I know that my best early work was with Pd+Ag. I used the old Shaffer fountain pin numbs (circa late 50's)
The diffusion palladium was 23% Ag if memory serves. Fleischmann's "boil off" cathode had Ce in it.... if memory serves. D2 From: Jed Rothwell Sent: Monday, February 28, 2011 2:16 PM To: [email protected] Subject: [Vo]:Fleischmann's "Type A" palladium Terry Blanton wrote: I agree. However, even people who bought their Pd from the same source as F&P (Johnson Matthey?) had less success because there was something "special" in the way it was processed. I think that process has yet to be revealed? I'm sure Jed would remember. The process wasn't all that special, and it is not secret. When he began this research, Fleischmann went to Johnson Matthey (JM) and told them he wanted Pd that can be highly loaded without cracking. They recommended the Pd material they developed in the 1930s for hydrogen filters. Fleischmann later called this "Type A." He distributed samples to many researchers, who had much higher success with it than with any other type. See Table 10 here, p. 43, for example: http://lenr-canr.org/acrobat/MilesManomalousea.pdf The cathodes labeled "(F/P)" came from Fleischmann. They all worked, and they produced more heat than the others. At BARC they used an actual hydrogen filter to run a cold fusion experiment. It worked splendidly. As I recall, someone at NASA also did this. JM has changed the method they used to make this type of Pd. The newer type might not work as well. Then again, it might work. As far as I know, no one has the money to find out. JM offered to make up a batch for Fleischmann and me, with cathodes cut to specification, but their minimum order was 1 kg and I could not afford it. Probably, by now Violante's group at the ENEA knows as much about how to make effective Pd as JM did. They may have wasted 15 years finding out, when they might have just asked JM to tell them. Or sell them some. During the Toyota cold fusion project in France, there was a strange agreement between Toyota and JM. JM supplied the materials and then took them back, doing all the analysis. They wouldn't tell Toyota what they found. No one I know has any idea what happened to the data. Their is bad blood between them. The way I heard it, Toyota wanted JM to share the information, and they offered them peanuts. (I believe that is how it was described to me, "peanuts," meaning a small amount, not the 1970s Japanese Lockheed scandal in which 1 peanut = $1 million). The key calorimetric data from that project also disappeared. Fleischmann had quite a lot of it on paper. Someone broke into his house and took it. They did not take anything else, so I suppose this was no ordinary thief. He asked Toyota for new copies but they never responded. He is pretty upset about the whole thing, as you can imagine. Below is a memo about Type A Pd that I wrote in February 2000. - Jed - - - - - - - - - - - - - - - - - The Type A palladium saga February 7, 2000 For many years Martin Fleischman has been recommending a particular type of palladium made by Johnson Matthey for cold fusion experiments. He has been saying this to anyone who will listen, but very few people do. He handed out several of these ideal cathodes to experienced researchers, and as far as he knows in every case the samples produced excess heat. The material was designated "Type A" palladium by Fleischmann and Pons. It was developed decades ago for use in hydrogen diffusion tubes: filters that allow hydrogen to pass while holding back other gasses. This alloy was designed to have great structural integrity under high loading. It lasts for years, withstanding cracking and deformation that would quickly destroy other alloys and allow other gasses to seep through the filters. This robustness happens to be the quality we need for cold fusion. The main reason cold fusion is difficult to reproduce is because when bulk palladium loads with deuterium, it cracks, bends, distorts and it will not load above a certain level, usually ~60%, I think. Below 85 to 90% loading bulk palladium never produces excess heat. A sample of palladium chosen at random from most suppliers will *never* reach this level of loading. You could perform thousands of tests for cold fusion with ordinary palladium, with perfect confidence that you will never see measurable excess heat. That is essentially what the NHE did: they performed the wrong experiment hundreds of times in succession, using materials which everyone knows cannot work. This is like trying to make a 27-story building out of doughnuts. It seems likely to me that most of the reproducibility problems with bulk palladium CF would have been solved years ago if people had only listened to Martin Fleischman's advice. Alas, in my experience, people seldom listen to advice or follow directions. Fleischman sometimes compounds the problem by speaking in a cryptic, convoluted style and by using complex mathematical equations that few other people can understand. He sometimes takes a long time to respond to inquiries; he answered one of my questions two years after I asked. However, in this case he has made himself quite clear on many occasions. For example, he wrote QUOTE: . . . We note that whereas "blank experiments" are always entirely normal (e.g. See Figs 1-5) it is frequently impossible to find any measurement cycle for the Pd-D2O system which shows such normal behaviour. Of course, in the absence of adequate "blank experiments" such abnormalities have been attributed to malfunctions of the calorimetry, e.g. see (10). [Ikegami et al.] However, the correct functioning of "blank experiments" shows that the abnormalities must be due to fluctuating sources of excess enthalpy. The statements made in this paragraph are naturally subject to the restriction that a "satisfactory electrode material" be used i.e. a material intrinsically capable of producing excess enthalpy generation and which maintains its structural integrity throughout the experiment. Most of our own investigations have been carried out with a material which we have described as Johnson Matthey Material Type A. This material is prepared by melting under a blanket gas of cracked ammonia (or else its synthetic equivalent) the concentrations of five key classes of impurities being controlled. Electrodes are then produced by a succession of steps of square rolling, round rolling and, finally, drawing with appropriate annealing steps in the production cycle. [M. Fleischmann, Proc. ICCF-7, p. 121] END QUOTE Fleischman recently