WO2019126206A1 - Calorimeter for low energy nuclear reaction experiments - Google Patents

Calorimeter for low energy nuclear reaction experiments Download PDF

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Publication number
WO2019126206A1
WO2019126206A1 PCT/US2018/066288 US2018066288W WO2019126206A1 WO 2019126206 A1 WO2019126206 A1 WO 2019126206A1 US 2018066288 W US2018066288 W US 2018066288W WO 2019126206 A1 WO2019126206 A1 WO 2019126206A1
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WO
WIPO (PCT)
Prior art keywords
core
calorimeter
gas
reaction chamber
operative
Prior art date
Application number
PCT/US2018/066288
Other languages
French (fr)
Inventor
Dennis G. LETTS
Carlos Ray JOBE
Michael Scott GUERRINA
III John Dewey WEAVER
Original Assignee
Ih Ip Holdings Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ih Ip Holdings Limited filed Critical Ih Ip Holdings Limited
Publication of WO2019126206A1 publication Critical patent/WO2019126206A1/en

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01KMEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K17/00Measuring quantity of heat

Definitions

  • the present invention relates generally to a calorimeter operative to measure heat from an exothermic reaction.
  • a calorimeter provides a high-temperature environment for an exothermic reaction chamber, and precisely measures any excess heat generated by an exothermic reaction.
  • the calorimeter may feature a thermally-conductive metal core, with a bore formed to hold an exothermic reaction chamber.
  • the core may also hold, in a plurality of bores, heater elements to heat the core and
  • thermocouples to monitor the core temperature. Seebeck effect thermoelectric generators (TEG) may cover substantially the entirety of the exterior of the core. The TEGs are biased against the core with spring washers. The TEGs may be substantially completely covered by heat sinks, and fans may direct convective airflow over the heat sinks. The calorimeter may be operated within a refrigerated container to further increase the temperature gradient across the TEGs. The TEGs may be connected in series, and their collective output voltage is determined by the temperature difference between their hot side, pressed against the core, and their cold side, cooled by the heat sinks and optionally convective airflow and/or a refrigerated environment.
  • the exothermic reaction may be triggered in a variety of ways, and excess heating of the core as a result of an exothermic reaction will be reflected in the TEG output voltage.
  • a gas manifold may facilitate experimentation by controlling the reaction chamber pressure and gas flow into and out of the reaction chamber. This facilitates experimentation using, e.g., hydrogen, deuterium, or some other gas, and allows for the collection of sample gas from the reactor.
  • At least one embodiment relates to a calorimeter operative to measure excess heat from an exothermic reaction.
  • the calorimeter includes a core of thermally conductive material.
  • a first bore operative to hold an exothermic reactor is formed in the core.
  • the calorimeter also includes plurality of thermoelectric generators (TEG).
  • Each TEG has a hot side and a cold side. The hot side of each TEG is affixed to the core.
  • the TEGs may be connected in series and are operative to generate an output voltage in response to the temperature of the core.
  • a calorimeter operative to measure heat from an exothermic reaction includes: a core comprising a thermally conductive material; a first bore defined in the core and operative to hold a reaction chamber; one or more second bores defined in the core, each second bore operative to hold a heating element; one or more third bores defined in the core, each third bore operative to hold a thermal sensor; and a plurality of thermoelectric generators, each operative to generate an output voltage in response to the temperature of the core, each thermoelectric generator having a hot side and a cold side, the hot side of each thermoelectric generator being in thermal communication with the core.
  • the core may be formed as a copper block.
  • thermoelectric generators may include Seebeck effect thermoelectric generators operative in a hot side temperature range from 120° C to 160° C.
  • the calorimeter may include a thermally conductive material interposed between each thermoelectric generator and the core.
  • thermoelectric generators may at least partially cover an outer surface of the core.
  • thermoelectric generator may be connected to the core with a retention clip.
  • thermoelectric generators may be biased towards the core with a predetermined force.
  • thermoelectric generators may be affixed to the core with shoulder bolts and spring washers, such that the spring washers are operative to apply a predetermined force biasing the thermoelectric generators against the core when the shoulder bolts are fully advanced.
  • One or more heat sinks may be in thermal communication with respective cold sides of the thermoelectric generators.
  • One or more fans operative may direct convective airflow over the heat sinks.
  • a refrigerated housing may be operative to contain the calorimeter in an environment having a predetermined ambient temperature.
  • a gas flow manifold may be operative to supply one or more gases to a reaction chamber in the first bore, the gas flow manifold including: a mass flow controller operative to control the flow of one or more supply gases into the reaction chamber at a predetermined rate; one or more supply gas storage chambers in gas flow relationship with the mass flow controller; one or more supply gas valves, each interposed between a respective supply gas storage chamber and the mass flow controller and operative to selectively isolate the supply gas storage chamber from the mass flow controller; and a port in gas flow relationship with the reaction chamber and operative to connect to a vacuum pump.
  • the mass flow controller and the one or more supply gas valves may be actuated electronically under the control of software executing on a processor.
  • the gas flow manifold may be further operative to sample gas from the reaction chamber, and further comprises a sample gas storage chamber removably connected to the gas flow manifold and in gas flow relationship with the reaction chamber.
  • the gas flow manifold may further include a coupling interposed between the sample gas storage chamber and the manifold, the coupling including: first and second sample gas valves; and a linking connector interposed between the first and second sample gas valves; wherein when the first and second sample gas valves are open, gas is operative to flow from the reaction chamber into the sample gas storage chamber; and wherein, when the first and second sample gas valves are closed, the second valve and sample gas storage chamber may be removed from the manifold at the linking connector.
  • the first and second sample gas valves may be manually actuated.
  • the first and second sample gas valves may be actuated electronically under the control of software executing on a processor.
