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Publication numberWO1996006434 A1
Publication typeApplication
Application numberPCT/US1995/010534
Publication date29 Feb 1996
Filing date18 Aug 1995
Priority date18 Aug 1994
Publication numberPCT/1995/10534, PCT/US/1995/010534, PCT/US/1995/10534, PCT/US/95/010534, PCT/US/95/10534, PCT/US1995/010534, PCT/US1995/10534, PCT/US1995010534, PCT/US199510534, PCT/US95/010534, PCT/US95/10534, PCT/US95010534, PCT/US9510534, WO 1996/006434 A1, WO 1996006434 A1, WO 1996006434A1, WO 9606434 A1, WO 9606434A1, WO-A1-1996006434, WO-A1-9606434, WO1996/006434A1, WO1996006434 A1, WO1996006434A1, WO9606434 A1, WO9606434A1
InventorsRichard A. Day, Kenneth A. Rubinson
ApplicantUniversity Of Cincinnati
Export CitationBiBTeX, EndNote, RefMan
External Links: Patentscope, Espacenet
Hydride condensation process
WO 1996006434 A1
Abstract
A process is disclosed for the generation of energy and the conversion of deuterium into tritium. The above effects are achieved when a deuteride source is maintained so as to form an interface in the presence of a positively polarized metal. An electric potential may also be used to drive the reaction.
Claims  (OCR text may contain errors)
What is claimed is:
1. A process for the production of tritium and the accompanying energy, comprising immersing in a deuteride salt, in a form in which it is electrically conductive, a material which conducts electricity and forms an interface with said deuteride salt, such that an oxidizing Faradaic process occurs at the surface of said conducting material.
2. The process according to Claim 1 wherein the deuteride salt is an alkali metal deuteride.
3. The process according to Claim 2 wherein the conducting material is selected from the group consisting of Au, Al, Ba, Bi, C, Ca, Cd, Co, Ga, Ge, Hg, In, Na, Pb, Pt, Pd, Si, Sn, Sr, Tl, V, Zn, Ag, Mg, Mn, Cr, Fe, Mo, Cu, Zr, Ce, Ti, Nb, Ta, the lanthanides, and mixtures thereof.
4. The process according to Claim 3 wherein the deuteride salt is substantially free of chloride ions.
5. The process according to Claim 4 wherein the deuteride salt is substantially free of any additional anions.
6. The process according to Claim 3 wherein the conducting material is continuously renewed without interrupting the process.
7. The process according to Claim 4 wherein the deuteride salt is present in the form of a liquid.
8. The process according to Claim 7 wherein the conducting material is present in the form of a liquid or a solid.
9. The process according to Claim 8 wherein no external voltage is applied to the system.
10. The process according to Claim 9 wherein the conducting material is selected such that the cation of the deuteride salt has a high solubility in the conducting material.
11. The process according to Claim 10 wherein the conducting material is selected from the group consisting of Au, Al, Ba, Bi, C, Ca, Cd, Co, Ga, Ge, Hg, In, Na, Pb, Pt, Pd, Si, Sn, Sr, Tl, V, Zn, and mixtures thereof.
12. The process according to Claim 11 wherein the conducting material is selected from the group consisting of Au, Al, and mixtures thereof.
13. The process according to Claim 11 where the deuteride salt is selected from the group consisting of lithium deuteride, sodium deuteride, potassium deuteride and mixtures thereof.
14. The process according to Claim 13 wherein the deuteride salt is lithium deuteride.
15. The process according to Claim 8 wherein an external voltage is applied to the system.
16. The process according to Claim 15 wherein a positive voltage is applied to the conducting material in an amount sufficient to drive the oxidizing Faradaic process.
17. The process according to Claim 16 wherein the applied voltage is at least 20 millivolts.
18. The process according to Claim 17 wherein the conducting material is selected from the group consisting of Ag, Mg, Mn, Cr, Fe, Mo, Cu, Pd, Zr, Ce, Ti, Nb, Ta, the lanthanides, and mixtures thereof.
19. The process according to Claim 18 wherein the conducting material is selected from the group consisting of magnesium, copper, molybdenum, niobium, palladium and mixtures thereof.
20. The process according to Claim 18 wherein the deuteride salt is selected from the group consisting of lithium deuteride, sodium deuteride, potassium deuteride and mixtures thereof.
21. The process according to Claim 20 wherein the deuteride salt is lithium deuteride.
22. The process according to Claim 21 wherein the conducting material is selected from the group consisting of magnesium melt, aluminum melt, copper, and mixtures thereof.
23. A process for the production of tritium and the accompanying energy, comprising:
heating a solid compound of anionic deuterium to a temperature of greater than about 300C in the presence of a metal selected from the group consisting of group 1A, group 2A, transition metals, lanthanides, actinides, and mixtures thereof; and applying a low positive electrical voltage to said metal; thereby producing tritium.
Description  (OCR text may contain errors)

