Regarding the insulation issue, keep in mind that alumina becomes conductive starting at around 700°C. Any thermocouples in contact with the insulation will be affected when that happens. It can be mitigated by isolation of the measurement circuit, for example a battery-powered meter would probably be OK, but any computer system used to record temperature data must be fully isolated from the heater mains connection.
RobertBryant Nicely done!
I suspect the discrepancy can be somewhat reduced by adjustment of the convective heat transfer coefficient. You used h = 4 which seems a bit low. In the example here 4.3 is used, and I've seen other examples using 5. The actual number would have depended on the ambient air temperature, pressure and humidity when the cell measurements were done.
The emissivity of stainless steel is another difficult parameter to specify. It will surely be lower than 0.83 for the polished reactor surface, for which 0.5 would be more typical. But there are what appear to be sections of film or coating on the tube, with unknown properties. Some exotic high-emissivity surface treatment might make the reactor Ɛ = 0.83 without it appearing black in visible light. Unfortunately, we just don't know enough to make the model really accurate.
This is an important detail that I have considered carefully and commented on in other contexts. Below is a chart of the correction factor to be applied to a conduction-type (Pirani) pressure gauge. These gauges depend on the thermal conductivity of the gas, so the chart directly shows the variation at low pressure and gas composition. You can see that Hydrogen has the highest thermal conductivity of the gases, and that the curves converge as the pressure declines below 1 mbar. However, a nominal 1kPa (10 mbar) H2 pressure measured with a Pirani type gauge would represent only ~1 mbar of actual gas pressure. Therefore a capacitance gauge or physical manometer should be used for accuracy.
Neither of the two reports from Mizuno gives specific details of the vacuum system components used. Figure 5 of the JCMNS article  shows what may be a capacitance gauge but it would be good to have this confirmed.
Regarding the chart of thermal gradient measurements Jed posted, the reactor in the image appears to be the earlier one with the heater sheath wound externally around the body. The measurements shown seem consistent with the expected thermal behavior of such a metal construction. The relatively massive end caps act as heat sinks for distributed thermal input, resulting in a gradient with the hottest areas furthest from the ends. Therefore the conclusion that the hotter spots result from excess heat should be reconsidered, absent a null calibration data set from the same reactor and measurement procedure.
What temperatures? 110 deg C? Surely that depends on how think the steel is?
No, 200 °C as specified in step 13. The thickness of the steel will have a relatively small effect on the external thermcouple positioned directly over the core heater. This is because the thermal conductivity of 304 stainless steel is fairly low, about 1/4 that of mild steel and just 7% of Aluminum. For my attempted bake out of the cell, I covered it with 1 inch thick tubular fiberglass pipe insulation. The heat loss through the insulation is pretty well controlled, as shown by the thermal image below. Much of the loss is through the left end cap where the thermowell is mounted. Even with this insulation, my 300 watt heater is not capable of bringing the center of reactor shell to 100 °C.
Here' a progress report as of 7 November 2019.
The Mizuno R20 experiment is deceptively difficult, unlike what most casual commentators might think. The difficulty starts in these simple directions from Jed's summary:
"11. Close reactor and install in calorimeter. Evacuate the reactor to 7.5 × 10-5 torr (0.01 Pa).
Hold for 2 hours.
12. While pumping, heat with sheath heater to 100° - 120°C for 5 - 20 hours. Pressure must
reach 7.5 × 10-5 Torr (0.01 Pa).
13. Increase temperature to 200°C with sheath heater while pumping for 1 - 2 hours. Most of
the water should be out of the sample and reactor at this point.
Reaching 0.01 Pa is not difficult with all-new components and a good turbo pump, but rather tricky lacking those. Not hard to remedy, all it takes is money and time....
I started with a collection of used conflat 1.33 parts and a decent two-stage rotary pump. After finding several leaks with 2 bar H2 and a leak sensor, I replaced several defective components and added a nice MKS 356 full-range vacuum gauge. The system now reliably pumps down to 0.1 Pa, the limit of the pump I have. But there is still some leakage (as always) - once the pump is turned off and isolated, it's about 1 Pa / minute which I think is through the main valve to the pump manifold. I ordered a new valve which should arrive today. Only once the system is vacuum tight long-term, will it be ready for a turbo pump.
