Electrically induced anomalous thermal phenomena in nanostructured wires

CHAPTER

Electrically induced anomalous thermal phenomena in nanostructured wires

7

Francesco Celania,b, Cesare Lorenzettia ISCMNS_L1, Ferentino, Italya INFN-LNF, Frascati, Italyb

It may not be elegant to start a chapter of a book on “Cold Fusion” by casting doubts as to whether the historical name attributed to this field of research still represents what is being observed in the laboratories around the word. Is this phenomenon actually nuclear fusion? In fact, three decades after the Fleischmann-Pons affair [1–3], certainties remain elusive, and the authors of this chapter do not want to give the impression of being close to an understanding of “Cold Fusion” phenomena. On the other hand, much progress has been made in the ability to reproduce and increase anomalous heat effects (AHE), a step which may prove fundamental for understanding its fundamental nature. Regarding the “Cold Fusion” strict definition of 1989, we want to believe that the jury may not remain out forever. But what have we been doing if after 30 years we do not yet know the answer to the simplest question? At the base of decades of development was an attempt to draw some generalization in a phenomenology that soon appeared overwhelmingly complex. And the generalization consisted mostly in the identification of the major parameters affecting the appearance and magnitude of AHE in hydrides and deuterides of transition metals and their alloys. We do not want to imply that we did not nurture an ambition to achieve an ultimate understanding of the underlying mechanisms, but simply that the experimental observations could not be made easily fit with the various models proposed over the years. On the other hand, this ample phenomenology could be compatible with a family of processes likely to be nuclear in nature, and possibly comprising “Cold Fusion” reactions after all, among many others. It is still an unproved opinion of the authors that the experimental conditions may drive the phenomenon toward one or more branches. It remains to be seen whether this “holistic” view of things will turn to be true, and if so, what the ultimate mechanism could be.

Historical background “Cold Fusion” is today seen as the legacy of the Fleischmann-Pons experiment. However, from an historical perspective, we must credit Fritz Paneth and Kurt Peters in the 1920s at the Chemical Institute of the University of Berlin and soon afterward to John Tandberg at Electrolux in Sweden for initiating this line of research. Interestingly, Paneth and Peters had chosen a noteworthy gas-phase approach, while Tandberg made attempts with an electrolytic system. Notwithstanding, the reason for starting from the very beginning of this long journey concerns some notable features of the Paneth-Peters experiment Cold Fusion. https://doi.org/10.1016/B978-0-12-815944-6.00007-5 # 2020 Elsevier Inc. All rights reserved.

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that we consider noteworthy for the work we initiated about seven decades afterward. In fact, in their 1926 article [4] they report the conversion of hydrogen to helium using colloidal palladium on asbestos, a material that already comprised a few of the key features needed to produce the anomalous effects that will be described in this chapter. The reader will not be surprised to know that the claims of Paneth and Peters were dismissed, and soon afterward their findings were retracted [5], maybe too soon—we would like to say. [For an investigation of these pioneering works, we want to bring to the reader’s attention the remarkable work of Steven Krivit [6].] In the early 2000s, our group increased the number of screening experiments based on palladium wires exposed to deuterium gas. Soon afterward, interesting results started to come from wires and plates made with palladium-yttrium alloys that were studied in electrolytic experiments, beginning in 1995. Neutron emissions and anomalous heat were observed in various experiments. The view that started to emerge at the time was that the surface features of palladium had an overwhelming role in predicting whether some anomaly would occur during the experiment. One of the key features turned to be the roughness/surface area, and possibly the presence of other elements such as alkaline metals and possibly silicates. At this moment in time, the analogy with the work of the German scientists started to take shape, in fact we could easily imagine that in their experiments they had already identified the need for superfine or nanosized particles of palladium on a support comprised of silicates and alkaline metals. Were they on to something after all? We cannot tell with certainty, but it is notable that the Cold Fusion community rediscovered the use of nanosized materials [7, 8] years after the Fleischman-Pons announcement, and nearly seven decades after the initial work of Paneth-Kurt. From our perspective, it was only in the years after 2000 that the need for an increased surface area and later also for the presence of certain elements became compelling. In fact, by this time we had collected overwhelming evidence of the importance of reduced particle size or increased effective surface area, together with the use of substances probably present already in the Paneth-Kurt experiment; judging by the effectiveness of these substances at increasing both the likelihood of occurrence of thermal anomalies as well as the magnitude of the anomalies. Before moving to the detailed description of the experiments that are the object of this chapter, we must mention the work of Francesco Piantelli, Sergio Focardi, and Roberto Habel at the Siena University (Italy) who in the early 1990s were pioneers of the gas-phase experiments with nickelbased materials [9]. These authors described multiple experiments and characterized the materials that seemed more likely to provide positive outcomes. Later, the first two authors measured also the presence of foreign elements on the surface of their active material [10] such as potassium, calcium, and others that later were recognized of extreme significance by the authors of this chapter. Having said that, soon after the reports of Piantelli-Focardi-Habel, our attention did focus on the cornerstone contribution of Yasuhiro Iwamura who while working for Mitsubishi Heavy Industries patented a process [11] for the transmutation of elements embedded in multilayer structures comprised of palladium and calcium oxide permeated with deuterium [12]. The work of Iwamura shows the importance of multilayer structures combined with substances featuring a reduced work function (i.e., the minimum value of energy required to remove an electron from a given surface), an approach that has been fundamental for the work at INFN-LNF in the following years [13].

