Condensed Matter Nuclear Reactions in Nano-Materials

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This presentation, delivered by Lawrence P. Forsley at the ARPA-E Workshop on Low-Energy Nuclear Reactions (LENR) in October 2021, reviews experimental evidence, material systems, and diagnostic requirements for anomalous heat effects in nano-materials. It examines excess power generation across various metal nanoparticle and thin film systems loaded with hydrogen isotopes, addressing the role of magnetism, experimental needs, and pathways toward scaling and commercialization.

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Condensed Matter Nuclear Reactions in Nano-Materials ARPA-E Workshop on Low-Energy Nuclear Reactions October 21-22, 2021 With additional backup slides that weren’t presented at the Workshop. Workshop presenters with additional details are in “[…]”. Lawrence P. Forsley CTO, GEC Deputy PI, NASA Lattice Confinement Fusion Project Research Fellow, University of Texas, Austin, Nuclear Engineering Teaching Laboratory Co-PI, Naval Surface Warfare Centers [email protected] V 2.0 Page 1 • Pd used as a hydrogen gas separator/purifier. [Benyo] • Has a unique electronic structure: 4d10 <> 4d95s1 : paramagnetic and ferromagnetic states • Pd will load H/D, e.g. PdDx to x < .56, α >> β phase • Fleischmann and Pons used electrolysis to bulk load x > .9, but takes days to weeks to load • McKubre has shown bulk PdDx, x > .86 for onset of LENR heat. [McKubre] • Szpak showed electrolytic Pd/D co-deposition rapidly loads x ≈ 1.0 [Mosier-Boss] • SEM analysis shows a size range from nm to μm scales • Miles and Barham: watts thermal • Storms suggests nm fissures provide a nuclear active environment (NAE) • Staker observed and created Pd Super-Abundant Vacancies (SAV) allowing high-densities of hydrogen isotopes • DeChiaro modeled itinerant ferromagnetism and SAV • Pianitelli, Ni, Takahashi, Celani and others have found NiCu exhibit excess heat with hydrogen Table of Excess Heat Results: - Arata: Excess Heat: 10 Wt | Duration: 12 weeks | Mass: 3 g | Material: Pd-black nanoparticles w/ D2 | Wt/g: 3.3 | Joules: 73 MJ - Takahashi: Excess Heat: 226 Wt | Duration: several weeks [5] | Mass: 505 g | Material: CuNi nanoparticles w/ H2 | Wt/g: 0.45 | Joules: 683 MJ - Ahern: Excess Heat: 21 Wt | Duration: 5 days | Mass: 5 g | Material: PdNi nanopowder w/ D2 | Wt/g: 4.2 | Joules: 9 MJ - Celani: Excess Heat: 18 Wt | Duration: 5 hours | Mass: 0.45 g | Material: CuNi nanolayers w/ H2 or D2 | Wt/g: 40.0 | Joules: 324 kJ LENR requires multiple science and engineering disciplines. Questions remain: Scaling, self-operating, reaction products, life-time, triggering, mechanisms. • Hydrogen isotope spillover1 • Three stages: adsorption, dissociation, absorption • Pd will do all three, Cu the first two2, Ni absorbs H at > 200 °C • Materials • Pd, Pd3Ni7, Pd1Ni9, Cu3Ni7, Cu55Ni44Mn1 often in ZrO2 • Structures • Nano-scale structures, 2 – 20 nm • Fabrication • Spin-cast powders3 [Narita] • Multi-layers4,5 [Narita] • Co-deposition6 [Mosier-Boss & Barham] • Double cathode7 [Nagle & Narita & McKubre] • Operation • H2 or D2 gas or electrolytic loading and/or flux [Benyo & McKubre] Less appreciated: The roles of magnetic order and disorder • Bulk Ni Curie Point ≈ 354 °C, • Nanoparticle Curie Point T < bulk material • Pd is paramagnetic • ZrO2 in contact with Pd strains the lattice induces ferromagnetism8,9 • PdH and PdD are superconductors10 • Superconductor YBCODx is LENR Active11 Is LENR a topological phenomena? Is magnetism a key? Excess Heat: Pd, PdNi favors D2 Ni, CuNi favors H2 Oxides often present Comparisons: 10^4 eV/H (Iwamura)4 10^3 – 10^5 eV/D (Takahashi)12 4.88 eV/H (oxidation: H2O) References: 1 Spillover of Adsorbed Species, Studies in Surface Science and Catalysis, 17, ed. G.M. Pajon, S.J. Teichner and J. E. Germain (editors) Elsevier (1983). 