Why is this level of vacuum stability so important although not mentioned by Jed? The Mizuno protocol requires maintaining 300-1000 Pa of D2 in the reactor for days or weeks, without any contamination of oxygen (air) getting in. I know from my past Glowstick work that this is the real challenge of the experimental protocol and must be correct. I'm not shy about buying good equipment, and have invested around $3k so far in building the apparatus. The turbo pump system will be around $10k new or $5k used for a known good system with low hours. Definitely not interested in junk parts for this important piece of the system!
OK now for some results. My reactor is 1/2 scale of Mizuno's (1/4 volume). The heater is a 300 watt cartridge in an axial thermowell. At full power with vacuum it only heats the reactor outside wall to ~80C, even with 1 inch of insulation over the entire tube. The thermal rise time is about 30 minutes. This result suggests that the temperatures quoted by Jed in the report are not possible with the 500 watt heater he specified. The Chinese replication reported in August used a 1500 watt heater element, and the cell was in a well-insulated calorimeter box. So my next improvement will be a 600 watt heater element installed naked through the 3/8" swagelok fitting in place of the thermowell. Then more leak checking and hopefully a proper bake-out of the cell.
During replication of the CAN electrolysis experiment earlier this year, I detected a RF signal at 228 MHz, shown below. This was probably from a stray LC resonance of the apparatus wiring, stimulated by the fast high current impulse from the sparker. I only mention it because a similar kind of resonance in the Mondaini apparatus could result in the RF he detected.
I believe someone did this. Also, they looked up the hardness of Pd and found that it varies more than we realized.
We discussed this back in July, when the R20 paper was first posted. Here's what I wrote in reply to Jed's earlier comment:
Mohs hardness refers to the scratch resistance - the ability of harder material to scratch softer material. The Brinell hardness (and similar Vickers scale) refers to indentation hardness - penetration of a calibrated indenter into the tested material. So while Ni is apparently harder to indent, it is softer to scratching (removal of material) by Pd.
Perhaps annealing the Pd before the rubbing would reduce the possible tendency to remove Ni rather than depositing Pd on its surface.
"Palladium is easily annealed with the use of a fuel-oxygen torch, with natural gas or propane and oxygen recommended. Flux is not necessary. Using the high-heat soldering surface and shade five or higher eye protection, adjust the torch to a slightly reducing flame, heat the palladium to a mild orange color, and hold for 10 to 30 seconds. The thicker the metal, the longer you must anneal it."
and a comment there: "Anneal to dull red and then leave to cool to room temp, also stops it from cracking."
I followed that procedure using a small propane torch, with good results.
My suspicion is that if transmutation occurred, it was induced by cavitation shock impacts on the material. The foil is 0.33 mm thick, with half-wave phonon resonance through the sheet of ~1.8 MHz. That is sufficiently above the ultrasonic stimulus that direct mechanical effects are not likely. The ~1.5% cleaning additive contained Sodium, Sulfur and Nitrogen, but no Calcium or Silicon. Those elements could have been from a contaminant inclusion in the foil, so their detection is not proof of transmutation and further study is needed.
Alan, I'm sure I missed it: What was the solvent you used?
The ultrasonic bath was ~1.5% Micro90 in DI water. It's a widely used cleaning product for lab ware and high vacuum components.
Upcoming repeats of the test will use pure DI water, and then with 10% D2O added, while monitoring with gamma and x-ray spectrometers.
I've posted a complete SEM/EDS report on the observed transmutation of Indium from ultrasonic cleaning.
It's a comprehensive document that will take some time to review. The first image on page 1 shows the crater about 2 mm wide that appeared following a 3 minute ultrasonic cleaning of pure Indium foil. We analyzed about 30 spots in and around this artifact using the Bruker Q75 EDS system's Esprit software. An area outside the artifact was also analyzed to confirm the purity of the material as received.
Bob, magicsound, please would you e-mail / post the scanning electron micrograph and the X-Ray flourescence data that you obtained from the
ultrasonically treated Indium foil , so that I can pass them on.
I just got home from Italy last night and did the usual unpack-and-sort-mail today. I will post the SEM/EDX images tomorrow. Further tests will be done later this week, to see if it's replicable.
Well done Bill for fixing a most excellent and enjoyable conference.
For me, the highlight of ICCF 22 was the announcement of a serendipitous discovery made by Alan Goldwater and Robert Greenyer that Indium
subjected to ultrasonic excitation ( 43 kilohertz , 35 watts ) for a few minutes showed unambiguous evidence of nuclear transmutation.
Have they discovered cavitation induced fission of the Indium nucleus ?
Their discovery was made only a few days before their travelling to Assisi , so there is much more to be researched.
