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DOE Award No. DE-SC0022463 Final Report

This phase II grant was canceled by the SBIR program when Nion was acquired by Bruker because Bruker is not "small". This final technical report is an effort to properly close out the paperwork for this canceled project.

Lovejoy, Tracy [Bruker]↗

Device- and System-Level Thermal Packaging for Electric-Drive Technologies (Final Technical Report)

Final Technical ReportThis project aimed to research, develop, and test electric traction drive system technology for use in vehicle applications that are capable of meeting the targets set by the Department of Energy Vehicle Technologies Office. The project is categorized into three major thrusts: Bonding interfaces for packaging, thermal management of electric vehicle (EV) power inverters, and electric motor thermal management. Device- and System-Level Thermal Packaging for Electric-Drive Technologies project aimed to develop, analyze, and validate transformative approaches in thermal management and packaging for power electronics and electric motor systems, with the ultimate goal of enhancing power density, efficiency, and reliability in electrified transportation platforms.

33 ADVANCED PROPULSION SYSTEMS↗

Report on Initial Sodium Testing on the Thermal Hydraulic Experimental Test Article (THETA) (Fiscal Year 2024 Final Report)

The Thermal Hydraulic Experimental Test Article (THETA) is a facility that is used to develop sodium components and instrumentation as well as to acquire experimental data for validation of reactor thermal hydraulic and safety analysis codes. The facility simulates nominal thermal hydraulic conditions as well as protected/unprotected loss of flow accidents in a sodium-cooled fast reactor (SFR). High fidelity distributed temperature profiles of the developed flow field may be acquired with Rayleigh backscatter based optical fiber temperature sensors. The facility was designed in partnership with systems code experts to tailor the experiment to ensure the most relevant and highest quality data for code validation. THETA is comprised of a traditional primary coolant and secondary coolant system. The primary system is submerged in the pool of sodium and consists of a pump, electrically heated core, intermediate heat exchanger, and connected piping and thermal barriers (redan). The secondary system, located outside of the sodium pool, consists of a pump, sodium to air heat exchanger, and connected piping and valves. In fiscal year 2023, thermal stratification tests were completed with the primary system online, while the secondary system was being constructed [1]. These tests had shown that the core barrel and intermediate heat exchanger (IHX) outlet required increased thermal insulation. The THETA primary system was removed from METL, cleaned, thermal insulators installed, and then inserted into METL Test Vessel 4. At the time of this writing the THETA primary and secondary system are operational. During this fiscal year 100+ hours of testing was completed to characterize thermal hydraulic phenomena associated with steady state and transient conditions in a pool type liquid metal cooled reactor. A majority of the testing campaign was completed to satisfy the experimental data acquisition requirements for the GAIN Voucher with Oklo, CRADA 2021-21121. THETA is still operational at the time of this publication and future testing is planned for fiscal year 2025. Work is underway to publish existing and future data to an online database to facilitate collaboration with SFR engineers looking to validate their systems code or computational fluid dynamics models.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Radiation Aging of Cable Insulation Systems to Support Extension of Cable Electrical Assessment Techniques - CRADA 562 (Final Report)

Radiation aging (primarily gamma radiation) affects a small subset of the LV cable population based on a 40-year operation. Increasing plant operating life to 60 or 80 years will result in additional cables experiencing degradation, either from radiation or from combined thermal and radiation effects. Previous research work done by EPRI and other researchers focuses on electrical diagnostics of thermal effects. However, the electrical diagnostic response of the cable system to radiation aging is minimally understood. In order to study the electrical responses from XLPE and EPR cabling and correlate these responses with radiation dose and level of thermal exposure, gamma radiation testing was performed at Pacific Northwest National Laboratory (PNNL). This report covers the radiation testing performed at PNNL, which involved irradiation of 30-foot long cables and short witness samples. The cabling was irradiated, at room temperature, using cobalt-60 gamma-rays to intervals of 10 million rads (10 Mrads), for a maximum of 70 Mrads. The results can be used to determine cable conditions (extent of damage) more accurately and localize where the degradation exists along the length of the cable (axial location). These insights can provide operators with the options to focus repair, mitigation, or replacement efforts locally.