  • the calorimeter may further include: a cylindrical gas reaction chamber operative to house an exothermic reaction; one or more toroidal magnets positioned around the gas reaction chamber; a gas flow connector at one end of the gas reaction chamber to connect to a gas flow manifold in gas flow relationship; and a flange at another end of the gas reaction chamber operative to retain the magnets around the gas reaction chamber.
  • the gas from the reaction chamber may be sampled in real time.
  • the gas from the reaction chamber may be analyzed for one or more signature gases.
  • the gas sample from the reaction chamber may be analyzed for energetic particle detection or radio frequency detection.
  • the calorimeter may further include an optical window for detecting an optical signal.
  • FIG. 1 is a section view of a calorimeter according to at least one embodiment.
  • FIG. 2 is a perspective view of a calorimeter core formed as a block according to at least one embodiment.
  • FIG. 3 is a plan view of first, second, and third bores formed in the calorimeter core according at least one embodiment.
  • FIG. 4 is a perspective view of TEGs covering the calorimeter core.
  • FIG. 5 is a perspective view of TEGs in retention clips.
  • FIG. 6 is a sectional view of a shoulder bolt and Bellville washers biasing a TEG against the calorimeter core.
  • FIG. 7A is a perspective view depicting heat sinks mounted over TEGs on one face of the calorimeter core.
  • FIG. 7B is a side view of heat sinks mounted over TEGs on one face of the calorimeter core.
  • FIG. 8 is a perspective view depicting heat sinks mounted over TEGs on all faces of the calorimeter block according to at least one embodiment.
  • FIG. 9 is a perspective view depicting fans directing convective air over the heat sinks according to at least one embodiment.
  • FIG. 10 depicts the convective block and fans in a refrigerated housing according to at least one embodiment.
  • FIG. 11 is a perspective view depicting couplings to the exothermic reaction chamber in the calorimeter according to at least one embodiment.
  • FIG. 12 is a more detailed perspective view of the couplings.
  • FIG. 13 is a perspective view of a gas flow manifold operative to connect to an exothermic reaction chamber in the calorimeter according to at least one embodiment.
  • FIG. 14 is a section view of an exothermic reaction chamber having a magnet retention flange according to at least one embodiment.
  • FIG. 15 is a section view of an exothermic reaction chamber in a calorimeter according to at least one embodiment.
  • an exothermic reaction chamber comprises a cylinder formed of a rugged metal, e.g., stainless steel.
  • the chamber may have an outer form as a right circular cylinder dimensioned as approximately one foot in longitudinal length and an inch in diameter taken perpendicular to the length.
  • the cylinder can be hermetically sealed and configured with fittings allowing the interior to be drawn to a vacuum of 10 6 - 10 7 Torr.
  • the interior wall of the cylinder may be plated with gold (Au), and then with palladium (Pd).
  • Hydrogen (H) has a known affinity for the metal lattice of palladium, and an aversion to that of gold.
  • the gold may act as a seal to maintain hydrogen nuclei in the palladium.
  • Gold also exhibits surface phenomena, such as phonon and/or plasmon activity, which may contribute to the exothermic reaction within the hydrogen-loaded palladium.
  • the metal cylinder can be grounded (cathode), and an anode rod can be positioned in the center.
  • Hydrogen or deuterium H, a stable isotope of H, also known as“heavy H” can be introduced into the cylinder at a low pressure. High-voltage, low-current power can be applied to the anode.
  • the high voltage along the anode generates an electric field directed radially outwardly, which ionizes the deuterium and accelerates it toward and into the palladium coating.
  • the palladium may achieve a 0.85 - 0.90 loading ratio.
  • Deuterium nuclei in the palladium metal lattice may then fuse.
  • palladium may be used as described, in some embodiments, a transition metals such as nickel, platinum, etc., can be used to plate the electrode.
  • FIG. 1 is a functional section diagram of some parts of a calorimeter 10 operative to measure the excess heat of an exothermic reaction, according to one or more embodiments of the present invention.
  • the calorimeter 10 includes a core 12 illustrated as a rectangular block in the drawings.
  • the core 12 in other embodiments can be formed in other shapes.
  • the core 12 serves as a structural frame, and as a bulk thermal mass that stores and distributes thermal energy and moderates against temporally rapid heat fluctuations and high-gradients in spatial temperature patterns. Thus, the core 12 regularizes heat flow and prevents excessive temperature
  • the core 12 in various embodiments is constructed of material having a high melting point, and good thermal conductivity.
  • the core 12, for example, may be constructed of one or metals.
  • the core 12 may be constructed of, in whole or at least in part, copper.
  • core 12 is constructed as a rectangular block of copper having bores for use as described in the following.
  • other metals may be used, taking into account their thermal transfer properties.
  • the core 12 is formed from aluminum, due to its thermal conductivity and ease of machining.
  • An exothermic reaction chamber 68 in some experiments surrounded by magnets 70, is disposed in a first bore 14 formed in the core 12.
  • the core 12 is heated to a relatively high temperature, such as 150 ° - 300° C, by a plurality of heating elements 74, each disposed in a respective one of multiple second bores 16 defined in the core 12.
  • the temperature of the core 12 is monitored by a plurality of thermal sensors 76, each disposed in a in a respective one of multiple third bores 18 defined in the core.
  • the thermal sensors 76 may be, for example, thermocouples.
  • a controller 100 receives input from the thermal sensors 76, and controls the heating elements 74, to maintain the core 12 temperature at a predetermined level.
  • the heating elements 74, thermal sensors 76, and exothermic reaction chamber 68 are each in thermal communication with the core 12.
  • the heating elements 74, thermal sensors 76, and exothermic reaction chamber 68 are in thermal communication with each other via the core 12.
