“Extraordinary Evidence” Replication Effort
In an article entitled “Extraordinary Evidence” published in Issue #19 of New Energy Times, Pam Boss and Stan Szpak of the US Navy’s SPAWAR lab in San Diego CA report the observation of copious pitting of CR-39 nuclear track detectors placed in close proximity to the cathode of their cold fusion cells. They claim that this pitting is evidence of nuclear activity in the cell. In December 2006, we joined The Galileo Project (TGP), a private collaboration among several labs organized by Steve Krivit, the editor of New Energy Times, to promote replication of the SPAWAR results. Our secret identity in this group was “Beta 2”.
We began our experimentation without the benefit of the official TGP protocol, using instead a similar protocol published by Boss and Szpak in “The Effects of External Fields on Surface Morphology of Codeposited Pd/D Films“. Our first experiments were highly successful. Our CR-39 “chips” were heavily pitted in the immediate vicinity of the cathode. This report details our efforts to determine the origin of these “SPAWAR pits”.
TGP Protocol
New Energy Times will make the TGP protocol is available to adults who will sign a liability waiver.
The TGP experiment consists of a fairly typical electrolytic cell run on the bench. It is an open (no recombiners) plastic cell with approximately 25 ml of electrolyte. The anode is 20 cm of 0.3 mm platinum wire and the cathode is several centimeters of 0.25 mm silver wire. The cathode wire is wrapped around the CR-39 chip to ensure that it is in contact with the chip. The electrolyte is 0.3M LiCl in heavy water plus 0.03M PdCl2 that is plated onto the cathode during the experiment. The current starts at 0.1 mA and is raised to 100 mA in several steps over the course of almost 3 weeks.
Initial Replication
We performed four experiments that closely followed the TGP protocol. Our first three experiments were based on the paper referenced above and the fourth was a replication of the TGP active cell (as opposed to the control cell). All four of these experiments produced results very similar to those reported in New Energy Times. Upon removing the cathode from the cell at the end of the 3 weeks, a cloudy area on the chip was visible in the area directly beneath the cathode. After etching, this cloudiness resolved into well defined and copious pits (approximately 106 tracks/cm2 ). The table below lists the four experiments, including links to logbook pages with more details about each (along with photographs). The logbook on cells A and B contain the most detail.
Experiment |
Protocol |
Electrolyte |
Magnets? |
SPAWAR pits? |
Near TGP |
Near TGP |
yes |
yes |
|
Near TGP |
Near TGP |
no |
yes |
|
Near TGP |
Near TGP |
no |
yes |
|
TGP |
TGP |
yes |
yes |
Magnetic Effect
The first version of the protocol we received for the TGP specified magnets on the active cell and no magnets on the control cell. The magnets are 2.5 cm square by 0.635 cm thick NdFeB magnets placed on the outside of the cell on the sides closest to the electrodes. It was reported in “Extraordinary Evidence” that an external field was necessary to create the SPAWAR pits. It can be seen from our initial replication effort that we did not observe any difference with the use of magnets. This observation was later confirmed by Pam Boss and the TGP protocol was changed accordingly. The control experiment using magnets was removed and replaced with one that used CuCl2 as the plating metal instead of PdCl2.
Location of magnets on the cell
Having successfully replicated the SPAWAR experiment, we began a campaign to determine the origin of SPAWAR pits. The New Energy Times article declared that the pits could only be due to nuclear particles. Compared to the often troublesome behavior of electronic detectors, CR-39 is generally considered to be an artifact-free method of detecting energetic particles. However, in the majority of applications, CR-39 chips are exposed only to air during use. In contrast, the SPAWAR experiment exposes the chips directly to the electrolyte and to the ions produced by the electrolysis in the vicinity of the cathode. This at least raises the possibility that chemical attack is involved in the making of SPAWAR pits.
