JPH04505505A - Improvement of materials - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] 1 field The present invention relates to improvements in materials. More specifically, "cold fusion" or "solid-state fusion" This invention relates to improved materials for the heat generation process known as ``nuclear fusion''.

Professors Fleischmann and Pons and others Unusual experimental effects obtained by electrolysis of heavy water (D20) using a radium cathode (J, Electroanal, Chea+,.

251, (1989) 301-308), interest in the "cold fusion" method spreads. It was. This effect is used to try to prove or disprove this nuclear fusion theory. Although being studied, other plausible explanations have not yet been proposed. Traditionally, heat generation The process that achieves this effect is usually considered to be a low-temperature fusion type process, and It includes variations on the process described by Reischman and Ponsum. especially, We use methods other than the electrochemical method described by Fleischmann and Ponda. It would be desirable to include a method for "charging" hydrogen/deuterium storage materials according to the invention. scientific research for research and develop this process into a reliable and industrially usable power source. Therefore, there is a need for cathode materials that exhibit high heat generation efficiency. This application concerns the heat generation effect. However, applications have also been found for other products of nuclear fusion, and therefore tritium It may also be used for the formation and/or generation of neutrons.

We used modified palladium to alter the local environment of deuterium under low temperature fusion conditions. Provided are compositions of materials that undergo cold fusion when intercalated with deuterium, including: .

- In embodiments, the present invention provides high and substantially stable dislocation densities, or point defect concentrations. It is thought that it can be obtained from palladium with In other aspects, the invention provides: The low temperature fusion process occurs either at the point defect or at the boundary region when stress occurs. It is thought that this is obtained from the incorporation of stress into the palladium material at the center of stress during the process. Also other Embodiments include materials with high muon capture cross sections. Still other aspects , of palladium improved by the incorporation of lithium, especially Li6-rich lithium. Regarding usage.

One of the objects of the present invention is that the processing or other Improved materials with high dislocation density or point defect concentration due to the addition of elements or substances. The objective is to obtain palladium that is There are various methods according to the invention to achieve this objective. There are many things, which will be explained in more detail.

A first method of forming improved palladium is by methods known in the art. For example, by melt spinning, preferably at speeds on the order of 105-10 b''C/sec. or by rapidly cycling the metal through the α and β phases. Includes mechanical methods of cold working metals or rapidly cooling molten metals.

The present invention aims to maintain the intrametallic muco-α phase with a high deuterium-to-metal ratio in the metallurgical field. It includes materials known to be processed by such methods. However, U2.1''': f'1. The introduction of point defects by the method of et al. Sometimes it's not appropriate. Additionally, some experimental results show that e.g. After the material is stretched, it is desirable to improve the particle size and shape by annealing. It shows something new.

The "cold fusion" process usually takes place at temperatures above room temperature, and the subsequent heat generation Point defects in pure metals are considered to cause local heating of the palladium anode, so It is thought that it will be lost relatively quickly. Therefore, use the second method described below. Alternatively, it is preferable to use a combination of the first and second methods.

A second method according to the invention produces controlled particle and sub-particle sizes. be. In its simplest form, controlled particle size is used in metallurgy This is achieved by recrystallization according to known principles, whereby particle surfaces and triple points are It is stipulated. Activity in point defects and cold fusion is concentrated at grain boundaries is one theory. Certain embodiments of the invention have particles with an aspect ratio of less than 10. Processing that gives a material with a fine grain structure with a ratio (ratio of length to diameter) Use conditions. We prefer substantially uniform particle sizes of 10 to 40 microns. The new controlled microstructure provides improved performance for at least the heat generation process. There is experimental evidence to suggest that This microstructure is known in the field This is achieved by metallurgists using known methods. Forming the desired particle size e.g. have a particle size less than 10 microns and have a particle aspect ratio of 1. Annealing the material with more than 0 active palladium exhibits excessive thermal effects. This is a method that attempts to form a sample. Suitable annealing for stretched materials The conditions are at a temperature of about 650°C, preferably under vacuum or if possible It is heated under active gas for about 1 hour. Even if these temperature and time conditions change good. It depends on the degree of work hardening and how many times the desired microstructure is achieved. This is because there is a time-temperature curve.

Other possible methods within this second group also contribute to its stability at high temperatures. or the incorporation of additives into the palladium that contribute to the formation of point defects. What are additives? , elements or compounds that contain substances that would be considered impurities in normal use. It has a broad meaning. In such cases, it is advantageous to introduce impurities. This impurity that has an effect on the body, or at least an adverse effect, is not purified. Remains within palladium. Reduce rather than eliminate such impurities It is desirable to As understood here, gold, carbon, as an additive, of lucium, copper, iron, and platinum, and of boron, carbon, sulfur, silicon, and lithium. The use of rare earth metals including elements such as cerium and cerium can be considered. It's this attachment The additive elements are concentrated at the grain boundaries and are susceptible to chemical and/or nuclear reactions that occur. This is because it has a negative impact. Other possible additives are uranium, especially U235. be.