2 A. Crucq, et al., “Hydrogen Spillover from Ni to CuNi Alloys”, Studies in Surface Science and Catalysis, 17, (1983) 137-147. 3 B. Ahern, “Program on Technology Innovation: Assessment of Novel Energy Production Mechanisms in a Nanoscale Metal Lattice”, EPRI Technical Report Update, 1025575, EPRI, Palo Alto, CA (2012). 4 Y. Iwamura, “Heat generation experiment using nano-sized metal composite and hydrogen gas”, Cold Fusion: Advances in Condensed Matter Nuclear Science, Elsevier, ed. Jean-Paul Biberian (2020) 157-165. 5 F. Celani and C. Lorenzetti, “Electrically induced anomalous thermal phenomena in nanostructured wires”, Cold Fusion: Advances in Condensed Matter Nuclear Science, Elsevier, ed. J-P (2020) 101-114. 6 Y. Arata and Y-C. Zhang, “Observation of Anomalous Heat Release and Helium-4 Production from Highly Deuterated Palladium Fine Particles”, Jpn. J. Appl. Phys. 38 Pt. 2, No. 7A, (1999) L 774–L 776. 7 US Patent # 8,419,919, “System and Method to Generate Particles”, (April 16, 2013). 8 L.F. Dechiaro, L. P. Forsley, and P.A. Mosier-Boss, “Strained Layer Ferromagnetism in Transition Metals and its Impact Upon Low Energy Nuclear Reactions”, JCMS, 17, (2015) pp. 1-26. 9 D.L.R. Santos, et al, ”Spin pumping and interlayer exchange coupling through palladium,” Phys. Rev. B 88 (2013) 054423. 10 US Patent # 7,033,568, “High Tc palladium hydride superconductor” (April 25, 2006). 11 Lipson, A.G., et al., “Generation of the products of DD nuclear fusion in high-temperature superconductors YBa2Cu3O7-deltaDy near the superconducting phase transition.” Tech. Phys., 40 (1995) p. 839. 12 Takahashi, et al., “Enhancement of Excess Thermal Power in Interaction of Nano-Metal and H(D)-Gas”, Proceedings of JCF20 of JCFRS, preprint (2020). Arata (nano-Pd black/D2 double cathode)1 [Narita & Nagle]: • Material: 20 nm diameter, Pd black, 3 g • Triggering: Electrolytically loaded, [1 kbar D2] • Excess Heat: 5 – 10 W, continuous • Duration: 12 weeks Celani (CuNiMn & oxide nanolayers, D2 or H2)3: • Material: Mod. Constantan [Cu55Ni44Mn] w/ oxides, 0.45g4 • Triggering: Thermal, 50 Hz A/C stimulation, 600 V, heating • Excess Heat: 18 Wt with 99.7 W Joule heating • Duration: 5 hours Ahern (nano-PdNiZrO2/D2)2: • Material: 10 nm diameter PdNiZrO2 powder, 5 g • Triggering: Thermal, T > 360 °C. [Ni Curie Point, 358 °C] • Excess Heat: ~ 21 watts, not repeated • Duration: 5 days, terminated for evaluation Takahashi5,6 (PdNiZrO2 & CuNiZrO2 nanopowders) [Narita]: • Material: PdNi10/ZrO2 (PNZ10), Cu3Ni7/ZrO2 (CNZ7) 505 g • Triggering: Thermal? • Excess Heat: PNZ10rr 186 W/kg5 D2; CNZ7rr 226 W/kg5 H2; reaction energy5 (η-value) 10^3 to 10^5 eV/D • Duration: several weeks References: 1 Y. Arata and Y-C. Zhang, Japan J. Appl. Phys. 38 Pt. 2, No. 7A, (1999) L 774–L 776. 2 B. Ahern, EPRI Technical Report Update, 1025575 (2012). 3 F. Celani and C. Lorenzetti, Cold Fusion: Advances in Condensed Matter Nuclear Science, Elsevier (2020) 101-114. 4 Personal communications with Celani during and after the ARPA-E Workshop. 5 A. Takahashi et al., JCMNS, 33, (2020) 14–32. 