Comparison to Alpha Particles Tracks
We exposed CR-39 chips to alpha particles under a variety of conditions. By varying the length of the air path between an Am-241 alpha source and the chip we were able to explore the effect of alpha energies from near zero (3-4 cm spacing) to ~5 Mev (nearly in contact). We also used other alpha emitters such as U ore placed in contact with the chip to observe the effects of highly oblique incidence.
We noted that the SPAWAR pits were strikingly different from the alpha tracks we had created from Am-241 and other sources in our lab.
All normal incidence 4 MeV alphas (400x)
SPAWAR pits (400x)
Under the same etching conditions, 4 MeV alphas produced tracks of about 7-8 microns, 1 MeV alphas produce a track of around 15 microns, and the SPAWAR pits averaged about 25 microns in diameter.
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The SPAWAR pits were also shallower and clumped together.Even when the CR-39 was exposed to enough alphas that the tracks overlapped, they did not have the same “soap bubble” appearance of the SPAWAR tracks.
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Additionally, none of the SPAWAR pits are elliptical. When a radioactive source is held in contact with the CR-39, tracks of all trajectories are recorded. However, even though the cathode wire is in contact with the chip in the electrolyte, we cannot discern any oblong shapes – all tracks appear to be nearly round.
Alphas from source held in contact (400x)
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We also noticed a phenomenon that did not match with our experience with alpha particles. After electrolysis, but before etching, one can see “evidence” of pits. It appears to be very small pock marks that later turn into well rounded tracks upon etching. In contrast, the path produced by an alpha particle cannot be seen with our microscope before etching.
- Also we observed two distinct types of SPAWAR pits. In the center of the damaged area, the pits tend to be dark and well-defined. At the edges, they become much lighter and shallower.
Light tracks on the edge of the cathode zone
Other Damage to CR-39
As part of our search for possible artifacts, we attempted to make CR-39 tracks using various mechanical means. We quickly discovered that mechanical damage often leads to round, track-like marks after etching. Any scratch on the surface would resolve itself into a chain of circular pits after etching. We were able to create various marks with sandpaper, needle points and simply by carrying around a chip in a pocket for a day.
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Mechanical damage to CR-39 |
Accelerating the Protocol
At the beginning of our campaign to explore this phenomenon, we experimented with shortening the run time. We ran at the maximum current, 100 mA, until the solution cleared (indicating that all the Pd had plated out). This took less than 48 hours. The growth on the cathode was rather different than that of the long running cell. The Pd was deposited in a thin film of “mud” across most of the CR-39 surface. In the long experiments, the Pd forms brittle dendrites that are more tightly clustered on the sliver cathode wire. However, these short runs did produce the SPAWAR pits on the areas where the Pd was in contact with the chip. This protocol was dubbed the “Beta 2 Impatient Protocol” or B2IP by Steve Krivit. We also tried another impatient protocol that lasted for three days. It started at 10 mA for 48 hours after which the current was increased to 100 mA for 24 hours. This produced a slightly more compact cathode deposit that covered less of the chip surface and still produced SPAWAR pits.
Experiment |
Protocol |
SPAWAR pits? |
B2IP |
yes |
Varying the Chemistry
Using the 3 day protocol, we ran a series of tests where parameters were held the same except for the electrolyte composition.Each test used the same molarity (0.3M) but different chemicals – HCl, LiCl, NaCl, KCl. The HCl electrolyte contained a slightly higher concentration of PdCl2 than the rest of the tests, but lower than the original replication tests. Our experiences had shown that the PdCl2 concentration did not affect the outcome. The test with HCl did not show pits, while the other 3 did.
Experiment |
Protocol |
Electrolyte |
SPAWAR pits? |
3 day run |
HCl |
no |
|
3 day run |
LiCl |
yes |
|
3 day run |
NaCl |
yes |
|
3 day run |
KCl |
yes |
In several cases, we also substituted light water for heavy water in the electrolyte. These tests showed no discernible difference in the quantity of SPAWAR pits produced. This seems quite significant as the nuclear behavior of deuterium, at least in high energy experiments, is significantly different than that of protium.