A particular embodiment of the use of additives is the formation of amorphous palladium materials, which This is achieved through the incorporation of additives such as silicon. PdSi and PdS icr alloy are quite easily produced in amorphous form, and these become opaque at about 400°C, but , these are considered stable up to this temperature. The shape of the crystal in a fairly short range By using improved hydrogen/heavy water diffusion/devitrification with controlled solubility to achieve Therefore, it is thought that it will be improved. by palladium for the formation of an amorphous material Elements suitable for forming eutectic mixtures include silicon, boron, carbon, lithium, and potassium. Contains sodium, sodium and iron.

Another example of the use of additives is oxide particles dispersed within a palladium matrix. , such as zirconia, dispersed intermetallic compounds such as LaNi, or FeT i, or the formation of dispersed hydride-forming metals. Unfavorable physics of such materials or to avoid other properties, e.g. standard electroless or electroplating followed by pressure Additives by depositing Pd on the additives by force sintering bonding and cooling deformation encapsulate. Other materials tried for cold fusion processes are e.g. palladium The powder metal compact encapsulated within the muskine and the amount of e.g. AlzOs baked 2~ 5% by weight of Pd/Al! 03, or titanium particles are in Pd/Ti solid solution. Dispersed in the liquid or dispersed in the palladium matrix, but P d / Pd/Ti surrounded by Ti solid solution. Such materials are “Charging” of palladium compounds with deuterium during or before the cold fusion process deuterium and related compounds, or the formation of solutions of deuterium. It is thought that the large internal stress is caused by the differential expansion caused by the volume change during the process. .

Preferably the amount of additive is less than about 20% by weight, more preferably less than about 10% by weight, Most preferably less than about 5% by weight.

The concentration of point defects is usually monitored by material resistivity and crystallography and surface spectroscopy. be done.

Embodiments of the present invention provide high point defect concentrations and high Use high stress. This coating may be palladium only or palladium /Additive mixture, electroplating, electroless plating, subtantaring, chemical vapor phase growth, thick film methods, electroforming (e.g. electroforming temperature to change stress and coating properties) (altered) or attached to the matrix by other methods that give the desired result. Ru.

The material of the present invention has been demonstrated for electrically induced cold fusion by Fleischmann and Pons. However, we have shown that the material is concentrated in the lattice due to the formation of deuterides due to pressure effects. Including processes with condensed deuterium. In theoretical physics, an appropriate fusion pressure is the conventional method. However, the low temperature fusion process can be achieved in many ways. This is considered to be contrary to the existing theory. To provide the highest deuterium pressure possible is desirable, and we believe that this method may involve sound waves, such as in experiments to study microgravity. We are envisioning this. Another method of generating high pressure is the use of a diamond anvil. use of magnetically induced pressure by localized domain wall movement with varying magnetic fields. including a method including.

The material of the invention may contain an element for increasing the susceptibility of the material to magnetic effects, for example It is desirable to incorporate a small amount of coir, which is less than % by weight. Also, high pressure It also includes variations in the method of cooling the material to below 0°C, for example -70°C. low temperature fusion Any method of induction may be developed, and the present invention does not rely solely on electrolytic methods.

As mentioned above, in one embodiment, the palladium is mixed with lithium. preferred Preferably, the amount of lithium is less than about 20% in the macroscopic area of the material, preferably about 1 Less than 0%, most preferably less than 5%.

In certain embodiments of the invention, the lithium used is enriched in the isotope Li6. I'm here. The normal proportion of Li6 in lithium is 7.4% by weight, and Lib It is thought that it contributes to the umium-deuterium reaction. A suitable concentration is the amount of lithium present. This provides a Li6 concentration of about 10% by weight of the film, which is typically greater than 20% by weight.

Lithium is incorporated into palladium by many different methods, including alloying, but Big difference between the melting point of lithium (-180°C) and palladium (-1800°C) The reason is that lithium has a very high vapor pressure at the melting point of palladium and is subject to evaporation. This means that it is more easily lost. Lithium is paralyzed in lithium salt solution. by using a nickel anode or by using a non-aqueous system containing e.g. a molten salt system. The palladium is incorporated electrochemically by using a stem. other possible One method is thermal diffusion of lithium atoms from the surface layer to which lithium is attached. , this layer is applied by plating or other deposition methods. The diffusion method is Other metals are known to those skilled in the art. For example, LiH and Pd spots in H/D atmosphere. A powder route starting with a powder may also be used.