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Gas-phase experiments The work in a gas-phase environment at INFN-LNF started in 1990 with the discovery of neutron emission in YBCO superconductors loaded with deuterium at high pressure. These measurements were performed at the Underground Laboratori Nazionali del Gran Sasso, which is characterized by extremely low values of background neutrons (about 1000 times lower than at sea level), and showed an increase of neutron counts mainly during the transitions of deuterated YBCO to the superconducting state [14, 15]. This work resumed at the beginning of the 2000s after a decade long investigation of electrolytic systems. The increasing evidence of successful experiments in gas phase reported by other researchers encouraged the initiation of a research program that could leverage on the long experience with wires in liquid-phase studies [16, 17]. In fact, a series of experiments with nanosized palladium were carried in the years 2000–2004. In an exemplary case [18], various types of palladium nanopowders were exposed to an atmosphere of deuterium at high pressure. These experiments did clearly show a modest source of anomalous heat correlated with the deuterium absorbed on palladium. This anomalous energy proved to appear only above a certain absorption threshold, similarly to the better known electrolytic experiments. With a view toward increasing the magnitude of the observed phenomena, a different approach followed soon afterward: 50–100-μm thick palladium wires were coated with multiple layers of silica glass and mixtures of thorium and strontium oxide [19] obtained, respectively, from the melting of a colloidal silica dispersion, and decomposition of the corresponding nitrates at about 1100 K. This treatment was based on the previous experience with electrolysis, where our group observed that in the most successful experiments, the palladium cathode presented a thin coating comprised of elements from the reactor (e.g., glass) and later other elements intentionally added to the electrolytic bath. These observations, supported by the reports of Iwamura on the effect of low work function material in multilayer structures, convinced us at experimenting with coated palladium wires in gas phase. Quite interestingly, the coating process developed by our group, produced a thin nanostructured layer of palladium oxide protected by a multilayer top coating comprised of silica glass and mixed oxides of thorium and strontium [19], elements positively associated with anomalous heat in previous electrolytic experiments. The concept being that after the reduction of the oxide in deuterium atmosphere, the wire would present a nanostructured spongy layer of palladium with an increased surface area directly exposed to low work function oxides. This multilayer coating proved also essential at preventing the sintering and densification of the palladium, a phenomenon that invariably leads to a suppression of the anomalous energy release. Modified palladium wires are then exposed to deuterium atmosphere and heated to 700 K passing a direct current through them. This new experimental setup [20] proved particularly successful and the released anomalous heat was two orders of magnitude higher than what measured with previous experiments with nanopowders, reaching values of 400 W/g of palladium. We could conclude that the current flowing in the palladium plays a fundamental role for the release of energy, possibly through the electromigration of deuterons, and their “confinement” in the lattice as consequence of the total voltage drop along the wires, as predicted by the model of G. Preparata and E. Del Giudice [21].

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It is at this moment in time that we could draw some guidelines that remained constant along the studies of the following years. In fact, the conditions that were identified for the occurrence of AHE could be summarized as follow: • • •

a need for rough, high surface metals (palladium); need to expose these surfaces toward low work function materials (i.e., strontium oxide, potassium oxide, calcium oxide, etc.); and need to flow an electric current along the metal to induce a voltage gradient.

This approach turned to be very successful and guided our experiments until the most recent developments.