  • a gas flow manifold 48 controls the pressure and flow of gases into and out of the exothermic reaction chamber 68, facilitating experimentation with various conditions and reaction triggering events.
  • the controller 100 can provide high voltage (e.g., 5 kVDC) to an anode in the exothermic reaction chamber 68, and in some embodiments may superimpose an RF signal on the provided voltage.
  • the entire calorimeter 10 may be placed in a refrigerated container.
  • The“hot side” and“cold side” of a typical TEG are indicated by the manufacturer so as to assure proper orientation of the generator in use.
  • the cold sides of some manufactured TEGs have part numbers or other textual or graphical indications.
  • the actual temperature of any given TEG side of course may vary according to its placement and use.
  • the“hot side” faces or thermally contacts a heat source or surface and the“cold side” faces away so as to cool radiantly or by thermal contact with a cooling device, structure, or flow.
  • the“hot side” typically has a higher temperature than the“cold side.”
  • the hot and cold sides may be temperature equilibrated according to conditions of their environment. Nonetheless, the sides of a TEG can be described for nominal purposes herein as hot and cold sides without ambiguity according to the construction and expected use of the TEG, for example according to manufacturer specifications.
  • FIG. 2 illustrates the core 12 of the calorimeter 10 as a metal block.
  • the core 12 holds an exothermic reaction chamber 68 (FIG. 1) and optionally magnets 70 (FIG. 1).
  • the core 12 can also hold heating elements 74 (FIG. 1) to heat the core 12, and thermal sensors 76 (FIG.
  • the core 12 spreads heat evenly from the heating elements 74 around the exothermic reaction chamber 68 and magnets 70. Additionally, the core 12 quickly conducts excess heat from the exothermic reaction chamber 68 to the exterior surface of the core 12.
  • the core 12 may completely or partially cover or surround the exothermic reaction chamber 68 and magnets 70, and additionally has room for the heating elements 74 and thermal sensors 76. Accordingly, the size or dimensions of the core 12 may exceed dimensions of the exothermic reaction chamber 68 and magnets 70. However, the core 12 is not required to mimic the shape of the exothermic reaction chamber 68. In the illustrated embodiment of at least FIGS. 2-4, the core 12 is rectangular (other regular polygonal shape may also or alternatively be used), with flat sides to which the“hot side” of TEGs 20 may be affixed. In the embodiment depicted in FIG. 2, the core 12 has a rectangular block shape, with: a square cross-sectional profile, which may have sides dimensioned as approximately three inches; and a longitudinal dimension longer than the sides, for example a longitudinal length extending approximately one foot.
  • the core 12 has a number of longitudinally defined holes, or bores 14, 16, 18 drilled or otherwise formed therein.
  • the first bore 14 is of sufficient diameter to accommodate an exothermic reaction chamber 68 and magnets 70.
  • magnets 70 arrayed around the exothermic reaction chamber 68 make solid, constant contact with the inner walls of the first bore 14.
  • the first bore 14 may be tapped to receive a threaded portion of the exothermic reaction chamber 68.
  • the second bores 16 are shown as positioned between the central first bore 14 and planar sides of the core 12.
  • the second bores are sized, in diameter and depth, to accommodate heating elements 74.
  • the heating elements 74 may comprise electrical resistive heating elements, which may be cylindrical in shape.
  • the plurality of second bores 16 may be formed all the way through the core 12, and two heating elements 74, each of which may be less than half the length of the core 12, may be inserted into the second bores 16 from either end of the core 12.
  • a plurality of second bores 16 is formed in the opposite end of the core 12, that are not aligned with the second bores 16 formed in the first end of the core 12. This may evenly heat the core 12.
  • the heating elements 74 are operative to heat the core 12 to 150° - 300° C.
  • a suitable heating element 74 is model SWH16519-00 available from Watlow Electric Manufacturing Company, Inc. of St. Louis, Missouri.
  • the third bores 18 are shown as positioned between the central first bore 14 and comers of the core 12 defined at the junctions of the planar sides of the core 12.
  • the third bores are sized, in diameter and depth, to accommodate thermal sensors 76.
  • the thermal sensors 76 may be cylindrical in shape. The thermal sensor 76 are operative to monitor the temperature of the core 12.
  • the second bores 16 may be formed deeply enough that, when installed, the most sensitive portion of the thermal sensors 76 are even with the center of the exothermic reaction chamber 68, where an exothermic reaction may be most likely to occur.
  • the thermal sensors 76 in at least one embodiment are precise to 0.1° C and withstand temperatures up to 1100° C.
  • a suitable thermal sensor for use is a thermocouple model TJ72-CASS-18U-6-CC-SB available from Omega Engineering, Inc. of Stamford, Connecticut.
  • FIG. 4 depicts the core 12 with TEGs 20 covering substantially the entirety of its external surface.
  • the TEGs 20 in the illustrated embodiment are Seebeck effect devices, which output a DC voltage dependent on the difference in temperature between“hot” and“cold” sides of the device 20.
  • Each TEG 20 has a positive and negative terminal.
  • the TEGs may be all wired in series for additive voltage output - that is, the positive terminal of each TEG 20 is connected to the negative terminal of the next TEG 20, and the positive terminal of the last TEG 20 and the negative terminal of the first TEG 20 are connected to a calibrated multimeter or other data recording device.
  • the TEGs may be wired in parallel relation for additive current output.
  • the TEGs may be wired independently.
  • a suitable TEG 20 for the core 12, other than the top, is model TEG1-PB-12611-6.0, and a suitable TEG 20 for the top of the core 12 (shown highest in FIG. 4) is model TEG1-PB- 07110-25, both available from Thermal Electronics, Inc. of Lake Elsinore, California. These TEGs 20 can withstand up to 300° C.