36 MATERIALS SCIENCE↗

Routine & Nonredundant Steel Tension Member (NSTM) Inspection Report (Final): Property ID No. 43-0434 - Los Alamos Canyon Bridge

This report covers the inspection findings for the Routine and Nonredundant Steel Tension Member (NSTM) Inspection of the Los Alamos Canyon Bridge over Omega Rd conducted on June 7-9, 2024. The inspections were completed according to the standards referenced in DOE O 437.1 Bridge and Tunnel Management including the National Bridge Inspection Standards (23 CFR Part 650, dated 12/14/2004) and other Federal Highway Administration (FHWA), New Mexico Department of Transportation (NMDOT), and American Association of State Highway and Transportation Officials (AASHTO) codes and standards.

42 ENGINEERING↗

Production of 1,3-Butadiene from Renewable Feedstocks Ethanol and 1,3-Butanediol - CRADA 560 (Final Report)

1,3-butadiene is a commodity chemical currently produced from petroleum sources. Producing 1,3-butadiene from renewable resources will contribute to decarbonization, provide new green jobs, and reduce our dependance on oil. Development of multifunctional catalysts that are active, selective, and stable for this reaction has been an area of research and development. This effort reported here builds on our prior work for the 1-step conversion of ethanol to butadiene. The goal of the additional scope performed here was to accelerate the commercial deployment of sustainable butadiene production. We demonstrated that the PNNL Ag-based catalyst is significantly more active than the WWII-era catalyst when operated under the same conditions. A butadiene selectivity of 68% was obtained at 64% conversion for the production of butadiene from ethanol. It was found that ethanol feedstock is preferred over 1,3-butanediol feedstock to produce butadiene due to higher yield resulting in lower butadiene selling price (i.e., $\$$0.4-1.7/ lb). Production of 3.0 Liter of butadiene solution in hexane containing 100 grams of butadiene was achieved and delivered to Bridgestone for producing a butadiene-derived test piece.

09 BIOMASS FUELS↗

Magnetic Nanoparticle Extraction of Lithium from Produced Waters - CRADA 483 (Final Report)

The demand for lithium in the energy production industry is expected to increase sharply, development of simple and cost-effective techniques for lithium production and recovery from various lithium sources is essential. In this project, core/shell magnetic nanoparticles were successfully designed to selectively extract lithium from aqueous lithium sources as an extension of Pacific Northwest National Laboratory’s magnetic nanofluid extraction technology. The core/shell magnetic nanoparticles are composed of manganese oxide-based lithium ion sieve shells, which allow selective lithium uptake from brines with multiple coexisting ions, over iron oxide cores, which can respond to external magnetic fields for effective recovery and reuse of adsorbents from a liquid. The synthesized lithium ion-sieves and core/shell magnetic nanoparticles were characterized using several techniques to reveal their crystallinity and morphology. The lithium uptake properties of the lithium ion-sieves and core/shell magnetic nanoparticles were evaluated in terms of lithium adsorption capacity, removal percentage, selectivity, and cycling performance in simulated and natural brines. Magnetic properties of the core/shell magnetic nanoparticles were tested by measuring magnetic saturation, and magnetic response of colloidal solutions containing the core/shell magnetic nanoparticles was tested with permanent magnets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

RDPP: Accelerating Diversity in DOE Climate Science and Resilience Research (Final Report)

The scope of the project was set out to accelerate the inclusion of diversity into the Department of Energy (DOE) Earth and Environmental Systems Sciences Division (EESSD) relevant climate science and resilience research to inclusively advance solutions. The Project Objectives were to usher in equitable use-inspired climate-related research with underrepresented Minorities of which this project helped fund 7 HU graduate students work with the DOE (three of which will graduate in Spring 2025). The two key aims underpinning that core goal were AIM1: developing partnerships (18 organized engaged, see partners list) and AIM2: Developing capabilities (3 visits to DOE facilities, 5 DOE partners visits to HU, increased visiting faculty participation in BNL-DOE lab, secured 5 grants together totaling 1.2 million in funds for HU). The project objectives were highly successful as they were designed to ambitiously pull together DOE lab researchers with the long-standing and successful transdisciplinary climate science research programs of the PI and local DC groups. The major outcomes of this RDPP program will be in the new fundamentally inclusive partnerships with DOE and HU tasked to understand the urban-rural impacts due to climate change in the US, Eastern South Atlantic (ESA) Region, related to energy issues driven by heat stress and the water cycle. Overall, this project contributes to the DOE and science community vision for catalyze connections for project-ready underrepresented minorities (URMs) at a prominent HBCU to DOE projects supported by the Biological and Environmental research (BER) Program; particularly, the Earth and Environmental Systems Sciences Division (EESSD).