Experiments with nickel alloys The substantially successful experiments with palladium wires still suffered a limited robustness as the wires tended to break quite frequently and the problem of wire deactivation due to the densification of the palladium surface was not completely solved. The most fruitful experiments were indeed those showing limited duration, possibly because the released energy (i.e., local hot spot) did play a role in the densification and consequent deactivation of the palladium surface. Furthermore, after the first positive results with palladium, we became increasingly worried of its cost and rareness both of which could substantially hinder the exploitation of the phenomenon in practical applications. Driven by the issue of palladium cost and the relatively short life of the wires, various solutions were attempted in the period 2007–11. Between them it is worth to mention the study of nickel wires coated with a thin palladium coating [22], similarly, to known solutions in the field of catalysis. In an exemplary test of this period, 200-μm thick nickel wires were coated with 1 μm of palladium; this approach has a positive impact on cost but also on the robustness of wires, whose durability was greatly increased. Also, we must highlight that this thin palladium coating enables the fast formation of nickel hydrides in the wire core also in conditions where nickel alone shows poor reactivity toward hydrogen or deuterium. Around this period (end of 2010), while still aiming at using materials with reduced cost, we were informed of the successful work of Brian Ahern with nickel-based powders occurred some years before in the United States. Having close experience with similar systems, we speculated on the possibility of a yet unidentified “trigger.” Among various possibilities, we became soon convinced of a possible role of a damaged thermocouple inserted within the powders (J-type or Fe-Constantan). Afterward, the work of Brian Ahern in the 1990s with nickel-copper multilayer materials was brought also to our consideration [23]. He describes several experimental designs comprising among others the use of alternating layers of nickel and copper in electrolytic experiments. At this moment in time, we could directly verify experimentally that Constantan alloys show a significant hydrogen absorption above 150°C (corresponding to a decrease of electrical resistance). While the whole captured our attention, it is only thanks to the work of Romanowski [24] on the remarkable activity of nickel-copper alloys as dissociation catalyst of molecular hydrogen that we eventually decided to initiate a series of experiments with these alloys.

Observation of thermionic-like behavior

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The chosen alloy was the “old” Constantan (Cu55Ni44Mn1) in form of 100–200-μm thick wires. These wires have then been heated in air by powerful electrical pulses, to produce a spongy oxide layer on its surface and, in later experiments, coated with mixtures of low work function oxides comprised of strontium and potassium [25]. Positive results came soon, in fact, when these wires were exposed to deuterium and heated above 700–1000 K, a significant AHE release was measured (although the results varied significantly in each experiment). While experimenting with various degrees of wire oxidation, we observed embrittlement of the wires and the separation of oxide flakes from the surface of the wire. This became a practical issue that we tried to limit by inserting the wire into a borosilicate glass fiber sheath. It was not a little surprising to discover that the use of this sheath positively affected the occurrence of AHE [26]. This effect was quite puzzling, at least until we stumbled upon the work of Irving Langmuir who a century earlier studied the interaction of atomic hydrogen and various surfaces. Between them he found an interesting weakly bound state of atomic hydrogen and borosilicate glass that under appropriate conditions could remain stable for a significant time, also at relatively high pressure and temperature [27–31]. The possibility that the synergistic effect of the glass fiber sheath in our experiment could be attributed to adsorbed atomic hydrogen or deuterium is intriguing, although still a speculative hypothesis.

Introducing iron Although the use of the glass fiber sheath brought an unexpected improvement in the magnitude of AHE (now approaching 100 W/g of wire material, when using 100-thick wires), we still observed a large variability in each experiment. Some parameter was certainly still out of control. A root cause investigation pointed toward the Constantan wires used in different experiments. We found that the wires producing the largest AHE were from a batch produced in the 1970s which contained about 0.5% iron, an element nearly absent in more recent Constantan lots. Also, the recent reports of Leif Holmlid [32–36] on the possible formation of ultradense states of atomic hydrogen and deuterium in iron-potassium catalysts made us feel confident that iron could play a role on AHE occurrence after all. From then on, we decided to add iron in the solution comprised of low work function compounds used in the coating of Constantan wires [37, 38] and later also for impregnating the glass fiber sheath. The use of iron in the low work function treatment of the wires and its sheath proved eventually to be fundamental in achieving consistency in AHE occurrence and magnitude, possibly through the formation of ultradense forms of atomic deuterium as postulated by Holmlid.