Production process involving diffusion of lithium into palladium either electrochemically or thermally is recognized to form a concentration gradient, and the absolute value of the concentration and the slope of the gradient depend on the method used and the slope. and conditions. The concentration gradient is caused by local stress and palladium lattice point defects on the surface. It is desirable that the hydrogen/deuterium solubility and mobility be present in the effect on the heat generation effect. The fusion process is still poorly understood I don't have one, so I won't try to theorize.

It may further contain other metals or substances that do not improve the general properties.

Another type B of the present invention has a large capture cross section for palladium and muons. A palladium material comprising an additive is provided. Generally, the muon capture cross section is It increases as the atomic number increases. Preferably, the additive is rare earth, An element selected from thorium and scandium, and gadolinium or cesium is specifically indicated. Both actinides and some heavier elements such as uranium It should be considered after all.

The additive may be a single additive or a combination of two or more such additives. May be combined with other substances that do not adversely affect the heat generation process. There is no problem in the presence of a mixture of

A suitable amount of additive is less than 15 atomic %, preferably 8 atomic %, based on palladium. less than 1 atomic %, especially about 1 atomic %. The inventors determined that the amount of additive present (this affects the material's ability to capture muons) and additives A balance has been achieved between the adverse effects of I believe that I should.

The present invention also provides a method for carrying out the method at a temperature below ambient temperature, preferably less than 10°C, more preferably less than 0°C, and most preferably less than -10°C and, for example, at a temperature of about -40'C to -70°C. It also extends to improved low temperature fusion methods, including Therefore, this method efficiently dissipates heat. For example, excess heat is removed by liquid flow through the anode material while removing It is preferable to operate with external cooling and optionally with external cooling. . Especially when using aqueous electrolytes, the freezing point of the electrolyte should not be below the operating temperature. It is recognized that this should not be the case. And this is a salt or organic “freeze protector”. Achieved by adding a “stopping” substance, e.g. methanol or ethylene glycol. can do.

The present invention has also not been proposed previously and Utilizing materials with the desired combination of and diffusion properties, includes raising the This material is made of rare earths, such as cerium among others. yttrium, scandium, actinide, uranium, tantalum, niobium, barium Nadium, intermetallic compounds and metals with desired properties, and palladium um/silver alloys. These materials provide distributed hydrogen storage Can incorporate elements or compounds, among which Pd/Ag and L a Particular mention may be made of Nis.

In particular, in the case of uranium and actinides, radioactivity caused by high-energy radiation can be considered to be able to initiate any fusion reaction, and therefore The present invention contemplates the use of materials rich in radioactive isotopes. Of course, Care should be taken to follow accepted procedures when handling radioactive materials.

Some of these new materials require water to be used as electrodes in aqueous systems. formation of an active surface layer or competing reactions in the presence of Due to gas formation or loss of physical properties, it is not ideally suited and The method includes surface coating the material with palladium or palladium/silver alloys. . Such surface coatings can be applied by electroless plating, electroplating, sputtering or This can be accomplished by a number of methods, including thin film growth methods such as chemical vapor deposition. Ru.

The present invention further provides novel materials that are dispersed in a stable matrix by conventional metallurgical techniques. palladium and palladium/silver alloys among the seven is convenient.

Although it has been proposed to use titanium in "cold fusion" methods, the present invention Titanium dispersed in or surface coated with gold or palladium/silver and believe it is particularly advantageous for use in aqueous electrolyte systems. It will be done.

In another aspect, the invention provides palladium with a modified surface. child The modified surface serves one or more of the following purposes:

・Increase hydrogen/shuutilium adsorption ・Hydrogen/shuutilium desorption control and suppress undesired surface reactions. ・Controlling surface area -Managing surface properties, including controlling surface impurity levels; ・Providing desired dimensional stability If hydrogen adsorption is increased while simultaneously decreasing hydrogen desorption, the overall The effect is to increase the amount of hydrogen (and its isotopes) that can be contained within the material , increasing the chances of fusion or other heat-generating processes. It would be recognized that

Specifically, the invention provides a material comprising a surface coating or modified surface area. provide. The matrix of this material is palladium or an alloy of palladium or may be a solid solution.

electroless or electroplating, depending on the desired coating and matrix composition; Thin or thick film growth, including sputtering, chemical vapor deposition, and other suitable coatings. In addition to surface coatings that can be applied by methods selected from the Incorporating the desired element or compound into the surface region, thereby adding the element or compound to the electrode material. Involves creating a concentration gradient of a compound. This is from coating to matrix , generally achieved by diffusion using thermally induced diffusion. and methods for creating modified surface areas with respect to other materials. known to those skilled in the art. The inventors have proposed that such modified surface regions with concentration gradients The inventors believe that this is highly stressed and has many lattice defects; and the adsorption of its isotopes and their diffusivity within the material, and also the heat generation within the material. believe that they will contribute meaningfully to the process.

Suitable coatings according to the invention include in particular palladium and palladium/silver alloys.