  • the TEGs 20 are shown in FIG. 4 to cover substantially all of the exterior surface core 12, including the top (shown highest in FIG. 4) and bottom (lowest and obscured from view in the perspective view of FIG. 4).
  • the TEGs 20 may be held firmly against the walls of the core 12 to obtain a consistent, optimal thermal conduction for thermal communication with the core 12.
  • TEGs 20 Attachment of TEGs 20 to metal surfaces may be accomplished via thermally conductive adhesive, such as epoxy. However, as some epoxies may not remain an effective adhesive at the anticipated high operating temperatures of the calorimeter 10. Accordingly, mechanical attachment of the TEGs 20 to the core 12 may be implemented.
  • the TEGs 20 may be attached directly to the core 12, such as by screws or other mechanical fasteners. However, the contact pressure by such attachment may change as the core 12 heated up. This may result in differing thermal conductivity due to changes in attachment pressure, which may damage the TEGs 20, which may be relatively fragile devices.
  • each TEG 20 may be biased against the core 12 with a constant force, such as by a mechanical spring.
  • TEG retention clips 22 are used to attach the TEGs 20 to the core 12.
  • FIG. 5 depicts the TEGs 20 and the retention clips 22.
  • a shoulder bolt 26 and Bellville washers 28 may be used.
  • a Bellville washer 28, also known as a conical spring washer, is a spring having a frustoconical shape, and adapted to be used on mechanical fasteners as a washer.
  • FIG. 6 depicts a shoulder bolt 26 disposed through a through-hole in a TEG retention clip 22, and into a threaded hole in the core 12.
  • the shoulder bolt 26 When the shoulder bolt 26 is tightened to the point that the bolt shoulder is flush with the face of the core 12, the head of the bolt 26 stops at a known distance d from the TEG retention clip 22.
  • the dimensions of the retention clip 22 and shoulder bolt 26 may be selected such that when one or more Bellville washers 28 are interposed on the bolt between the retention clip 22 and the bolt head - that is, confined within the distance d - the washers 28 are compressed and generate a known force along the longitudinal axis of the bolt 26. This operates to bias the retention clip 22, and hence the TEG 20, against the core 12 with the known force.
  • a thermally conductive material 24, supplied by the TEG manufacturer, may be interposed between the TEG 20 and the core 12.
  • the hot side of each TEG 20 directly contacts the metal core 12.
  • Seebeck effect devices exhibit an inherently non-linear relationship between temperature differential and output voltage. By maintaining a constant attachment bias, and by operating within a limited temperature range, the devices may be limited to a more linear range. Additionally, different TEG 20 devices may be utilized for different anticipated operating temperatures of the calorimeter 10, to achieve such linearity. In any event, the calorimeter 10 must be well calibrated before an exothermic reaction is triggered, to account for discrepancies.
  • FIGS. 7 A, 7B, and 8 depict heat sinks 30 over the TEGs 20.
  • the heat sinks 30 help the cold side of the TEGs 20 to maintain a constant, uniform temperature substantially cooler than that of the core 12 before, during, and after any exothermic reaction.
  • the heat sinks 30 may cover substantially all of the cold sides of the TEGs 20 as illustrated in FIG. 8.
  • the heat sinks 30 are attached to the core 12 with compression screws. Of course, the compression screws must not go through any TEG 20, to prevent damage.
  • the compression screws must not go through any TEG 20, to prevent damage.
  • the heat sinks 30 are formed from aluminum, due to its good thermal conductivity and ease of machining.
  • the heat sinks 30 may be formed from other material. As with any heat sink, a large surface area exposed to the air increases thermal transfer efficacy.
  • the heat sinks may be formed with fins, increasing the surface area and allowing air flow between the fins.
  • the fins are oriented vertically, although this is not a requirement.
  • FIG. 9 depicts one or more fans 32 disposed and oriented to generate convective airflow over the heat sinks 30, preferably in the direction of the fins. This helps remove heat from the cool side of the TEGs 20, creating a greater thermal differential between the hot and cold sides.
  • four 12V DC brushless fans 32 are placed beneath the calorimeter 10, and oriented so as to maximize convective airflow over and between the fins of the heat sinks 30. Such fans are commonly used in computer housings to cool electronics.
  • FIG. 10 depicts the calorimeter 10 - including the exothermic reaction chamber 68, metal core 12, TEGs 20, heat sinks 30, and convective airflow fans 32 - disposed in a
  • container 34 has a glass (or other transparent) door 36 for observing the calorimeter 10 during an experiment.
  • the cool side of the TEGs 20 is further lowered, and maintained at a constant temperature, against which changes in the temperature of the core 12 may be measured by changes in the TEG 20 output voltage.
  • water or other fluid may be sprayed on the calorimeter 10 in a low humidity environment to take advantage of evaporative cooling.
  • water or other fluid may be circulated over the surface of the calorimeter 10 in tubes or pipes with high thermal conductivity.
  • the calorimeter 10 may be immersed in an ice bath or fluid that is circulated through a chiller to maintain a constant low temperature. In general, any means of cooling the cooling the cold side of the TEGs 20 may be utilized.
  • FIG. 11 depicts the calorimeter 10 with the exothermic reaction chamber 68 installed within, and thus not visible in FIG. 11, in the first bore 14.
  • a sealing nut 40 is attached.
  • a safe high voltage connector 42 protrudes from the sealing nut 40, and a gas flow tube 44 connects to the interior of the reaction chamber 68.
  • FIG. 12 is an enlarged view of the gas flow tube 44, and an electrical connector 46, which may for example receive an RF signal.
  • electrical connections to the heating elements 74 and thermocouples 76, as well as both ends of the TEGs 20, will exit the top of the calorimeter 10.