Observation of thermionic-like behavior In 2014, while running an experiment with multiple independent wires in the same reactor (in order to continue the tests should a wire fail), we observed that when passing a current and heating one of the wires (see Fig. 1, Scheme B) we observed a voltage and a current arising in the floating wire close by.

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Evolution of the experimental set up –30 V/–100 V DC

–30 V/–100 V DC

–

–

2–3 mm Wire

+

Anode

+

(A)

(B)

–30 V/–100 V DC

–30 V/–100 V DC

1–2 mm – Anode DC ±300 V

+

–

(C)

1–2 mm –

AC (sinusoidal) 50 Hz with bias ±600 Vpp

+

+

(D)

FIG. 1 Evolution of the electrical scheme of the wire reactor. The active wire (cathode) and the anode are exposed to a D2-based atmosphere.

This voltage turned to be a function of the wire temperature, gas pressure, and the distance between the wires [26], in accordance with the well-known Richardson law [39] for the thermionic emission at reduced pressure: W

J ¼ AT 2 e kT

where J is the current density emitted (A/m2), T is the emitter temperature (K), W is the work function (eV), k is the Boltzmann constant (J/K), and A is a constant (in the simplest form of the law). 1:5 In our experiments, the current follows a trend analogous to the Child-Langmuir law: B  S  Vd2 , where B is a constant, S is the anode surface, V is the voltage among anode and cathode, and d their distance. If on one hand, this behavior could be expected from a wire comprised of a coating of low work function compounds, on the other, it was surprising to measure it at the pressure range of our experiments (50–2000 mbar), where thermionic emission becomes negligible. Most importantly the occurrence of this current was correlated with the magnitude of AHE phenomena.

Effect of gas mixtures In all of the gas-phase studies reported above, the wires were exposed to a D2 atmosphere at a pressure that was varied between 2 bar and 50 mbar during the experiment. In fact, an initial high pressure enables the reduction of the oxides and the loading of the wire. When the loading and resistance of the wire reaches a plateau, the pressure is slowly reduced. In these conditions, we observe a rising AHE

Recent improvements in reactor design and AHE control

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with the increasing thermionic emission enabled by low pressure and high temperature. AHE tends to persist as long as the wire loading does not decrease excessively. In fact, AHE occurrence requires a relatively high loading of the wire, aided by high D2 pressure, while the thermionic emission of the wire occurs at a much lower pressure that generally leads to the wire “de-loading.” In order to boost and stabilize AHE occurrence overtime, without the need for very low pressure, which leads invariably to the de-loading of the wire, we experimented with mixtures of D2 and a noble gas (Xe or Ar). This causes a rise of the reactor internal temperature T due to the low thermal conductivity of the noble gas as well as a rise of the thermionic current (proportional to T2). Interestingly, other authors have observed a positive impact of noble gases on AHE occurrence during the oxidation of hydrogen chemisorbed on a variety of catalysts [40–42], this leads us to speculate whether the AHE occurrence may be due to, in both cases, a common underlying mechanism.

Recent improvements in reactor design and AHE control The observation of a macroscopic thermionic emission from the wire and its correlation with AHE occurrence and magnitude was soon followed by attempts to increase it by reducing the distance between the active wire and the anode, as well as by applying an external voltage bias, as shown in Fig. 1C. Both actions had a positive impact on AHE magnitude and provided the ultimate proof that the thermionic-like current and AHE phenomena are related. Figs. 2–4 show the most recent assemblage: a Constantan wire after being inserted in its glass fiber sheaths is impregnated with low work function compounds. The wire is then coiled and inserted into

Longitudinal section of the coil Steel tube cover aluminum foil Anode

Costantan coil extremity

Thermocouple

Costantan coil extremity Coil winding

Glass fiber sheath

FIG. 2 Assemblage of the Constantan wire in a cartridge configuration.