For example, a palladium matrix is coated with palladium to coat it with palladium black. Surface coating may be desirable. Surface coatings also generally have large stresses. In addition, there are many point defects, and these can be solved by "cold fusion" or thermal fusion, as discussed earlier. Although this may be advantageous in the developmental process, the inventors I don't want to be bound by any theory.

The present invention uses the modified palladium material described above in a "cold fusion" type process. It includes things. The invention further provides that shuutilium in the material according to the invention is D20 is electrolyzed using a cathode made of the modified palladium material described above. Electrochemistry that generates heat of the "cold fusion" type, including condensation by provide a method for Moreover, the present invention provides an anode and a modified parasitic tube as described above. A "cold fusion" type of heat-generating electrochemical The present invention provides an electrolytic cell for use in a commercial manner. As an illustration of the invention, a small amount of additives Palladium containing I did it twice and made electrode rods with a diameter of 8 dishes. One sample of the electrode was placed under vacuum at 650″C. I annealed it for 1 hour. Annealed bar compared to non-annealed bar From the investigation of the microstructure of the non-annealed bars, the maximum dimension is less than 10 mm. In grain size, the aspect ratio of the grain is greater than 10, whereas the annealed bar is said to be recrystallized to a grain size of 10 to 40, and the aspect ratio is less than 10. It was shown that These rods were then “cold fused” under conditions reported in the literature. ” Used in an electrolytic cell.

Bars that have not been annealed will generate heat even after being charged for a considerable period of time. The annealed rods showed an excessive exothermic effect, whereas they did not show any vitality. , a fever suddenly occurred. Palladium is found in small amounts of aluminum, magnesium and nitrogen. In addition to nickel, silicon and silver, 0. OO2% boron, 0, OO1% copper , 0.001% iron, O, OO 1% platinum, 0, OO 3% gold and 0. OO It contained 3% calcium.

Yet another example is a 25%Ag-75%Pd alloy as a cathode for heavy water electrolysis. was used, and both Li0D and Na0D glue and O solution were used as electrolytes. 20 Current densities ranging from 0111 A/Cl11 to 750 mA/cd were used.

The detected products contained tritium and neutrons, which were fused together. I let it happen.

The inventors conducted studies using temperature-programmed reduction and electrochemical studies to Palladium hydride produced using LiCIH in water can be prepared using NaOH or Compared to hydrides using KOH, it is not stabilized for reasons that are not yet understood. I was able to conclude that.

Procedural amendment (formality) December 1991 ceremony date

Claims (19)

[Claims] 1. A composition in which low temperature fusion occurs when deuterium is incorporated; Palladium modified to change the local environment for deuterium under suitable conditions A composition comprising. 2. Claims in which palladium is combined with a material with a large muon capture cross section The composition according to item 1. 3. The combination material is selected from rare earths including yttrium and scandium. The composition according to claim 2, wherein the composition comprises: 4. the substance for combination is one or more of gadolinium and cerium; The composition according to claim 3. 5. The set according to claim 1, wherein palladium has a high and stable dislocation density. A product. 6. A composition according to claim 5, wherein palladium is coated thereon. . 7. The coating increases the stress on the palladium particles and/or reduces the point defect concentration. 7. A composition according to claim 6, which acts to increase. 8. Because the coating increases the adsorption of deuterium and/or The modified surface area on the palladium is effective to control the desorption of the palladium. 7. The composition of claim 6, comprising: 9. The modified surface region comprises palladium black or palladium-silver alloy. The composition according to claim 8. 10. Ingredients Cerium, Yttrium, Scandium, Actinide, Tantalum, Ni dispersed with one or more of vanadium, silver, LaNis, and titanium. Claim 1, comprising palladium, which is made of or alloyed with palladium. Composition of. 11. Claim 1, wherein the palladium has a particle size in the range of 10 to 40 μm. The composition according to any one of items 1 to 10. 12. Claim 11, wherein the particles have approximately a single aspect ratio. Composition of. 13. Claim 1 or 1, wherein the palladium is modified by the incorporation of lithium. Composition according to item 6. 14. 14. The composition of claim 13, wherein the lithium is enriched in 6Li. 15. Palladium is stated in any one of claims 1 to 14. By the low temperature fusion of deuterium incorporated into palladium, the composition A method for producing one or more of heat, neutrons and tritium. 16. Claim 15 carried out or disclosed at a temperature below ambient temperature. Method described. 17. The method according to claim 16, which is carried out or started at a temperature below 10°C. Method. 18. Lithium is carried out by electrolysis in a 6Li-rich lithium salt electrolyte. 18. A method according to claim 15, 16 or 17, characterized in that: 19. Modified palladium according to any one of claims 1 to 14 A low-temperature fusion electrochemical cell containing a cathode that is a fusion cell.