HYDRIDE CONDENSATION PROCESS

CROSS REFERENCE TO RELATED APPLICATION

This application is a continuation-in-part of U.S. Patent Application Serial No. 08/292,489, Day, filed August 18, 1994.

FIELD OF THE INVENTION

The present invention relates to a process for allowing the joint redistribution of the constituent particles between two atomic nuclei at relatively low ( < 1000 K) temperature and under easily controlled chemical conditions. More specifically, the present invention provides a process for the production of tritium from a deuterium source wherein one form of the deuterium is present as deuteride ion, D .

BACKGROUND OF THE INVENTION

In 1989, two chemists working at the University of Utah announced that they had built a simple, room-temperature laboratory device that generated more energy in the form of heat than was fed into it as electricity. The researchers - Stanley Pons of the University of Utah and Martin Fleischmann of the University of Southampton in England - attributed this heat to a nuclear fusion reaction and referred to the effect as "cold fusion. " This work spawned a great deal of research in the area. Much of this work is summarized in Bockris, et al. , Fusion Tech. 18: 11 (1990), and Chechin, et al. , Critical

Review of Theoretical Models for Anomalous Effects in Deuterated Metals, Intl. J. Theor. Phys. 33: 617-670 (1994). 6/06434 PC17US95/10534

- 2 -

Fusion requires the joining together of two atomic nuclei, both of which have a positive electric charge and so repel each other strongly. It has been believed that only by making the nuclei extremely energetic could they overcome this electrostatic repulsion - the "coulomb barrier" (a coulomb is the SI unit of electrical charge). "Hot fusion" is thought to achieve this result by stripping the electrons from atoms using high temperatures to expose the nuclei to be fused. The nuclei then interact, for example, in a powerful magnetic field. For deuterium nuclei, this fusion reaction creates tritium and helium nuclei, as well as a shower of neutrons and gamma radiation. Fusion had been thought to occur only through the use of mega-electron-volt particle accelerators, at high temperatures in stars, in thermonuclear bombs, in confined high temperature plasmas, and in inertia! confinement brought to fusion conditions with high power lasers.

Nevertheless, some of the earliest nuclear experiments in 1934-35 in

Rutherford's laboratory in Cambridge illustrated the production of high-energy protons and neutrons with relatively low energy collisions of deuterium nuclei. The effect was observed in the experiment which tritium was discovered. See Oliphant, et al., Rutherford Transmutation Effects observed with Heavy Hydrogen, Nature 133:413 (1934). In one subsequent set of experiments, 150 keV deuterium nuclei hit solid ND4C1 or (ND4)2SO4 targets with the same effect for both: emission of 1.9 MeV (megaelectron-volt) neutrons, 3.2 MeV protons and 1 MeV tritium. See Dee, Some Experiments upon Artificial Transmutation using the Cloud - Track Method, Proc. Roy. Soc. Lond. A. 148: 623-637 (1935). In addition, no gamma radiation was observed. However, the 150 keV

(kiloelectron-volt) kinetic energy of the deuterium nuclei is still about six orders of magnitude greater than the room temperature equivalent: 25 meV (millielectron-volt) .