54 ENVIRONMENTAL SCIENCES↗

Methane Pyrolysis for CO2-free H2 and Carbon Nanomaterials - CRADA 576 (Final Report)

In this CRADA project we continued to develop the Pacific Northwest National Laboratory (PNNL) patent-pending Regenerable Catalytic Pyrolysis (ReCaP) process technology for producing CO 2 -free hydrogen (H 2 ) from inexpensive and domestically-abundant natural gas (NG), while simultaneously reducing H 2 ’s net production cost to $\$$1.0/kg through the sale of valuable crystalline solid carbon co-product. Producing clean hydrogen at this price is a DOE Hydrogen Energy Earthshot goal. This effort builds on our prior catalyst and processing advances made thermocatalytic decomposition of methane (TCD). The additional scope performed here accelerated the commercial deployment of TCD for CO 2 -free H 2 and valuable solid carbon nanotubes (CNT) co-product, by i) scaling up the production of CNT co-product using a fluidized bed reactor (25 g catalyst scale versus the 1 g catalyst scale demonstrated prior), ii) producing approximately 1 kg of CNT byproduct, produced via multiple cycles of TCD, carbon-catalyst separation, and catalyst re-synthesis, to enable the production of sufficient quantities of solid carbon so as to explore its market potential, iii) understanding the quality of the co-product CNTs, produced at larger scale, using advanced characterization, and iv) beginning to explore multiple promising high volume carbon product applications (e.g., aluminum and polymer composites, steel additive, and cement reinforcement applications). We are in discussions with Department of Energy and potential commercial partners to continue funding of this effort with the goal to facilitate eventual commercial deployment.

08 HYDROGEN↗

Advancing the Understanding of Cloud Microphysical Processes and Aerosol Indirect Effects in High-Latitude Mixed-Phase Clouds by Linking ARM Measurements with Climate Model Simulations (Final Report)

The key objectives of this project were to advance our understanding of cloud microphysical characteristics and aerosol indirect effects on mixed-phase clouds in high latitudes. To improve the representation of ice and mixed-phase clouds in Earth System Models (ESMs), we propose an integrated observation and modeling study of cloud macro- and microphysical properties, including spatial heterogeneities, mass partitioning between ice crystals and supercooled liquid water, effects of ice nucleating particles (INPs), and efficiency of secondary ice production (SIP), etc. Specifically, we took four main approaches in this project: (1) examining macro- and microphysical properties of ice and mixed-phase clouds based on in-situ and ground-based observations from multiple field campaigns funded by the U.S. Department of Energy (DOE) Atmospheric Radiation Measurement (ARM) program, including the Mixed-Phase Arctic Cloud Experiment (M-PACE), Indirect and Semi-Direct Aerosol Campaign (ISDAC), Ice Nucleating Particle Sources at Oliktok Point (INPOP), ARM West Antarctic Radiation Experiment (AWARE), Measurements of Aerosols, Radiation, and Clouds over the Southern Ocean (MARCUS), and Macquarie Island Cloud and Radiation Experiment (MICRE); (2) evaluating the DOE Energy Exascale Earth System Model (E3SM) simulations based on observations, particularly for ice and mixed-phase cloud microphysical properties; (3) examining the impacts of INPs on ice and mixed-phase clouds. Specifically, a series of comparisons were conducted using observations over the Arctic, Southern Ocean, and Antarctica, including comparisons between the lower and higher southern latitudes as well as comparisons between the northern and southern hemispheres. In addition, aerosol indirect effects from distinct sources of dust particles were examined; and (4) investigating the impacts of SIP. Ultimately, these results helped to improve cloud microphysics and aerosol-cloud interaction parameterizations in the E3SM model. Overall, the project provided improved understanding regarding various factors, including thermodynamic, dynamic, and aerosol conditions, on the micro- and macrophysical properties of ice and mixed-phase clouds in the high latitudes. Resulting analysis helped to provide an improved physical basis for refining the current cloud microphysics parameterizations related to ice and mixed-phase clouds in E3SM.