Interestingly Leo Szilard submitted a British Patent (No. GB 630726 ) in 1938 for a chain reaction involving Beryllium and Indium.
I believe that for security reasons the submission was D-noticed, but that the patent was granted and published after the war,
when the chain fission cat was out of the bag. Pete.
Thanks for your encouraging comment Peter. I do have to point out that our "serendipitous discovery" was exactly that, an unexpected observation following a simple cleaning process. Therefore it would be a mistake to call the result unambiguous, and I made no such claim. I do find it intriguing and well worth further testing and possible replication.
There was definitely no Beryllium in the foil or the ultrasonic bath, so the connection to the Szilard patent is probably unfounded. It's worth a look though, if you can provide a link to the document.
Just a remark about the calcite: tap water varies enormously in its mineral content - minimum effort best guess at replicating process (given no-one can know what as aspect of the Mizuno methodology generated the R20 results, copying faithfully everything published is good idea) would be to measure or look up local tap water calcium content and match to the average of that in Mizuno's lab by dilution with distilled H20, or addition of carbonate heavy bottled water, if that is needed.
THHuxleynew If you have not read my complete paper, please follow the references I included at the end. Analyses of tap water for my lab and for Sapporo municipal water show similar concentrations of Calcium. Of course, we cannot be sure if Mizuno's "tap water" is from the municipal supply, but that seems a reasonable assumption.
Note also my included reference showing the characteristic morphology of precipitated Calcite crystals. However, from my investigation I believe that the crystal size is not very relevant, since they are ground up and intercalated with the Pd deposited by rubbing.
Pd is easy to anneal. Heat it gently in the oxygen rich tip of a small propane torch flame. When the metal reaches an even soft orange color let it cool completely in air.
My live doc previously posted describes the process in full detail. The deposition of the Pd depends on the sharp scraping edges created by the prior sanding of the mesh, and without that step the deposition will not succeed.
I arrived Sat am from NY. Staying at an Airbnb at the beach today to catch up on sleep. Will pick up Bob Greenyer tomorrow in Rome and drive to Assisi.
I got a small (40 cu ft?) Argon bottle from my local Matheson welding supply, around $50. I’m in northern Cal.
It seems that as you say, if the Ni has not work hardened in the mesh production, it is ductile enough to make finer burrs. But they must be very fine because the edges look quite sharp. It seems that at this level of importance of every detail, you daren't even rely on what you think is experience. It seems necessary to start with a clean sheet, and build the picture pixel by pixel.
It could be that there is little or no actual burr, but rather just a very sharp edge defined by the boundary of the land and the round Ni wire substrate. As the size of the land increases, so will be the angle subtended by that transition. The effect of this edge on the Pd is clearly that of a scraper. I will have a closer look after ICCF with that in mind.
Mizuno recommends starting rough and working with successive finer grits, as is the norm with a flatting/smoothing process. Also, as I recall, Mizuno a) never uses anything a rough as 100 grit , and b) starts at around 400 and works to around 1500 grit. This would give a much smoother finish. I also suspect this will get rid of a lot of the rough edges which will alter the nature of the Pd deposition. I have a deal of experience of this process over the years, and when you start rough, it produces the rough edges you have. But as you go smoother, it produces an increasingly well defined, burrless, clean edge
In my initial test on the mesh sample, I followed Mizuno's sequence of increasingly finer sanding grit. Evidence from the subsequent burnishing showed that the sharp burrs did not disappear with 1500 grit. It looked like the finer grit only resulted in a sharper edge on the burr. I suspect that at micron scale the Ni is sufficiently ductile that the material displaced by the sanding is not entirely removed, and is partially smeared over the edge of the land resulting in the observed burr. A further look at the sanded but unburnished material is possible.
This leads to the second point which is that you point out that the most Pd is deposited on the rough 100 grit mesh. Have you measured the actual weight gain of Pd on the mesh, and is it sufficiently well defined, area and consistency of treatment wise, to be able to calculate the equivalent weight that would be deposited on mesh of area Mizuno used. If so, does this match the ~ 50mg that TM recommends?
With the latest test I was not attempting to precisely quantify the deposition of Pd, but rather to explore the parameter space of burnishing on Ni foil or plate, as suggested by Ed. Whether the apparent increased deposition rate with coarser sanding would be beneficial to LENR activation of the material is unknown. At least it is now a somewhat controllable parameter. Further testing will certainly be done, but not until after ICCF.