6 A. Takahashi, et al., Proceedings of JCF20 of JCFRS, preprint (2020). Table of Related Experiments: - Ahern1: Nano-material: PdNi/ZrO2, nanopowder | H/D Isotope: D2 | Country: US | Year: < 2012 - Arata2 [Narita, Nagle, McKubre]: Nano-material: Pd black nanopowder, double cathode | H/D Isotope: D2 from D2O | Country: Japan | Year: < 1997 - Barham [Barham]: Nano-material: Fast Pd/D Co-deposition | H/D Isotope: D2 from D2O | Country: US | Year: < 2021 - Beiting3: Nano-material: ZrO2NiPd nanopowder | H/D Isotope: H2 | Country: US | Year: < 2017 - Celani4: Nano-material: NiCuMn (Fe) oxide nano-layers | H/D Isotope: H2, D2 | Country: Italy | Year: < 2014 - Iwamura5 [Narita]: Nano-material: CuNi, nanolayers | H/D Isotope: H2, D2 | Country: Japan | Year: < 2018 - Kitamura6 [Narita]: Nano-material: Pd, ZrO2 nanopowder | H/D Isotope: H2, D2 | Country: Japan | Year: < 2009 - Miles7,8 [McKubre]: Nano-material: Pd/D Co-deposition (ammonia complex) | H/D Isotope: D2 from D2O | Country: US/Japan | Year: < 1999 - Snoswell9: Nano-material: Ni nanopowder | H/D Isotope: H2? | Country: Australia | Year: < 2012 - Storms10 [Nagle]: Nano-material: compressed Ni or Pd micropowders | H/D Isotope: H2, D2 | Country: US | Year: < 2021 - Swartz11 [Nagle]: Nano-material: PdNi-ZrO2, PdZrO2 nanopowder | H/D Isotope: D2 | Country: US | Year: < 2017 - Takahashi12 [Narita]: Nano-material: PdNi-ZrO2 and CuNi-ZrO2 nanopowder | H/D Isotope: H2, D2 | Country: Japan | Year: < 2013 References: 1 B. Ahern, EPRI Technical Report Update, 1025575 (2012). 2 Y. Arata and Y-C. Zhang, Jpn. J. App Phys. 38 Pt. 2, No. 7A, (1999) L 774–L 776. 3 E. Beiting, Aerospace Report No. ATR-2017-01760 (2017). 4 F. Celani, et al, JCMNS, 33 (2020) 1-28. 5 Y. Iwamura, Cold Fusion: Advances in Condensed Matter Nuclear Science (2020) 157-165. 6 A. Kitamura, et. al., Phys Lett A., 373(35), (2009) 3109-3112. 7 S. Szpak, P.A. Mosier-Boss, and M. H. Miles, Fusion Technology, 36 (1999) 234-241. 8 M. H. Miles, JCMNS, 13 (2014) pp 401-410. 9 Communication between B. Ahern and M. Snoswell, EPRI Report 1025575, p. 4-7, ref [30]. 10 E. Storms, ICCF-23, Xiamen, China (2021). 11 M. Swartz, JCMNS, 22, (2017) 35-46. 12 A. Takahashi et al., JCMNS, 33, (2020) 14–32. • Experimental Improvement (minimum sensitivity to detect rare products or swamped by background) • High Temperature Calorimetry • Range 30 °C – 500 °C, > 100 mW sensitivity • Nuclear, HPGe, RF, IR, UV diagnostics, (> 5 sigma over background) • in situ and adjacent to operating devices: watch out for cosmogenic muons and neutrons, natural BG radiation • Real-time energetic particle spectroscopy preferred: TOF if possible (gold standard for particle energy) • Witness materials with HPGe in situ, post HPGe monitoring and material assays • Material assay and limitations (interferences) Indicates the roles of various structures and materials, contaminants • SEM/EDX: wide area FOV, qualitative surface structure, limited elemental sensitivity (parts per ten thousand) • ICP-MS: quantitative, isotope specific, but multi-ion (e.g. Hn+, Ar feed gas) complexes, ppb-ppm • TOF-SIMS: isotope specific, qualitative, small FOV, ppb-ppm • NAA/PGNAA: quantitative, isotope specific, limited isotope detection, ppt-ppm • Alpha/Beta Liquid Scintillator Spectrometer: tritium, activation products, limited energy resolution, ppm • Patent Rights • USPTO treats LENR heat as “perpetual motion”, hence, unpatentable, yet necessary for investment and commercialization • Licensing • NRC and IAEA providence • Patents and patent interference • Health Physics Concerns • Nanoparticles, especially non-encapsulated Ni-based nanopowder and their escape via seal and valve seat fouling • Self-generated B and EM fields • Bremsstrahlung radiation • Neutron radiation Fundamentally, there is a need to run longer with simultaneous diagnostic measurements to correlate effects. • Diagnostics: - Nuclear: HPGe x-ray/γ 10 keV – 3 MeV or LaBr3 or NaI(Tl) [in decreasing energy resolution, but increasing detection (size) efficiency] - CR-39, in situ (< 50 °C), external [Detect both charged particles and neutrons, speciation and energy resolution] - Neutron scintillators for time resolved (< 200 nsec resolution) [neutron