An extension of this type of experiment was performed more recently at

Brookhaven National Laboratory. Unexpectedly large yields of protons and tritium were observed when clusters of D2O of up to 100 molecules each impacted a TiD target with a total energy between 200 and 325 keV. Beuhler, et al. , Cluster-Impact Fusion, Physical Review Letters, 63: 1292-1295 (1989).

Attempts to harness fusion for energy generation have, thus far, been unsuccessful. Despite decades of work and great expense, hot fusion in confined plasmas has yet to produce more energy than that needed to heat the fuel and power the magnets. Similarly, in inertial confinement the energy generated could not drive the lasers. The Pons-Fleishmann announcement started a major scientific controversy while, at the same time, the notion that significant amounts of fusion energy could be produced by a tabletop apparatus at room temperature raised hopes among many people for a more realizable energy source.

Pons and Fleischmann' s experiment is based on the use of electrolysis of

D2O ("heavy water") to load electrically uncharged deuterium into the bulk of a metal cathode. This is done as follows: An electrode pair consisting of a strip of palladium surrounded by a coil of platinum wire is immersed in a container of heavy water. A salt, typically lithium deuteroxide, is dissolved in the heavy water to make it more conductive. When a voltage is applied across the electrodes, an electrical current flows through the liquid and causes the heavy water to decompose into its constituent atoms: deuterium migrates to and dissolves in the palladium electrode and oxygen is released as a gas at the platinum electrode. As deuterium builds up in the palladium, it supposedly undergoes the fusion reaction. The palladium's atomic lattice captures the energy released by the reaction and the metal heats up.

Heat is sometimes detected during the production of tritium and neutrons under "cold fusion" conditions; sometimes it is not. The Bhabha Atomic Research Center (BARC) in Bombay, India, has produced tritium at several thousand times "background noise" levels, using a variety of electrode materials, including alloys of palladium and titanium. This work is described in a series of contiguous articles in Fusion Technology, Volume 18 (1990). See Iyengar, et al. , Bhabha Atomic Research Centre Studies in Cold Fusion, Fusion Tech. 18: 32-102 (1990).

The use of a palladium sheet to form one electrode within an electrolytic cell to produce excess heat, the electrolytic cell being a Pons-Fleischmann-type has been taught by Edmund Storms. The description of the Storms electrolytic cell and his experimental results are described in an article entitled "Measurements of Excess Heat from a Pons-Fleischmann-Type Electrolytic Cell

Using Palladium Sheet" appearing in Fusion Technology, 23:230-245 (1993). In a previous article, Storms reviewed experimental observations about electrolytic cells for producing heat in an article entitled "Review of Experimental Observations About the Cold Fusion Effect", Fusion Technology, 20:433-477 (1991).

In a different approach from the electrolytic cell, at the Los Alamos National Laboratory, Thomas Claytor and Dale Tuggle have produced tritium in various ways. In one method, they applied a voltage to a deuterium gas-filled cell containing alternating electrodes of palladium and silicon. The electric discharge between the electrodes has repeatedly generated 10 billion atoms of tritium per hour (1.9 nCi/hr). More recently, the Los Alamos group has obtained even higher production rates by sending pulses of current through the palladium rather than applying a voltage through the gas. Apparently, one key may be to induce a sudden change in temperature. The amount of tritium in the materials was measured before each study was begun, each system was completely sealed from the environment, and tritium production was monitored continuously during the studies. See, Storms, Technology Review, May-June, Yet another set of experiments suggests that external voltages are not necessary for fusion to occur in low yield. A simple oxidation-reduction reaction in free solution in the presence of deuterium supplies the needed conditions. Thus, Arzhannikiv and Kezerashvili identified a few excess neutrons in the reaction of LiD with D2O. Arzhannikiv, et al., First observation of neutron emission from chemical reactions, Phys. Letts. A. 156: 514-518 (1991). However, Szeflinski, et al., Upper limit of neutron emission from the chemical reaction of LiD with Heavy Water, Phys. Letts. A. 168: 83- 86 (1992), suggest that such neutrons are not present clustered in time as expected.