gave the some additional information. The ammonia atmosphere leaves hydrogen in the palladium which controls recrystallization. Unfortunately, this material is very difficult to acquire and there is practically none left in the world, because Johnson Matthey stopped making it several years ago. Palladium for diffusion tubes is now made using a different process in which the palladium is melted under argon. Material made with the newer technique might also work satisfactorily in cold fusion experiments, but Fleischman never had an opportunity to test it so he does not know. There should be plenty of the new material available, so perhaps someone should buy a sample and try it. Johnson Matthey has offered to make more of the older style Type A for use in cold fusion experiments. They will charge ~$20,000 per ingot, which is a reasonable price. Fortunately, the precise methodology for making the older material is well-documented and an expert who helped fabricate previous batches has offered to supervise production. So, if anyone out there has deep pockets and once a batch of the ideal material to perform bulk palladium cold fusion experiments, we can arrange it. I do not know any cold fusion research scientists or institutions who can afford $20,000 worth of material, but perhaps several people could get together and pool their resources. The above description of Type A is not comprehensive. We know little about the material. We cannot begin to explain why it resists distortion and allows high loading. The experts in Johnson Matthey probably know, but they are not talking. When Ed Storms read this description, he immediately thought of a number of important questions about fabrication techniques: "What is the crucible made of in which it is melted? Pick-up of crucible material can not be avoided. How is oxygen removed? Is calcium boride used, which is the usual method? What is the boron content?" Unfortunately, such details are trade secrets which Johnson Matthey will not reveal. Fleischman does not know the answers. Anyone who has a sample can quickly find out what elements are present in the alloy, in what proportions. But questions such as "How is the oxygen removed?" may not be as easy to ascertain. The trade secrets are not what is in the metal, but how it got there and why it stays. I asked Fleischman how confident he is that this material is effective, and how much batch-to-batch variability he observed. He said that since 1980 he has used samples from eight or nine batches. Only one batch failed to work, and was returned for credit. In general, any material from Johnson Matthey works better than palladium from other sources. The most dramatic proof of this can be seen in M. Miles, "Anomalous Effects in Deuterated Systems." See especially Table 10, p. 42, summarizing the effectiveness of palladium from various different sources. The success ratio with Johnson Matthey material was 17 out of 28 (17/28) compared to 2/5, 0/19, and 2/35 with other sources. Only the alloys fabricated in-house by the NRL worked better, with a 7/8 success ratio. Miles tested two samples of Type A palladium supplied to him by Fleischman and Pons. Both produced excess heat at much higher power density than samples from other suppliers (3 - 14 W/cm3 compared to 0.3 - 2.1 W/cm3). Fleischman reported success with pure palladium, as well as silver and cerium alloys. So did Miles, and he also had good results with boron alloys. The NRL in Washington reported no heat with samples from the same batches Miles tested, but their calorimeter was an order of magnitude less sensitive than his (with 200 mW precision compared to 20 mW), so even if their samples had produced the same level of heat Miles observed, they could not have detected it. In their Final Report, the NHE claimed that they used "the type of palladium recommended by Fleischman and Pons" in a series of experiments in the final stage of the project, after all else had failed. This is incorrect. They did not have any of the Type A palladium. Perhaps they used some other Johnson Matthey material instead. They have refused to reveal the batch number or say when or where they acquired the material, but as far as Fleischman knows, there was no Type A material available at that time. When the NHE program began, Fleischman supplied them with three Type A cathodes. Two of them produced excess heat, and one failed because of a prosaic problem with the equipment. The NHE disagrees with Fleischman's conclusion. Based on their nonstandard method of evaluating calorimetric data, they say all three samples failed to produce heat. They refuse to release detailed data which would allow others to analyze the results using standard methods. Fleischman, McKubre and Miles have criticized their methodology, in which a single calibration pulse made a few days after the experiment begins, when low-level excess heat is probably already present. (See the Fleischmann quote above, and M. Miles, "Report on Calorimetric Studies at the NHE Laboratory in Sapporo, Japan.") The question is: At this late date does anyone care about bulk palladium electrochemical cold fusion? Does anyone still want to try it? Even with the proper materials, this is still a very difficult experiment. Fleischman and McKubre agree that if techniques can be used, they should be. McKubre said, "the world is fascinated by electrochemistry, except electrochemists. If they can find another way of doing the job they will always choose the other way." Fleischman believes that the qualities of the palladium material are not be as important with electrodiffusion, which pushes deuterons through the bulk of material rather in through the surface. "Solid-state works better than interface chemistry." (Other people may not find the Italian electrodiffusion results as convincing as he does.) McKubre has successfully replicated the Case experiments using gas loading into commercial catalysts made of palladium on carbon. Researchers may feel that this kind of technique is more promising than bulk palladium, and there is no point to revisiting obsolete, 10-year-old experiments. We may no longer need Type A palladium. We can hardly afford it, anyway. I once asked Fleischman how he learned about Type A palladium. He said: "It is very simple. When we began this work I went to Johnson Matthey, I told them what I needed, and they recommended this material." As I said, he has a baroque imagination and he often goes about doing things in indirect, complex ways, but in this case he used the direct approach.