54 ENVIRONMENTAL SCIENCES↗

Wholly Sustainable, Cost-Effective Carbon Fiber-Nylon Compounds CRADA 592 (Final Report)

Carbon fiber composites have attracted considerable attention due to the potential for substantial mass savings, with many examples now implemented in the low-volume luxury car market. However, migration to higher volume applications has been hindered by: (a) high material cost, (b) high processing times, and (c) perception of low Sustainability. This project will address all three of these barriers: (a) carbon fiber material to replace aluminum in structural components at a cost penalty of no more than $5/Kg-saved (aka weight buy), (b) fitting into high-rate processes for automotive production like injection molding, and (c) end-to-end Sustainable material – based on post industrial waste carbon fiber and nylon 66 and ability to recycle end-of-life auto parts. The opportunity lies in combining DowAksa capabilities in carbon fiber manufacturing, resin chemistry intermediate production with the unique testing capabilities inherent within PNNL. The teams from PNNL and DowAksa held several meetings virtually and in-person in Michigan and at PNNL, including a lab tour at PNNL. Throughout, the teams discussed DowAksa material sources, commercially available recycled base materials, and preliminary material properties. The teams also engaged in multiple discussions and evaluations of potential automotive applications based on the ideas suggested by PNNL. The teams discussed several potential automotive applications in which recycled carbon fiber and recycled PA resin can be used. The PNNL team identified 38 cast aluminum components that can potentially be assessed for redesign using the DowAksa materials system. The PNNL team also identified 27 polyamide components. The teams discussed the lists and narrowed it down to a handful of applications that are exterior and interior to common vehicle architectures. The team also considered semi-structural and structural components and short-listed the highest potential candidates, such as cross-car-beam. The cross-car beam was considered to be highly suitable and potentially viable demonstration applications based on the properties of the materials as well as the weight savings potentials and the reduction in embodied energy by utilizing wholly sustainable materials, since both materials, carbon fiber and resin, were derived from recycled materials. The next step was to reach out to potential OEMs and/or Tier1s who were interested in exploring such technology for future applications. However, the project was terminated, and no further discussions or exchange of information took place. No new data were generated, including no IP and no publications.

36 MATERIALS SCIENCE↗

Preliminary Workforce Development and Environmental and Co-use Management Plans for a Floating Offshore Wind Platform - CRADA 609 (Final Report)

Pacific Northwest National Laboratory (PNNL) provided technical assistance to Glosten, Inc. and its affiliate, PelaStar, LLC to advance the development of their floating offshore wind (FOSW) platform. PNNL provided guidance and assessment in two areas that are important to address in the development of FOSW platforms: (1) workforce development and (2) environmental impacts and ocean co-use considerations. This work was funded by the U.S. Department of Energy’s (DOE) Wind Energy Technologies Office (WETO) through Phase 2 of the FLoating Offshore Wind ReadINess (FLOWIN) Prize. It should be noted that the Plans presented in this report are specific to the PelaStar tension-leg platform (TLP) and may not be applicable to all FOSW platforms. Workforce development and environmental/co-use impacts are highly dependent on the geographical region in which activities take place. At the request of PelaStar, PNNL focused on two regions where development may take place: the Gulf of Maine and Northern California. PNNL generated a preliminary Workforce Development Plan for PelaStar, which includes estimated job numbers and skillsets required to establish a workforce to manufacture, install, and operate their platform as part of FOSW projects. The Plan offers methods to increase diversity, equity, and inclusion practices when developing a new workforce and includes colleges and training centers for potential recruitment. Both positive and negative impacts to communities are evaluated, with potential mitigation strategies for reducing negative impacts. The structure of Community Benefit Agreements and Project Labor Agreements are discussed, noting the limitations of the role of a platform manufacturer versus the offshore wind developer. PNNL also drafted a preliminary Environmental and Co-Use Management Plan that serves as a guide to preparing an environmental assessment related to the installation and operation of PelaStar’s unique TLP design, including its potential ecological, socioeconomic, and emissions impacts. The Plan summarizes information on relevant regulatory requirements, potential impact producing factors, monitoring and mitigation measures, and physical and biological resources in the Gulf of Maine and Northern California. One of the primary perceived benefits of the PelaStar TLP is its reduced footprint due to its tensioned tendons versus catenary or taut moorings, but more research must be done as there are no studies on PelaStar’s TLP system to-date. The section also highlights ocean co-use considerations for PelaStar’s TLP system, specifically for fisheries, including existing perspectives, methods, examples, and limitations. The PNNL team established through this preliminary work and review of available literature and resources that there is not yet much research or planning around FOSW. With FOSW being a new industry, many of the findings and planning are adapted from fixed bottom offshore wind, which itself is only just taking off in the United States. More research is needed to establish best practices for workforce development and to assess environmental and ocean co-use impacts and mitigation approaches.