Other publications of interest with regard to the present invention include the following:

Liaw, et al. , J. Electroanal. Chem. 319: 161 (1991), describes an experiment wherein a palladium electrode was placed in an LiCl-KCl eutectic saturated with LiD. A significant amount of excess heat was measured.

U.S. Patent 5,318,675, Patterson, issued June 7, 1994, describes an electrolytic cell and method of electrolysis and heating of water containing a conductive salt in solution. The electrolytic cell includes a non-conductive housing having an inlet and an outlet and spaced apart first and second conductive foraminous grids connected within the housing. A plurality of non-conductive microspheres, each having a uniformly thick outer conductive palladium layer, are positioned within the housing in electrical contact with the first grid adjacent to the inlet. An electric power source is operably connected across the first and second grids whereby electrical current flows between the grids within the water solution. While no claims are specifically directed to cold fusion, Figures 14 and 15 are said to show " a prominent discontinuity with respect to heat output vs. wattage input ... indicating an unexpected increase in that heat output. " See, column 9, lines 43-63 in the patent. U.S. Patent 5,372,688, Patterson, issued December 13, 1994, describes an electrolytic cell used for a Pons-Fleishmann-type reaction. The cell utilizes a liquid electrolyte (D2O or H2O) with a conductive salt dissolved in it, and palladium-coated microspheres loaded with hydrogen to form a metallic hydride.

PCT Patent Application WO 90/16,070, Brumlik, et al. , published December 27, 1990 (cited in Chem. Abs. 114:216545 (1991)).

PCT Patent Application WO 90/15,415, Coupland, et al. , published

December 13, 1990 (cited in Chem. Abs. 114:216546 (1991)).

PCT Patent Application WO 90/13, 127, Joshi, published April 18, 1989 (cited in Chem. Abs. 115:80697 (1991)).

Japan Kokai JP 06 75,072, Kunimatsu, et al. , published June 24, 1991 (cited in Chem. Abs. 111:240370 (1994)).

While most of the scientific community has rejected the idea of cold fusion (see, generally, Bad Science - The Short Life and Weird Times of Cold

Fusion by Gary Taubes, Random House, 1993, and Cold Fusion: the scientific fiasco of the century by J.R. Huizenga, Oxford University Press, 1993), recently there has been some renewed interest in the phenomenon as indicated by U.S. Patents 5,318,675 and 5,372,688. This interest is also noted in two review articles by Edmund Storms: "Review of Experimental Observations about the Cold Fusion Effect" in Fusion Tech., 20:433 (1991) and "Review of Experimental Observations About the Cold Fusion Effect" in Warming Up to Cold Fusion, Technology Review - May /June 1994.

The available cold fusion literature indicates that aqueous electrolysis and deuterium gas saturation in the presence of palladium have been the preferred methods tried, unfortunately without much success or reproducibility. There is therefore a need for a process for achieving cold fusion which overcomes the inadequacies of the prior art processes.

SUMMARY OF THE INVENTION

It is a primary object of the present invention to provide a process for facilitating the reaction in which deuterium atoms produce tritium and energy at relatively low temperatures ( < 1000 K) and low voltages ( <20 V) applied.

In accordance with one aspect of the present invention, there is provided a process for the production of tritium and the accompanying generation of energy, comprising: immersing in a deuteride salt, in a form in which it is electrically conductive, a material which conducts electricity and forms an interface with said deuteride salt, such that an oxidizing Faradaic process occurs at the surface of said conducting material.

In a specific embodiment of the present invention tritium is produced by heating a solid ionic compound of deuterium to temperatures of greater than about 300C in the presence of a metal selected from group 1A metals, group

2A metals, transition metals, lanthanides, actinides and mixtures thereof, and applying a low positive electrical voltage to said metal.

BRIEF DESCRIPTION OF DRAWINGS

Fig. 1 is a schematic of an apparatus for practicing the present invention. It is comprised of a reaction cell and several units following in the gas-flow stream to assay for tritium.

