate-oligomer endo-hydrolase (nylon hydrolase, NylC) in a high-throughput (8–20 s/sample) manner. The OPSI-MS technique required minimal sample preparation and was amenable to 96-well plate formats for automated processing. Enzymatic hydrolysis of PA characteristically produced soluble linear oligomer products that could be identified by OPSI-MS. Incubation temperatures and times were optimized for PA6 (65 °C, 24 h) and PA66 (75 °C, 24 h) over 108 experiments. In addition, the I.DOT/OPSI-MS quantified production of PA6 linear dimer (8.3 ± 1.6 μg/mL) and PA66 linear monomer (13.5 ± 1.5 μg/mL) by NylC with a lower limit of detection of 0.029 and 0.032 μg/mL, respectively. For PA6 and PA66, linear oligomer production corresponded to 0.096 ± 0.018% and 0.204 ± 0.028% conversion of dry pellet mass, respectively. The developed methodology is expected to be utilized to assess enzymatic hydrolysis of engineered enzyme libraries, comprising hundreds to thousands of individual samples.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Unimodal Imaging of Monovalent Metal-Chelator Complexes and Lipids by MALDI Imaging Mass Spectrometry

Careful regulation of monovalent metal ions (M + ) is necessary to maintain a functional cellular system. Of these ions, appropriate sodium (Na + ) and potassium (K + ) concentrations are particularly integral for electrochemical signaling, as well as the secondary transport of nutrients and waste. Dysregulation of M + homeostasis can disrupt these mechanisms, potentially influencing the metabolism of downstream biomolecules such as lipids. Thus, the relationship between M + abundances and related biomolecular distributions must be elucidated to better understand the physiology of healthy and disordered tissues. Traditional techniques for imaging biological metal distributions include SIMS, LA-ICP-MS, and XRF; however, these capabilities are limited to elemental analysis or the analysis of molecular fragments and must be paired with other modalities to visualize distributions of more complex biomolecules within the same or similar samples. Conversely, matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI IMS) is a powerful tool often used for mapping such biomolecular distributions, but current methods are unable to detect metals within tissue. This study illustrates a novel methodology that adds metal detection to the MALDI IMS repertoire through which the simultaneous detection of M + metals and lipids is achievable. Using a robotic sprayer for homogeneous application, on-tissue deposition of the chelator deferiprone (DEF) enables subsequent detection of the ionizable metal-chelator complex by MALDI without hindering lipid detection. Our work provides proof-of-concept data for the simultaneous detection of K + , Na + , and intact lipids using MALDI IMS.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Response Surface Methodology As a New Approach for Finding Optimal MALDI Matrix Spraying Parameters for Mass Spectrometry Imaging

Automated spraying devices have become ubiquitous in laboratories employing matrixassisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI), in part because they permit control of a number of matrix application parameters that can easily be reproduced for intra- and interlaboratory studies. Determining the optimal parameters for MALDI matrix application, such as temperature, flow rate, spraying velocity, number of spraying cycles, and solvent composition for matrix application, is critical for obtaining high-quality MALDI-MSI data. However, there are no established approaches for optimizing these multiple parameters simultaneously. Instead optimization is performed iteratively (i.e., one parameter at a time), which is time consuming and can lead to overall non-optimal settings. In this report, we demonstrate the use a novel experimental design and the response surface methodology to optimize five parameters of MALDI matrix application using a robotic sprayer. Thirtytwo combinations of MALDI matrix spraying conditions were tested, which allowed us to elucidate relationships between each of the application parameters as determined by MALDI-MS (specifically, using a 15 Tesla Fourier transform ion cyclotron resonance mass spectrometer). As such, we were able to determine the optimal automated spraying parameters that minimized signal de-localization and enabled high MALDI sensitivity. We envision this optimization strategy can be utilized for other MALDI-MSI applications, tissue types, and matrix application approaches.

60 APPLIED LIFE SCIENCES↗