17 WIND ENERGY↗

Coal to Carbon Fiber (C2CF) Continuous Processing for High Value Composites (Final Report)

Coal tar is a condensed and recovered by-product of the coking of metallurgical coal for steel production. The heaviest fraction of distilled coal tar is an isotropic pitch largely used as a binder in the manufacturing of carbonaceous electrodes for primary aluminum smelting and in electric arc furnaces. Coal tar pitch offers high carbon yield upon carbonization. In this project, a process to convert the domestically sourced isotropic coal tar pitch, containing very low particulates (QI = 0.32 wt.%), to form flow-domain mesophase pitch amenable for melt spinning into precursor (green) fibers for carbon fiber, was developed and optimized. The final reproducible processing developed is reviewed in this report, along with several characterizations of the mesophase pitch. A final definition of the characteristics of a ‘spinnable’ mesophase pitch is presented. With this mesophase pitch, reproducible and stable multifilament melt spinning was developed, producing green fiber tows with filament diameters of approximately 20 m. The multifilament melt spinning was the most challenging aspect of the project and required the most effort. The best practices learned from this project for melt spinning are reviewed in this report. Once spun, the green fibers were oxidatively stabilized, carbonized and graphitized under inert gas atmosphere to form the final carbon fibers. Given the relatively high softening point of the mesophase pitch, no issues of interfilament fusion were observed during batch oxidation, and subsequent batch carbonization and graphitization went smoothly in all cases. An ~ 80 wt.% conversion of the green fiber mass to final carbon fiber was achieved. After graphitization, the carbon fibers showed high tensile moduli (most were ~ 600 GPa, or 87 Msi) consistent with commercially-available high-performance pitch-based carbon fiber. However, tensile strength and strain to failure were comparatively low. Further work to reduce defects in and on the fiber surfaces would increase these properties. SEM imaging of the graphitic fiber textures is presented herein. Rudimentary composites were fabricated from the carbon fibers and characterized showing similar modulus to baseline composites fabricated with commercial carbon fiber. Finally, a basic economic analysis was done showing the potential to increase the value of the isotropic coal tar pitch by up to 13.6 to 136 times based on a carbon fiber value of $\$$5/lb to $\$$50/lb, respectively. Moreover, the site case study suggests that the coal tar from the single integrated steel mill could supply production of up to 16 kt/yr of carbon fiber. Finally, a technological gap analysis was done which shed light on remaining technical challenges. These challenges included: recovery and utilization of condensates from the mesophase pitch processing, further advancing and increasing stability of the multifilament melt spinning processing, optimization of the oxidation processing, defect reduction for increased carbon fiber strength, and the development of a weaving process towards carbon fiber fabrics. To maximize the coal value chain, the primary objectives of this project were to (a) develop and scale efficient processing technology for producing melt-spinnable mesophase pitch from isotropic coal tar pitch, (b) clarify and simplify tedious continuous fiber processing technologies (particularly multifilament melt spinning of mesophase pitch) towards the efficient production of high performance carbon fiber, and (c) demonstrate and characterize representative composite parts derived from the final carbon fiber. Immense progress was made on all 3 objectives and is detailed in this report.