Experiment |
Protocol |
Electrolyte |
SPAWAR pits? |
TGP |
light water |
yes |
|
B2IP |
light water |
yes |
|
3 day run |
light water |
yes |
Plating metal changes
We also investigated the effect of metals other than Pd co-deposited on the cathode.We found that whenever the metal was deposited in a dense, dendritic mass on the cathode, pits were formed.When the metal formed a soft spongy mass, no pits were formed. This differentiation is especially apparent in the case of CuSO4. For the first experiment we ran with CuSO4 (exp. 6), we set the current at 100 mA and within 90 minutes, a soft mass had formed around the cathode and all of the color had gone out of the solution. The chip in this cell had no pits. However, when we ran the same electrolyte using the TGP current settings, a tight dendritic structure was formed and pits were formed. The last experiment (exp. 19) behaved slightly differently. As the current was increased, the structure of the cathode began to fall apart. No pits were formed even though the Cu had formed a dendritic structure in the early stages of the run.
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Dense dendritic structure | Soft spongy mass |
Experiment |
Protocol |
Plated Metal |
Structure |
SPAWAR pits? |
100 mA for 90 min. |
CuSO4 |
soft mass |
no |
|
TGP |
NiSO4 |
soft mass |
no |
|
11 | TGP | CuSO4 | dendritic | yes |
14 | 3 day run | NiCl2 | dendritic + soft mass | yes |
3 day run |
CuCl2 |
soft mass |
no |
|
TGP |
CuCl2 |
dendritic during the plating phase, became soft mass at higher currents |
no |
Isolating the CR-39 from the Electrolyte
We protected the CR-39 from contact with the electrolyte in various ways with varying degrees of success.When we were successful, we did not observe tracks (above the background).
For experiment 1, we glued a small piece of 6 micron Mylar with Devcon 2-ton clear epoxy to the bottom half of the CR-39 chip. The adhesive formed a complete seal around the edge of the Mylar. During electrolysis, the adhesive swelled and forced the cathode wire away from the chip surface. After removing the Mylar and etching the chip, faint tracks could be seen in the area not protected by Mylar and no tracks were visible underneath the Mylar.
For experiment 7, we used the same epoxy to glue a piece of 6 micron Mylar on the bottom half of the chip but only with dots of epoxy in the corners. We ran the experiment at 100 mA for 2 days (B2IP). We hoped that the Pd deposit on the cathode would not grow between the Mylar and the chip, but this was not the case. SPAWAR pits were found on the chip surface under the Mylar where Pd deposits had formed.
For experiment 10 and 16, we wrapped a piece of CR-39 in Mylar, forming a bag. The opening of the bag was above the electrolyte level and the entirety of the chip remained dry. Experiment 10 was run using TGP current settings and experiment 16 was run using our three day protocol. The Mylar bag in experiment 16 inflated noticeably during the run and forced the cathode wire away from the chip surface. Upon removing the bag from the cell, it was obvious that the bag was full of gas. However, the gas filled gap (of about 0.5 cm) between the cathode and the chip surface would not cause significant attenuation of any nuclear particles. The bag in experiment 10 did not inflate as much and the Mylar, and thus the cathode wire, remained nearly in contact with the chip. After etching, both of these chips exhibited minor mechanical damage – we had sanded the edges to ensure that the Mylar would not be punctured. This caused some scratching of the surface which produced track-like damage similar to that described above. Despite this complication, we observed orders of magnitude fewer tracks than in our replication experiments and no spatial correlation between tracks and the location of the cathode.