  • a heat sink 30 may be fitted to the top, with provisions for these connectors to protrude through it.
  • FIG. 13 depicts a gas flow manifold 48, which facilitates implementation and investigation of triggering events for an exothermic reaction in the exothermic reaction chamber 68.
  • the manifold attaches to the gas flow tube 44 (Figs. 11, 12) at nut 50.
  • a port 52 allows a pressure meter to be attached, to monitor the pressure (vacuum) in the exothermic reaction chamber 68.
  • a port 54 allows for attachment to a vacuum pump, to evacuate the exothermic reaction chamber 68 to 10 6 -10 7 Torr prior to introducing hydrogen gas.
  • a particular gas flow valve 56 selectively isolates the port 54 from other elements of the manifold 48 after the desired vacuum is achieved. Additional gas flow valves 56 selectively close to isolate respective supply gas storage chambers 60 from the manifold 48 or open to permit the entry of respective gases from the gas storage chambers 60.
  • the gas flow valves 56 may be electronically actuated, and hence may be controlled by software executing on a processor. In other embodiments, the valves 56 may be manually actuated.
  • a mass flow controller 58 permits precise amounts of gas - stored, in one
  • one supply gas storage chamber 60 stores“light” hydrogen gas (H), and the other stores“heavy” hydrogen gas (deuterium).
  • Gas flow valves 56 isolate the supply gas storage chambers 60, and selectively allow gas to flow from one or the other through the mass flow controller 58 into the exothermic reaction chamber 68.
  • gas in the exothermic reaction chamber 68 may be sampled for analysis, such as by mass spectroscopy. For example, the presence of 4 He nuclei may indicate that a nuclear fusion reaction occurred in the exothermic reaction chamber 68.
  • the illustrated embodiment of the gas flow manifold 48 of FIG. 13 includes a sample gas storage chamber 62 for collection of gas from the exothermic reaction chamber 68.
  • the sample gas storage chamber 62 may be evacuated to a vacuum, along with the exothermic reaction chamber 68, by opening both of two sample gas valves 64 during the vacuum pump operation.
  • the sample gas valves 64 are then closed as one or more supply gases are introduced and an exothermic reaction is triggered in the exothermic reaction chamber 68.
  • the sample gas valves 64 may both be opened, and the pressure differential will transfer gas from the exothermic reaction chamber 68 into the sample gas storage chamber 62.
  • both sample gas valves 64 may be closed, and a linking connector 66 therebetween, illustrated as a connection nut that can be loosened, can be used to release the connection between the first sample gas valve 64, on the manifold side of the linking connector 66, and the second sample gas valve 64, on the sample gas storage chamber 62 side of the linking connector 66.
  • a linking connector 66 illustrated as a connection nut that can be loosened, can be used to release the connection between the first sample gas valve 64, on the manifold side of the linking connector 66, and the second sample gas valve 64, on the sample gas storage chamber 62 side of the linking connector 66.
  • the first sample gas valve 64 remains connected to the manifold 48
  • the second sample gas valve 64 remains connected to the sample gas storage chamber 62.
  • instrumentation such as a mass spectrometer for testing of the collected gas.
  • the first and second sample gas valves 64, and the linking connector 66 interposed therebetween serve as a coupling interposed between the sample gas storage chamber 62 and
  • an entrance port to an instrument may replace the gas storage chamber 62, and the analysis of sample gas performed in“real time.”
  • Real time gas sample analysis can be used to monitor the progress of an exothermic reaction in the reaction chamber 68.
  • the analysis may be focused on detecting an indication that a reaction is actually taking place.
  • the analysis can also be used as feedback to control the reaction.
  • the sample gas valves 64 are manually actuated; in other embodiments, they may be electronically actuated and controlled by software executing on a processor. By programming the processor, gas samples can be extracted at a pre-determined time interval by a pre-determined amount. The gas samples can be used to detect one or more signature gases.
  • the content of a sample can be analyzed to determine how much reactant gas, e.g., deuterium gas, has been consumed or how much resultant gas, e.g., 4 He, has been produced.
  • the amount of helium detected in the gas sample may indicate whether the reaction rate is slowing down or will slow down imminently.
  • the reaction rate can be accelerated or moderated based on the amount of helium detected in the samples to maintain a desired reaction rate.
  • the mass flow controller 58 can be controlled to allow more gas supply to flow from the gas storage chambers 60 into the reaction chamber 68.
  • gas samples extracted in real time may be analyzed to detect energetic particles.
  • energetic particle detection can be carried out by placing detectors around the calorimeter 10.
  • one or more ports may be added to facilitate RF detection. Additionally or alternatively, an optical window may be introduced on the calorimeter 10 to allow optical signals to pass through. Often, optical signals are reliable indicators of how a reaction is progressing.
  • more than two supply gas storage chambers 60 may be provided, and/or more than one sample gas storage chamber 62 may be provided, as desired or required for a given experiment.
  • a suitable supply/sample gas storage chamber is the HydroStik lO-liter canister available from Jameco Electronics of Belmont, California.
  • FIG. 14 depicts an exothermic reaction chamber 68, according to one embodiment, which may function as a gas reaction chamber.
  • the reaction chamber 68 includes the sealing nut 40 and gas flow tube 44.
  • one or more generally toroidal magnets 70 surround the reaction chamber 68.
  • One feature of the reaction chamber 68 is a flange 72 on the end opposite the sealing nut 40 - that is, the end of the reaction chamber 68 that is inserted into the first bore 14 in the core 12.
  • the flange 72 acts to retain the magnets 70 as the reaction chamber 68 is removed from the core 12.
  • the flange also allows the end of the reaction chamber 68 to be attached and sealed by orbital welding, yielding a stronger and more robust chamber 68.