01 COAL, LIGNITE, AND PEAT↗

Two-Phase Cooling for High Packaging Density Planar Inverter: Cooperative Research and Development Final Report, CRADA Number CRD-15-00592

The project objective was to utilize two-phase heat transfer to enable compact and power-dense inverters. The high heat transfer capacity and near isothermal characteristics of two-phase cooling can enable higher power densities, reducing the size and cost of the power electronics system. This project focused on developing efficient, passive (no pump or compressor) two-phase cooling strategies that consist of an air-cooled condenser and evaporator. This report describes the modeling work conducted to design the evaporator and air-cooled condenser for a prototype inverter development work underway in the John Deere. Prototypes of the final evaporator and condenser designs were then fabricated via 3D printing for testing. Experiments on the evaporator confirmed that this component can meet the heat load and junction temperatures requirements for Si IGBT (insulated-gate bipolar transistor) inverter. Experiments with the air-cooled condenser were not possible due to leaks through the condenser walls.

33 ADVANCED PROPULSION SYSTEMS↗

Advanced Cellobiohydrolases (CRADA Final Report)

The purpose of the TCF project was to develop and transfer advanced Cel6A and Cel7A cellulase enzymes to Novozymes for testing on NREL provided DMR treated corn stover. In both cases, we developed advanced Cel6A and Cel7A enzymes that outperform the baseline T. reesei enzymes that are commonly available. The final milestone was to demonstrate an 80% glucan conversion on DMR treated corn stover with an enzyme loading of 10 mg/g glucan. This goal was achieved relatively early in the project and a new stretch goal for Novozymes became to test these enzymes in the Gen 1.5 yeast fermentation platform. The outcome was marginally successful due to temperature and pH optima mismatches between the enzymes (initially developed for use in a standard enzyme cocktail) and conditions suitable for yeast fermentation. Covid-19 and several re-organizations at Novozymes did significantly impact the project timeline, extending it to 2023. However, all of the original goals of the were successfully met or exceeded.

60 APPLIED LIFE SCIENCES↗

Essence2.0 Development and Deployment (Final Report)

The objective of the project was to take two core technologies that have been developed under the Recipient’s solid laboratory products and integrate them into a single CyberPhysical awareness platform and complete development on current field-tested prototypes that will extend the integrated capability of the platform. During the final development phase, the Recipient development team and its selected industry partners tested and hardened the platform to ensure resilient and secure operation of the integrated platform. The team also executed substantial field testing and established the framework for defining the organization and/or commercial infrastructure needed to sustain operations and provide readiness for a national scale deployment. The focus of the project was (1) the improvement, refinement, and deployment of technology for the detection of cyber-attacks on utility operational technology (OT) and information technology (IT) networks and assets, including Supervisory Control and Data Acquisition Systems (SCADA) systems; and (2) support for containment and remediation of adversarial threats and actions against those systems and environments.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

MC Formula Protocol for H35HF Fueling (CRADA Final Report)

The National Renewable Energy Lab (NREL), Frontier Energy, and the industry partners worked together to help SAE J2601-5 develop an H35 high-flow (HF) medium-duty (MD) and heavy-duty (HD) fueling protocol. The team upgraded NREL's hydrogen filling simulations (H2FillS) model to accommodate an MC Formula fueling (t-final) table generation capability by leveraging NREL's high-performance computing system. Based on protocol boundary conditions (e.g., allowable maximum flow rate, range of storage system size) set by SAE J2601-5, the team generated the fueling tables and then validated the reliability of those tables by installing them on NREL's HD dispenser and ZBT's H35HF dispenser and then performing H35HF fueling experiments. Through the validation process, this team certified that the fueling tables generated were reliable to install in commercial H35HF dispensers and then performed H35HF fueling of commercial MD/HD vehicles.

08 HYDROGEN↗

Multi-Scale Design And Advanced Manufacturing Of Seismic Metamaterials (CRADA Final Report)

As part of the Cyclotron Road program, METAseismic sought to investigate a multi-scale approach, both in terms of manufacturing and design, for seismic metamaterials with applications in the energy sector. Specifically, this project explored the feasibility of using nanofabrication to enable the incorporation of 3D nanostructured components into a mechanical metamaterial. These components were explored to increase the seismic resilience of our infrastructure to earthquakes, with the final aim of providing customized levels of protection for its components. This was envisioned as the base of a multi-scale design approach that consisted of using a multiplicity of metamaterial architectures ranging from the nano- to the meso-scale to address the stringent seismic design objectives of electric-power equipment.

36 MATERIALS SCIENCE↗