counting and/or spectroscopy] - Plastic/glass scintillators (in situ ion counting), (< 20 nsec resolution) [Detect charged particles] - Silicon Barrier detectors (200 keV – 20+ MeV ion detection) [Resolve charged particle energy and nuclear exit channel] - Optical: Fiberoptic feedthrough for spectroscopy, digital camera [Resolve spectra and spatial relationship of “hot” spots] - IR: NIR, MIR 1 μm – 12 μm range, notch-filters [Detect down-shifted bremsstrahlung, non-black-body radiation] - RF: 100 kHz – 10 GHz, with H/V Stokes parameter polarization [Detect magnetic effects] - Low temperature Calorimetry: 25 °C – 100+ °C, < 50 mWt sensitivity [suitable to aqueous electrolysis] - High temperature Calorimetry: 100 °C – 500+ °C, 200 mWt sensitivity [suitable to high temp gas operation] • Experiments: - Electrolytic co-deposition with fractal surface nano-particles: - PdCl2, LiCl electrolyte with Pt, Ag, Au cathodes, e.g. patent1 and Trackers STEM Protocol™ - Operation > 100 °C, approaching 150 °C, 15 bar - Slow, ramped up V/I for 2+ weeks [determine effect lifetime by running longer] - Fast, constant or ramped down, V/I, for 2 weeks [determine effect lifetime by running longer: Letts/Dahlgren/HIVER] - Gas Cycling of nanopowders and nanolayers: - nanopowders and nanolayers, H2, D2, HD, He, Ar - Operation > 200 °C, << 1 bar (often less than 100 torr) - Double Cathode with nano-powders: - nano-powders placed within sealed, electrolyzed Pd tubing for high loading • Triggers: - Low Energy: thermal, RF, laser, gas cycling/flux - High Energy: neutron, e-beam, bremsstrahlung 1 US Patent 8,419,919, “System and Method to Generate Particles” (April 16, 2013) • Drive towards LENR/Lattice Confinement Fusion (LCF) Scaling • Self-sustaining operation • Establish LENR/LCF lifetime, power output/gm, available Delta T • Thermal or direct power conversion • Path to Commercialization: Watts, kW or MW? • Investigate multiple LENR/LCF-capable experiments: “Lab rats” • Develop predictive modeling of materials and nuclear effects • Setup cooperative teams: share knowledge and findings! • Publish results in “Tier 1” journals • Recognition by scientific and engineering communities • Acceptance by government agencies and universities • Harness private sector funding • Beyond ARPA-E Program • Multi-agency supported LENR/LCF Program • Foreign entity participation • Develop university and student support to create the technology workforce • Deploy the technology Catch-22: Government agencies won’t recognize LENR unless Tier 1 journals publish results. These journals won’t publish results unless LENR is recognized by these agencies.1 1 P.A. Mosier-Boss, L.P. Forsley and F.E. Gordon, “How the Flawed Journal Review Process Impedes Paradigm Shifting Discoveries”, JCMNS, 12 (2013) 1-12. Backup Slides Backup material wasn’t presented at the ARPA-E Workshop. However, both Takahashi’s and Iwamura’s research were discussed by Narita in the Workshop. Page 9 Observations: PdNi10/ZrO2 (PNZ10) Cu3Ni7/ZrO2 (CNZ7) melt-spun, calcinated or recalcinated nano-powders. Calorimetry1: • 80–400 Wex/kg excess thermal repeatable for several weeks at elevated temperature ≈ 300 °C with re-calcined PNZ-type with D. • Specific reaction energy2 (η-value) 10^3 to 10^5 eV/D. • 50-140 Wex/kg obtained by CNZ-type with H • 50–70 Wex > two weeks by 505 g CNZ7r (re-calcined) Neutron Counting1: Neutron yield: 0.1 n/J: 1.0 × 10−13 of bare d–d fusion. AHE is largely aneutronic! Diagram Description: Kobe University C system AHE calorimetry schematic showing oil-flow-calorimeter system with flow-rate-monitors and dual heaters (W1, W2). References: 1 A. Takahashi et al.,” Latest Progress in Research on AHE and Circumstantial Nuclear Evidence by Interaction of Nano-Metal and H(D)-Gas”, JCMNS, 33, (2020) 14–32. 