  • FIG. 15 depicts a functional block diagram of a complete and functional calorimeter 10, according to embodiments of the present invention.
  • the exothermic reaction chamber 68 comprises a metal container 78 plated with a layer of gold 82 and a layer of palladium 84, and contains an anode 86.
  • a lid 88 seals the exothermic reaction chamber 68, with a gas flow pass- through 90.
  • a Teflon cap or spacer 92 insulates the anode 86 in the small region on which the metal container 78 is not plated with gold 82 and palladium 84, to prevent arcing between the anode 86 and this portion of the metal container 78 under very high voltage.
  • one or more magnets surround the exothermic reaction chamber 68.
  • the exothermic reaction chamber 68, and the magnets if used, are disposed in a central bore of the core 12.
  • a feature 80 between the container 78 and core 12 represents, in various embodiments, one or more of: one or magnets, and a thermally conductive material.
  • a plurality of heating elements 74 are disposed in second bores 16, and operate to heat the core 12 to a predetermined temperature (e.g., 150° - 300° C).
  • a predetermined temperature e.g. 150° - 300° C.
  • thermocouples 76 are disposed in third bores 18, and operative to monitor the temperature of the core 12, allowing for a closed-loop control system to maintain the core 12 at a steady, predetermined temperature.
  • the trigger may comprise the application of high voltage (e.g., 5 kV) at low current between the anode 86 and metal container 78 (grounded to act as cathode).
  • the trigger may comprise the high DC voltage with an RF signal superimposed, e.g., at a resonant frequency.
  • the trigger voltage generates a very low current, very little power is input to the system by triggering the exothermic reaction.
  • the triggering power may be 0.1 W.
  • the entirety of any temperature rise of the core 12 may be attributed to an exothermic reaction in the exothermic reaction chamber 68.
  • Such a thermal rise is detected by monitoring the output voltage of the gas storage chambers 60 TEGs 20, which may be series connected, and which may cover substantially the entirety of the external surface of the core 12.
  • the TEG retention clips 22 and thermal transfer material 24 (Fig. 6) may be used in the calorimeter 10 in FIG. 15.
  • the TEGs 20 are covered by heat sinks 30 to aid in cooling the cold side of the TEGs 20.
  • cooling is further supplemented by convective airflow and/or a refrigerated ambient environment.

Abstract

A calorimeter provides a temperature-controlled environment for an exothermic reaction chamber, and precisely measures any excess heat generated by an exothermic reaction. The calorimeter features a thermally-conductive metal core, with a bore formed to hold an exothermic reaction chamber. The core also holds, in a plurality of bores, heater elements to heat the core and thermocouples to monitor the core temperature. The TEGs can be biased against the core with spring washers. The TEGs may be connected in series, and their collective output voltage is determined by the temperature difference between their hot side, pressed against the core, and their cold side, cooled by the heat sinks and convective airflow. The exothermic reaction may be triggered in a variety of ways, and excess heating of the core as a result of an exothermic reaction will be reflected in the TEG output voltage.

Description

CALORIMETER FOR LOW ENERGY NUCLEAR REACTION EXPERIMENTS
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of priority of U.S. provisional patent application no. 62/607,192, titled“CALORIMETER FOR LOW ENERGY NUCLEAR REACTION
EXPERIMENTS,” filed on December 18, 2017, which is incorporated herein in its entirety by this reference.
FIELD OF INVENTION
[0002] The present invention relates generally to a calorimeter operative to measure heat from an exothermic reaction.
BACKGROUND
[0003] The release of thermal energy has been observed when hydrogen/deuterium reaches high loading in a variety of metals or alloys. This thermal energy has been attributed to exothermic reactions between occluded nuclei. In one theory, two deuterium nuclei, when trapped in the small confinement inside the metal lattice, have a wide spread of momentum based on the Heisenberg uncertainty principle. The combined probability of two deuterium nuclei having requisite momenta to overcome the Coulomb barrier may become statistically significant, triggering fusion reactions in the trapped deuterium gas. According to a second theory, the two trapped deuterium nuclei overcome the Coulomb barrier by going through a quantum tunnel to reach the lower energy state, i.e., to form a 4He nucleus. [0004] Low-energy nuclear reactions (LENR) investigations resulting in observations of thermal energy generation have been replicated around the world. Various conditions, in which the generation of heat can be triggered at will and with control, have been documented.
However, the triggering of exothermic reactions to generate heat in a metal or alloy loaded with hydrogen/deuterium are a topic of significant ongoing theoretical and practical research. A significant impediment to the systematic exploration of such triggering mechanisms is the lack of a consistent, reliable, and calibrated systems, and methods for their use, for both detecting and quantifying exothermic reactions if and when they do occur, particularly at relatively high temperatures.
SUMMARY
[0005] The following presents a simplified summary of the disclosure in order to provide a basic understanding to those of skill in the art. This summary is not an extensive overview of the disclosure and is not intended to identify key/critical elements of embodiments of the invention or to delineate the scope of the invention. The sole purpose of this summary is to present some concepts disclosed herein in a simplified form as a prelude to the more detailed description that is presented later.