Fig. 2 is a schematic of a fused silica reactor with its associated heater and electrode connections. Fig. 3 is a schematic cut-away view of a reactor which comprises a stainless steel thimble and a central thermocouple/electrode.

DETAILED DESCRIPTION OF THE INVENTION

It is well known that several metals are potent catalysts for adding or removing hydrogen in its various isotopic forms (*H, 2H, 3H) to or from appropriate chemical substrates. In this environment, on or in the metal matrix, the hydrogen experiences a different environment which affects its reactivity.

It is accepted that in relatively cold conditions, since the nuclei of isotopes of hydrogen are surrounded by electrons, they can approach one another no more closely than is allowed by the molecular bonds.

The process of the present invention is believed to be based on a process where D+ and D' are able to approach within tunneling distance. Tunneling is the property where a particle can pass through a barrier to motion (an energy barrier) that it cannot surmount with any probability by classically passing over the barrier. Tunneling can occur at distances where the wavelike properties of the nucleus can take effect. The deBroglie wavelength provides a measure of this distance; the deBroglie wavelength is 1.0A for neutrons and 0.7A for the deuterium nucleus at the temperatures used here.

The reaction that is believed to occur is

D+ + D- τ* (D* D- ) → Η + p + heat

where (D+D ) represents a state where the nuclei of the respective hydrogen isotopes are within tunneling distance, and p is the proton. The reaction is highly exothermic. Along with the production of heat, a signature that a nuclear process has occurred is the production of new atomic nuclei; in the present case formation of μCi amounts of tritium (Η) has been observed.

In practicing the process of the present invention, an electrically conductive material is immersed in and forms an interface with a deuteride salt, such that an oxidizing Faradaic process occurs at the surface of the conducting material. As will be discussed below, this process may be carried out with or without the use of an external electric potential depending upon the characteristics of the particular conducting material selected.

Deuteride salts useful in the present invention include the alkali metal deuterides, particularly lithium deuteride, sodium deuteride and potassium deuteride. Lithium deuteride is most preferred. Lithium hydride can be combined with the deuteride salts, but that is not required. The deuteride salts can contain various trace metals without significantly affecting the claimed process. However, it is preferred that the deuteride salt be substantially free of any anions and particularly chloride anions in order to assure optimum performance. As used herein, "substantially free" means that the deuteride salt contains no more than about 10 mole percent of the anions in question. The deuteride salt may be present in any physical form; however, the liquid form is preferred.

The conducting materials useful in the present invention include any metals in which lithium is soluble. The degree of lithium (or other alkali metal, if lithium deuteride is not used) solubility in the metal will determine whether an external electric potential is required to drive the reaction. If the lithium has a relatively high solubility in the conducting electrode material (i.e. , if the electrode metal forms a binary alloy with lithium) then no electric potential needs to be added to the system for the reaction to occur. If the lithium has a relatively low solubility in the conducting material, then the reaction can be driven by an applied electric potential. In that case, the potential applied is an oxidative (positive) voltage applied at the working electrode in an amount sufficient to drive the reaction. The voltage required is typically at least about 20 millivolts, preferably at least about 0.5 volt, up to a maximum of about 3.5 volts at the working electrode surface. Any conventional voltage source can be used. The relative solubilities of lithium (or other alkali metals) in the conducting electrode material can be determined by looking at a phase diagram of the metal/lithium alloy. Such phase diagrams can be found in, for example, the following volumes: Binary Alloy Phase Diagrams, Massalski, Murray, Bennett and Baker (editors), American Society for Metals, 1986; Binary Alloy Phase Diagrams, Massalski, Okamoto, Subramanian and Kacprzak (editors), 2nd edition, ASM International, 1990: Moffott, Binary Phase Diagrams Handbook, General Electric, Schenectady, New York, 1976; M.H. Hansen and K. Anderko, Constitution of Binary Alloys, 2nd edition, McGraw-Hill, New York, 1958; R.P. Elliott, Constitution of Binary Alloys, first supplement, McGraw-Hill, New York, 1965.