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Chapter 7 Electrically induced anomalous thermal phenomena

Scheme of the coils Stainless steel armored thermocouple type K Costantan coil extremity Coil winding Head of floating anode wire

Anode wire chrome nickel

Costantan coil extremity

Detail of costantan wire in its sheath

Nanostructured skin

Fused quartz + glass fiber hybrid sheath Costantan wire

FIG. 3 Schematic representation of the coil comprised of Constantan wire in its sheath impregnated with a low work function oxide, the nickel chrome anode and the thermocouple.

stainless steel “cartridges,” while the current collector (anode) is a straight nichrome wire inside an untreated sheath. While testing this configuration, we observed a notable effect on AHE of a positive bias for a pressure of D2 below 100 mbar, which is similar to results obtained by other researchers [43]. Above this pressure instead a negative bias seems to be more effective at increasing AHE. Puzzled by this last observation [44], we decided to evaluate the effect of an alternating current (AC) (Fig. 1D) around different values of bias with respect to the active wire. To date, this approach proved to be the most effective at stimulating AHE, especially at reduced pressure when a typical dielectric barrier discharge (DBD) is observed between the wires [44–46]. De facto, the occurrence of this discharge follows qualitatively the Paschen law [47] in terms of discharge

Recent improvements in reactor design and AHE control

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Reactor Ceramic frame support

V2

Anode wire inserted inside the coil

Thermocouple inserted inside the coil

V1

Coil power supply

V3

Glass vessel · 40 ¸ 34 mm - L 300 mm

Connection to the frame (grounding) Coil wire to ground

Head of floating anode wire

Support of the steel frame

V1— Platinum wire coil · 0.100 mm Thermocouple inserted inside the frame

V2— Constantan wire coil · 0.200 mm V3— Constantan wire coil · 0.350 mm

FIG. 4 Reactor configuration comprised of three cartridges (one for calorimetric calibration has a platinum wire in place of Constantan), and a detail of the treated constantan wire in its impregnated sheath.

voltage and electrodes gap. Notably, the pressure at which this discharge arises may be increased using D2-Ar or D2-Xe mixtures, while still providing a powerful stimulus to AHE release. As a matter of fact, in the current reactor configuration (Fig. 1D), we achieve 8–9 W of AHE when using 80 W of Joule heating of the Constantan under AC stimulation (50 Hz, up to 600 V). This value slowly decreases to 0 W if the stimulation is absent, but the application of about 0.3 W of a 50 Hz AC reverses the decline, leading to an additional 4 W of AHE. To appreciate the magnitude of this result, we note that this is an average of 10%–11% AHE with respect to the energy used for heating the wire, whereas we measure above 2700% AHE with respect the modest energy used to sustain the DBD. The information collected to date points toward a feedback mechanism of high intensity arising from the interaction of a DBD plasma with nanostructured surfaces comprised of various transition metals and their oxides as well as Group I and II elements. Furthermore, if we consider the thermionic emission of the active surfaces and its interaction with the DBD discharge, we may speculate about the

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Chapter 7 Electrically induced anomalous thermal phenomena

contribution of a nonneutral plasma, comprised of the elements in the electrodes. A research program is currently underway to explore the effects of various geometrical configurations of the electrodes, the bias between them, the AC frequency (from a fraction of Hz up to a maximum of 50 kHz), its waveform and duty cycle, as well as the ratio between the power input for the Joule heating of the wires and the J . power for sustaining the DBD discharge PPDBD

Conclusions This chapter is a very short summary of the two decades of investigations of AHE phenomena in nanostructured wires. The latest experiments show that this phenomenon is indeed closely related to thermionic emission, and plasma discharges (DBD) seems to be particularly effective at boosting its magnitude, pointing toward an electron mediated singularity [35, 36, 48–51]. On the basis of this, we believe that AHE occurrence can be triggered and controlled electrically, opening the possibility for further scale up toward practical applications. We understand that these statements may seem preposterous, but on the other hand we would point out that, if this is the case, it certainly would not be the first time that a practical application precedes the full understanding of a phenomenon. On the contrary, the fact that this phenomenon is now close to practical exploitation may eventually open up the human and financial resources needed to arrive at the comprehension of “Cold Fusion.”

Acknowledgments We are indebted to our Colleagues Giorgio Vassallo, Salvatore Fiorilla, Enrico Purchi, Misa Nakamura, Renato Burri, Stefano Cupellini, Pietro Cerreoni, Pierlorenzo Boccanera, Antonio Spallone who are coworkers and coauthors of the more recent papers. We cannot forget colleagues now sadly deceased, who made large progresses in the LENR-AHE field and with whom we had the opportunity and honor of collaborating: Piergiorgio Sona, Giuliano Preparata, Emilio del Giudice, Makoto Okamoto, Francesco Premuda, Naoto Asami, Paolo Marini, and Yoshiaki Arata. Last, we must thank Jed Rothwell for the kind revision of this chapter.

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