[0006] According to one or more embodiments described and claimed herein, a calorimeter provides a high-temperature environment for an exothermic reaction chamber, and precisely measures any excess heat generated by an exothermic reaction. The calorimeter may feature a thermally-conductive metal core, with a bore formed to hold an exothermic reaction chamber. The core may also hold, in a plurality of bores, heater elements to heat the core and
thermocouples to monitor the core temperature. Seebeck effect thermoelectric generators (TEG) may cover substantially the entirety of the exterior of the core. The TEGs are biased against the core with spring washers. The TEGs may be substantially completely covered by heat sinks, and fans may direct convective airflow over the heat sinks. The calorimeter may be operated within a refrigerated container to further increase the temperature gradient across the TEGs. The TEGs may be connected in series, and their collective output voltage is determined by the temperature difference between their hot side, pressed against the core, and their cold side, cooled by the heat sinks and optionally convective airflow and/or a refrigerated environment. The exothermic reaction may be triggered in a variety of ways, and excess heating of the core as a result of an exothermic reaction will be reflected in the TEG output voltage. A gas manifold may facilitate experimentation by controlling the reaction chamber pressure and gas flow into and out of the reaction chamber. This facilitates experimentation using, e.g., hydrogen, deuterium, or some other gas, and allows for the collection of sample gas from the reactor.
[0007] At least one embodiment relates to a calorimeter operative to measure excess heat from an exothermic reaction. The calorimeter includes a core of thermally conductive material. A first bore operative to hold an exothermic reactor is formed in the core. A plurality of second bores, each operative to hold a heating element, is formed in the core. A plurality of third bores, each operative to hold a thermocouple, is formed in the core. The calorimeter also includes plurality of thermoelectric generators (TEG). Each TEG has a hot side and a cold side. The hot side of each TEG is affixed to the core. The TEGs may be connected in series and are operative to generate an output voltage in response to the temperature of the core.
[0008] In at least one embodiment, a calorimeter operative to measure heat from an exothermic reaction includes: a core comprising a thermally conductive material; a first bore defined in the core and operative to hold a reaction chamber; one or more second bores defined in the core, each second bore operative to hold a heating element; one or more third bores defined in the core, each third bore operative to hold a thermal sensor; and a plurality of thermoelectric generators, each operative to generate an output voltage in response to the temperature of the core, each thermoelectric generator having a hot side and a cold side, the hot side of each thermoelectric generator being in thermal communication with the core.
[0009] The core may be formed as a copper block.
[0010] There may be a plurality of second bores defined in the core evenly spaced radially around the first bore.
[0011] There may be a plurality of third bores defined in the core evenly spaced radially around the first bore.
[0012] The thermoelectric generators may include Seebeck effect thermoelectric generators operative in a hot side temperature range from 120° C to 160° C.
[0013] The calorimeter may include a thermally conductive material interposed between each thermoelectric generator and the core.
[0014] The thermoelectric generators may at least partially cover an outer surface of the core.
[0015] Each thermoelectric generator may be connected to the core with a retention clip.
[0016] The thermoelectric generators may be biased towards the core with a predetermined force.
[0017] The thermoelectric generators may be affixed to the core with shoulder bolts and spring washers, such that the spring washers are operative to apply a predetermined force biasing the thermoelectric generators against the core when the shoulder bolts are fully advanced.
[0018] One or more heat sinks may be in thermal communication with respective cold sides of the thermoelectric generators. [0019] One or more fans operative may direct convective airflow over the heat sinks.
[0020] A refrigerated housing may be operative to contain the calorimeter in an environment having a predetermined ambient temperature.
[0021] A gas flow manifold may be operative to supply one or more gases to a reaction chamber in the first bore, the gas flow manifold including: a mass flow controller operative to control the flow of one or more supply gases into the reaction chamber at a predetermined rate; one or more supply gas storage chambers in gas flow relationship with the mass flow controller; one or more supply gas valves, each interposed between a respective supply gas storage chamber and the mass flow controller and operative to selectively isolate the supply gas storage chamber from the mass flow controller; and a port in gas flow relationship with the reaction chamber and operative to connect to a vacuum pump.
[0022] The mass flow controller and the one or more supply gas valves may be actuated electronically under the control of software executing on a processor.
[0023] The gas flow manifold may be further operative to sample gas from the reaction chamber, and further comprises a sample gas storage chamber removably connected to the gas flow manifold and in gas flow relationship with the reaction chamber.
[0024] The gas flow manifold may further include a coupling interposed between the sample gas storage chamber and the manifold, the coupling including: first and second sample gas valves; and a linking connector interposed between the first and second sample gas valves; wherein when the first and second sample gas valves are open, gas is operative to flow from the reaction chamber into the sample gas storage chamber; and wherein, when the first and second sample gas valves are closed, the second valve and sample gas storage chamber may be removed from the manifold at the linking connector. [0025] The first and second sample gas valves may be manually actuated.
[0026] The first and second sample gas valves may be actuated electronically under the control of software executing on a processor.
[0027] The calorimeter may further include: a cylindrical gas reaction chamber operative to house an exothermic reaction; one or more toroidal magnets positioned around the gas reaction chamber; a gas flow connector at one end of the gas reaction chamber to connect to a gas flow manifold in gas flow relationship; and a flange at another end of the gas reaction chamber operative to retain the magnets around the gas reaction chamber.
[0028] The gas from the reaction chamber may be sampled in real time.
[0029] The gas from the reaction chamber may be analyzed for one or more signature gases.
[0030] The gas sample from the reaction chamber may be analyzed for energetic particle detection or radio frequency detection.
[0031] The calorimeter may further include an optical window for detecting an optical signal.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the invention are shown. However, this invention should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Like numbers refer to like elements throughout. Parts referenced in discussion of one drawing may not appear in that drawing, but are still provided with reference numbers in the text. [0033] FIG. 1 is a section view of a calorimeter according to at least one embodiment.
[0034] FIG. 2 is a perspective view of a calorimeter core formed as a block according to at least one embodiment.
[0035] FIG. 3 is a plan view of first, second, and third bores formed in the calorimeter core according at least one embodiment.
[0036] FIG. 4 is a perspective view of TEGs covering the calorimeter core.
[0037] FIG. 5 is a perspective view of TEGs in retention clips.