Conducting electrode materials useful in the present invention include the following conductors: Au, Al, Ba, Bi, C, Ca, Cd, Co, Ga, Ge, Hg, In, Na, Pb, Pt, Pd, Si, Sn, Sr, Tl, V, Zn, Ag, Mg, Mn, Cr, Fe, Mo, Cu, Zr, Ce,

Ti, Nb, Ta, and the lanthanides. Mixtures of these metals can be used. These metals may be present in the system in any physical form, although it is preferred that they be present as a liquid or a solid. The preferred processes of the present invention have a deuteride salt/electrode interface which is either liquid/liquid or liquid/solid. A conducting material (electrode) in paniculate form may be dispersed throughout a liquid deuteride salt (or vice versa). When the electrode is placed in the deuteride salt it must form an interface (i.e. , a distinct boundary between phases) to be effective in the present invention. For practical use, it is important to pick for the electrode a metal which remains intact through the deuteride condensation process. If the electrode is destroyed by the process, it will have to be periodically replaced, presenting added costs and time delays. Thus, it is also preferred that the conducting material (electrode) be one which can be continuously renewed without interrupting the process. For example, where liquid magnesium or liquid aluminum is used as the conducting material, it may be pumped out of the reacting cell and renewed (i.e. , separate out the lithium from the alloy formed) in a separate process.

For reactions where no external electric potential is to be added to the reaction, useful electrode materials include the following: Au, Al, Ba, Bi, C, Ca, Cd, Co, Ga, Ge, Hg, In, Na, Pb, Pt, Pd, Si, Sn, Sr, Tl, V and Zn.

Preferred electrode materials include gold and aluminum.

For reactions where an external electric potential is to be applied to the reaction system, useful electrode materials include the following: Ag, Mg, Mn, Cr, Fe, Mo, Cu, Pd, Zr, Ce, Ti, Nb, Ta, and the lanthanides. Preferred electrode materials include magnesium, copper, molybdenum, niobium and palladium, with magnesium melt, aluminum melt, and copper being particularly preferred.

The temperature at which the reaction is carried out is not critical. The present invention shows the deuteride condensation reaction taking place at relatively low temperatures ( < 1 ,000 K). The particular temperature to be utilized will depend on the materials utilized in the reaction, whether they are to be used in solid or liquid form, and on the temperature dependence of the particular reaction itself. In a preferred embodiment, the reaction mixture is heated to a temperature of greater than about 300C, preferably greater than about 500C, in order to sinter or melt the deuteride salt.

In one embodiment of the present invention, the process for producing tritium comprises: heating a solid compound of anionic deuterium (i.e. , a deuteride salt) to a temperature of greater than about 300C in the presence of a metal selected from the group consisting of group 1A metals, group 2 A metals, transition metals, lanthanides and actinides; and applying a low positive voltage to said metal.

Unlike the failed attempts at cold fusion carried out in an aqueous environment, the reaction of the present process must be carried out in an environment in which H, D" and T" are stable. Such an environment is afforded by the metals listed above, using fused/melted salts of hydrogen isotopes and only in the absence of water.

Fig. 1 shows, in block diagram form, a generalized set-up for practicing the present invention. Fig. 2 shows one reactor used to practice the process of the present invention. The vessel depicted by the numeral 10 is a quartz cylinder which is supported by a stand 20. The quartz cylinder 10 has a thermocouple well 12 built therein. A solid quartz pedestal 15 is positioned within the cylinder 10 so as to envelop the thermocouple well 12. A quartz test tube 13 is placed upon and within the pedestal 15. On either side of the well 12, within the tube 13 are placed tungsten electrodes 18 and 18A (in the form of rods). The tungsten rods are supplied by Weldco. Inc. of Cincinnati, Ohio under the trade designation 1 TUN 187 G. The tungsten electrode 18A on one side of the well 12, is wrapped in its bottom portion with palladium foil 11. The palladium foil 11 is supplied by Aldrich Chemical Co. and has the trade designation 26,721-0[7440-05-3] . A nichrome heating wire 22 is placed in close proximity with the tube 13. The heating wire 22 is heated using platinum heater leads 24. The electrodes 18 and 18A are connected to a low voltage source of electricity so as to be able to alternate between positive and negative polarization across the electrodes.