2 A. Takahashi, et al., “Enhancement of Excess Thermal Power in Interaction of Nano-Metal and H(D)-Gas”, Proceedings of JCF20 of JCFRS, preprint (2020). Experiment & Six-layer nano-composite setup: Diagram shows Ni/Cu multilayers (Ni 14 nm / Cu 2 nm repeated on Ni 0.1 mm substrate) in chamber with infrared radiation thermometer, heater, and Gamma-ray NaI(Tl) detector. Excess power (W) vs heater temperature (°C) chart shown for 3, 6, 8, and 15 layers. Released excess energy per hydrogen (Six Layers Cu 2nm, Ni 14nm): - Absorbed H [mol]: 7.3 × 10^−4 - Absorbed number of H: 4.4 × 10^20 - Total excess energy [J]: 1.1 × 10^6 - Excess energy per hydrogen [J/H-mol]: 1.5 × 10^9 - Excess energy per hydrogen [eV/H]: 1.6 × 10^4 Total Excess: 1.1 x 10^6 J Excess Energy: 1.6 x 10^4 eV/H Comparisons: 10^4 eV/H (Iwamura) vs 10^3 – 10^5 eV/D (Takahashi) vs 4.88 eV/H > H2O (oxidation) 1 Y. Iwamura, “Heat generation experiment using nano-sized metal composite and hydrogen gas”, Cold Fusion: Advances in Condensed Matter Nuclear Science, Elsevier, ed. Jean-Paul Biberian (2020) 157-165. Ahern (2011, nanopowders)1: “…nanotextured nickel in the presence of hydrogen gas, tests of similar materials conducted under this EPRI research grant produced only milliwatt-scale thermal power releases… one experiment, a 21-watt release was observed but not replicated.” Reproducibility depended upon triggering by raising temperature above 360 °C. The excess heating rate output did not exceed 200 milliwatts. …thermal power estimated to be 100 milliwatts per degree C of elevation above the value of the outer resistance thermal device (RTD)….10-nm nickel powder from Quantum Sphere Corp. The inner RTD was 208 °C hotter than the outer RTD (533 °C versus 325 °C) …~ 21 watts from 5 grams of nanopowder… maintained for five days… terminated for evaluation. Issue: Is heat produced by global collapse of magnetic order at Curie Point or are reactions initiated by the same? It appears that the excess power over time exceeds the magnetic field collapse energy storage. Celani (< 2020, nanolayers)2: …the successful work of Brian Ahern with nickel-based powders and having close experience with similar systems, we speculated on the possibility of an unidentified “trigger”… AHE can be triggered and controlled electrically, opening the possibility for further scale up toward practical applications…we achieve 8–9W of AHE when using 80W of Joule heating of the Constantan [Cu55Ni44Mn1] under AC stimulation (50 Hz, up to 600V). Constantan wires producing the largest AHE were produced in the 1970s which contained about 0.5% iron, nearly absent in more recent Constantan lots. Holmlid reported the possible formation of ultradense states of atomic hydrogen and deuterium in iron-potassium catalysts. Takahashi3,4 (nanopowders) [see Narita overview of Japanese research]: PdNi10/ZrO2 (PNZ10) Cu3Ni7/ZrO2 (CNZ7) melt-spun, calcinated or recalcinated nano-powders. 80–400 W/kg excess thermal Wex repeatable for several weeks at elevated temperature ≈ 300 °C with re-calcined PNZ-type with D3. Specific reaction energy4 (η-value) 10^3 to 10^5 eV/D. 50-140 W/kg Wex obtained by CNZ-type with H and 50–70 W continued > two weeks by 505 g CNZ7r (re-calcined) Neutron yield: 0.1 n/J: 1.0 × 10−13 of bare d–d fusion. AHE is largely aneutronic! References: 1 B. Ahern, EPRI Technical Report Update, 1025575 (2012). 2 F. Celani and C. Lorenzetti, Cold Fusion: Advances in Condensed Matter Nuclear Science, Elsevier (2020) 101-114. 3 A. Takahashi et al., JCMNS, 33, (2020) 14–32. 4 A. Takahashi, et al., Proceedings of JCF20 of JCFRS, preprint (2020).

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