Richard Oriani reported positive results with a cell in which the CR-39 was located outside the cell and separated from the electrolyte by a Mylar window. We adopted a similar design for our next experiments. We machined an opening in the side of the cell and glued Mylar film over it (using Devcon 2 ton clear epoxy). The chip was held in contact with the outside of the window and the cathode wire was positioned against the inside. We ran four experiments with this set-up. The first three used near-TGP electrolyte. One ran for 3 days, the other two for the full three weeks. We used magnets on one of the full TGP runs because at this time Ludwik Kowlaski had reported negative results when not using magnets. Our final test used an electrolyte suggested by Oriani – 0.022 gm of Li2SO4 per mL of light water. Note that this electrolyte contains no metal to be plated out and that the cathode was nickel wire. Oriani reported positive results with this arrangement.
The chip in the first of these experiments, 24, was scratched too badly from sanding to get an accurate track count, but clearly there was no copious distribution of tracks as seen in our replication experiments. The other three tests, 25, 26, and 27, showed only background track densities.
We performed background counts on both sides of 8 chips. The average was approximately 100 pits/cm^2. According to the reports of others, this number is somewhat high. We attribute this to fact that our CR-39 is 4 years old.
Experiment |
Protocol |
Electrolyte |
Notes |
TGP | TGP | Mylar covered half | |
B2IP | TGP | Mylar covered half | |
10 | TGP | TGP | bag |
16 | 3 day | TGP + light water | bag |
3 day | TGP | window | |
TGP | TGP | window | |
26 | TGP | TGP | window – with magnets |
27 | 100 mA for 3 days | LiSO4 | window – nickel cathode |
Other Observations
Accelerated Etching
During our investigation, we observed one effect that was clearly caused by chemical damage to the CR-39.We carefully measured the thickness of the CR-39 at various stages of the experiment.The thickness did not change after exposure to the electrolyte.However, when chips that had been exposed to the electrolyte for weeks were placed in the etching solution, the etch rate was unusually high at first, but returned to a normal rate after a few hours. Normally, CR-39 will etch at a rate of 1.5 microns per hour using TGP etch parameters.However, these chips lost 80 microns in the first 1.5 hours.The cathode wire and associated Pd deposits provide some degree of protection from this effect. In our replication experiments, this area was only etched about 15 microns during this same time and therefore a perceptible ridge formed underneath the cathode.
It should be noted that the expected range of 5 MeV alpha particles in CR-39 is approximately 40 microns, considerably less than the thickness of CR-39 removed from the bulk of the chip in many of these experiments.
Nickel Cathode
Pam Boss reported (during the March 2007 APS meeting) that a nickel cathode in the absence of an external electromagnetic field would not produce SPAWAR pits. However, we observed moderate densities of SPAWAR pits when using this arrangement. We also performed an experiment with a Ni fibrex cathode and no Pd in the electrolyte (or any other plating metal). The nickel fibrex was intended to mimic the dendritic palladium. This test did not produce SPAWAR pits.
Experiment |
Protocol |
Electrolyte |
Cathode |
SPAWAR pits? |
TGP |
TGP |
Ni wire |
yes |
|
18 | B2IP | light water and LiCL | Ni fibrex | no |
Conclusions
Our results do not provide a positive identification of the origin of SPAWAR pits.However, they do show that chemical origin is a distinct possibility and therefore that nuclear origin is not a certainty. The accelerated etching rate observed for CR-39 that has soaked in TGP electrolyte for several weeks proves that there is a chemical interaction.The observation that SPAWAR pits are visible before etching shows that they are unlike the tracks made by ionizing particles.The observation that SPAWAR pits are stopped by a 6 micron Mylar film is consistent with a chemical origin but only proves that they cannot be due to nuclear particles which would penetrate such a barrier (e.g. alpha particles of energy >1 MeV).The rest of our observations, such as the invariance of the result when the electrolyte is changed from heavy water to light water, are less conclusive but are still consistent with chemical origin of SPAWAR pits.
It has been suggested that SPAWAR pits are a mixture of chemical and nuclear pits.This is a difficult hypothesis to evaluate.Frankly, the idea of trying to identify pits which “look nuclear” is not very appealing from an objectivity standpoint.