The process of the present invention is started by placing within tube 13, a sufficient quantity of solid, powdered lithium deuteride 19, so that the powder reaches the thermocouple well and the electrode: about 2cm deep. An argon atmosphere is maintained in the cylinder 10, by supplying argon at inlet 14, which leaves the cylinder 10 at exit 16.

Using the heating wire, the temperature of the cell was raised to and held at 670C, and the temperature was monitored with a thermocouple in thermal contact with the cell. To the palladium (91 mg) wrapped electrode 18 alternately was applied +6V and -6V relative to the counter electrode. The periods at each potential were about two minutes as seen in column 1 of Table 1. It is seen that when a positive potential was applied to the palladium- wrapped electrode 18A, a temperature increase occurred; while when a negative potential was applied, the temperature fell back toward the baseline 670C held by the external heater.

The reaction was terminated within approximately 20 minutes from the start. 32 mg of the palladium was lost from the electrode.

Table 1

Δt. min Electrical Polarization of Pd +/- ΔI

1 + + 14

3 - -15

2 + + 10.5

2 - -6.5

2 + +6.9

2 - -0.8

2 + +4.7

2 - -5.0

2 + +2.2

2 . -4.7

Table 2 shows the results of a scintillation study of various residues from the above reaction in comparison with control samples. The equipment used for the scintillation measurements was Model 1282 manufactured by LKB of Sweden. CPM in Table 2 stands for counts per minute for a particular sample observed by the scintillation equipment. The "A" in CPMA stands for the lower energy channel observation and the "B" in CPMB stands for a higher energy channel observation, such as higher energy beta ray emission. Sample numbers 1, 3, 4 and 6 are all unreacted lithium deuteride samples. Sample numbers 2 and 5 are samples from the broken quartz test tube 13 of the apparatus of the present invention. Sample 5 was the supernatant scintillation fluid (Scintiverse II*, by Fisher Scientific), after soaking the quartz tube for approximately one hour. The broken end of the broken quartz test tube 13 of the apparatus was subsequently ground to fine particles in a mortar and pestle in the presence of the scintillation fluid to give Sample 2. Sample 7 is the scintillation material itself.

Table 2

Sample # CPMA CPMB Identity

1 12.0 28.0 Unreacted LiD (2nd counting)

2 60226.0 30.0 Solid residue including quartz tube ground up immersed in scintillation fluid

3 6.0 26.0 Unreacted LiD (2nd counting)

4 38.0 26.0 Unreacted LiD

5 54.0 22.0 Solid residue soaked in scint fluid

6 10.0 20.0 Unreacted LiD

7 24.0 32.0 Scintillator fluid blank

It is seen that sample 5 shows a slightly higher CPMA than all samples except 2. However, sample 2 shows a very high CPMA of 60,226, which is three orders of magnitude greater than the CPMA for the other samples. Such a CPMA count is consistent with the presence of at least 27 nCi activity of tritium. Hence, it is clear that some of the deuterium is converted to tritium.

A modified reactor was used for subsequent experiments, and a cross- section schematic of its design is shown in Fig. 3. In this figure, a stainless steel thimble (30), which holds the reactants, rests on outer (31) and inner (32) fused silica supports. Heater coil wires (33) encircle the thimble for controlling the reaction temperature, and a wire (34) is connected to the outside of the thimble. A thermocouple (35) is located within the thimble. This thermocouple, which is connected (36) to a power source, has a cover (37) along its length. For solid anodes, a layer of anode material (38) surrounds its tip. For liquid anodes, the material rests under the reactants in contact with the bottom of the thimble.

The following examples, which utilize this modified reactor, provide representative protocols for three embodiments of the present invention: a run when tritium is produced without applying an external voltage source using aluminum as the metal forming an interface with molten LiD; a run with niobium as a solid anode with an external voltage applied; and a run with liquid magnesium as the anode lying below the molten LiD.

For aluminum: 0.8361 g of aluminum was melted in the bottom of the stainless steel thimble. 0.8001 g of lithium deuteride powder was added, and the thermocouple covered with a stainless steel cap was placed in the powder. The temperature was raised to 650C over 20 minutes. Over that time a cell potential rose from zero to 1.105 VDC and back to near zero. At 650C, the ionization meter indicated evolution of Tritium. The non-condensing (at -78 C) gases were assayed by conversion of isotopic dihydrogen to isotopic water over CuO at 650C. The isotopic water was assayed by adding an aliquot to 19 mL of Scintiverse II liquid scintillation fluid. The cooled solid remaining in the stainless steel thimble was treated with water in a closed tube under flowing argon with the evolved gases assayed by conversion of the isotopic dihydrogen to isotopic water over CuO at 650C and counted by liquid scintillation. The output of the scintillation counter is in disintegrations per minute (DPM) corrected for quenching of the light emission. From the chemical reaction, the yield of gaseous tritium was 17,727 DPM, 8.0 nCi. From the reaction of the remaining cold solid, an additional 62,502 DPM, 28.1 nCi was found. A blank scintillant yielded 23 DPM, 0.010 nCi.

For niobium: 0.5350 g of niobium foil (6 mm x 50 mm) was fastened around the stainless steel cap of the thermocouple. To this, 0.8053 g of LiD was added. The temperature was raised to 711C over 60 minutes. At 274C, a cell potential of 1.4V was measured. A +0.9V potential at 3.6A was placed across the cell for 11 minutes. The temperature measured rose 2.6C over that time. The external potential was turned off for 12 minutes. The temperature dropped 4.1C. Then, a second 10 minute application of 2.78 V,

> 15 A was done. The temperature rose 42.4C. The non-condensing (at - 78 C) gases were assayed by conversion of isotopic dihydrogen to isotopic water over CuO at 650C. The isotopic water was assayed by adding an aliquot to 19 mL of Scintiverse II liquid scintillation fluid. After the run, the cell was allowed to cool for an hour. The solid remaining in the stainless steel thimble was treated with water in a closed tube under flowing argon with the evolved gases assayed by conversion of the isotopic dihydrogen to isotopic water over CuO at 650C and counted by liquid scintillation. The total number of DPM for the gaseous product of the electrolysis was 13,777 DPM, or 6.2 nCi. From the reaction of the remaining cold solid, an additional 74,790 DPM,

33.7 nCi, was found. A blank scintillant yielded 25 DPM, 0.011 nCi. The niobium metal was intact with only some discoloration of the surface.

For magnesium: 0.4583 g of Mg turnings were melted in the bottom of the stainless steel thimble. Above this was placed 0.8311 g LiD powder. The analysis protocols were the same as for niobium. After bringing the temperature to 709.4C over 59 minutes, +0.96+_0.6V, 3.4 amps was applied to the liquid magnesium for 10 minutes. The temperature rose over that time to 721.9C. While the voltage was off for 10 minutes, the temperature dropped back to 715.6 C. Then, -2.8V was applied, > 15 A, for 10 minutes. The temperature rose to 756.2C. After the current was shut off, over 15 minutes the temperature dropped to 695.8 C, and the heater was turned off. The remaining solid was treated with water in a closed tube under flowing argon, and the tritium as water collected in a separate trap. From the electrolysis, yield was 7,243 DPM, 3.3 nCi. From the remaining cold solid, the yield was 43,390 DPM, 19.5 nCi. A blank scintillant yielded 32 DPM, 0.014 nCi.

Thus, it is apparent that there has been provided in accordance with the present invention, a process for using deuterium to produce tritium which fully satisfies the objects, aspects and advantages set forth above. While the invention has been described in conjunction with a specific embodiment thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications and variations which fall within the spirit and scope of the following claims.

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Classifications
International ClassificationG21B3/00
Cooperative ClassificationG21B3/00, Y02E30/18
European ClassificationG21B3/00
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