[0038] FIG. 6 is a sectional view of a shoulder bolt and Bellville washers biasing a TEG against the calorimeter core.
[0039] FIG. 7A is a perspective view depicting heat sinks mounted over TEGs on one face of the calorimeter core.
[0040] FIG. 7B is a side view of heat sinks mounted over TEGs on one face of the calorimeter core.
[0041] FIG. 8 is a perspective view depicting heat sinks mounted over TEGs on all faces of the calorimeter block according to at least one embodiment.
[0042] FIG. 9 is a perspective view depicting fans directing convective air over the heat sinks according to at least one embodiment.
[0043] FIG. 10 depicts the convective block and fans in a refrigerated housing according to at least one embodiment.
[0044] FIG. 11 is a perspective view depicting couplings to the exothermic reaction chamber in the calorimeter according to at least one embodiment.
[0045] FIG. 12 is a more detailed perspective view of the couplings. [0046] FIG. 13 is a perspective view of a gas flow manifold operative to connect to an exothermic reaction chamber in the calorimeter according to at least one embodiment.
[0047] FIG. 14 is a section view of an exothermic reaction chamber having a magnet retention flange according to at least one embodiment.
[0048] FIG. 15 is a section view of an exothermic reaction chamber in a calorimeter according to at least one embodiment.
DETAILED DESCRIPTION
[0049] These descriptions are presented with sufficient details to provide an understanding of one or more particular embodiments of broader inventive subject matters. These descriptions expound upon and exemplify particular features of those particular embodiments without limiting the inventive subject matters to the explicitly described embodiments and features. Considerations in view of these descriptions will likely give rise to additional and similar embodiments and features without departing from the scope of the inventive subject matters. Although the term“step” may be expressly used or implied relating to features of processes or methods, no implication is made of any particular order or sequence among such expressed or implied steps unless an order or sequence is explicitly stated.
[0050] Any dimensions expressed or implied in the drawings and these descriptions are provided for exemplary purposes. Thus, not all embodiments within the scope of the drawings and these descriptions are made according to such exemplary dimensions. The drawings are not made necessarily to scale. Thus, not all embodiments within the scope of the drawings and these descriptions are made according to the apparent scale of the drawings with regard to relative dimensions in the drawings. However, for each drawing, at least one embodiment is made according to the apparent relative scale of the drawing.
[0051] Like reference numbers used throughout the drawings depict like or similar elements. Unless described or implied as exclusive alternatives, features throughout the drawings and descriptions should be taken as cumulative, such that features expressly associated with some particular embodiments can be combined with other embodiments.
[0052] In at least one embodiment, an exothermic reaction chamber comprises a cylinder formed of a rugged metal, e.g., stainless steel. For example, the chamber may have an outer form as a right circular cylinder dimensioned as approximately one foot in longitudinal length and an inch in diameter taken perpendicular to the length. The cylinder can be hermetically sealed and configured with fittings allowing the interior to be drawn to a vacuum of 106 - 107 Torr. The interior wall of the cylinder may be plated with gold (Au), and then with palladium (Pd). Hydrogen (H) has a known affinity for the metal lattice of palladium, and an aversion to that of gold. Hence, the gold may act as a seal to maintain hydrogen nuclei in the palladium. Gold also exhibits surface phenomena, such as phonon and/or plasmon activity, which may contribute to the exothermic reaction within the hydrogen-loaded palladium. The metal cylinder can be grounded (cathode), and an anode rod can be positioned in the center. Hydrogen or deuterium ( H, a stable isotope of H, also known as“heavy H”) can be introduced into the cylinder at a low pressure. High-voltage, low-current power can be applied to the anode. In a process known as“dry electrolysis,” the high voltage along the anode generates an electric field directed radially outwardly, which ionizes the deuterium and accelerates it toward and into the palladium coating. The palladium may achieve a 0.85 - 0.90 loading ratio. Deuterium nuclei in the palladium metal lattice may then fuse. While palladium may be used as described, in some embodiments, a transition metals such as nickel, platinum, etc., can be used to plate the electrode.
[0053] Quantifying the heat produced, and documenting when it occurs, are important to validate exothermic reaction experiments, and to assess the efficacy of various triggering mechanisms. These tasks can be difficult, particularly at relatively high temperatures (compared to room temperature).
[0054] FIG. 1 is a functional section diagram of some parts of a calorimeter 10 operative to measure the excess heat of an exothermic reaction, according to one or more embodiments of the present invention. The calorimeter 10 includes a core 12 illustrated as a rectangular block in the drawings. The core 12 in other embodiments can be formed in other shapes. The core 12 serves as a structural frame, and as a bulk thermal mass that stores and distributes thermal energy and moderates against temporally rapid heat fluctuations and high-gradients in spatial temperature patterns. Thus, the core 12 regularizes heat flow and prevents excessive temperature
differentials in its mass. Thus the core 12 in various embodiments is constructed of material having a high melting point, and good thermal conductivity. The core 12, for example, may be constructed of one or metals.
[0055] The core 12 may be constructed of, in whole or at least in part, copper. In at least one embodiment, core 12 is constructed as a rectangular block of copper having bores for use as described in the following. In other embodiments, other metals may be used, taking into account their thermal transfer properties. In one embodiment the core 12 is formed from aluminum, due to its thermal conductivity and ease of machining.
[0056] An exothermic reaction chamber 68, in some experiments surrounded by magnets 70, is disposed in a first bore 14 formed in the core 12. The core 12 is heated to a relatively high temperature, such as 150 ° - 300° C, by a plurality of heating elements 74, each disposed in a respective one of multiple second bores 16 defined in the core 12. The temperature of the core 12 is monitored by a plurality of thermal sensors 76, each disposed in a in a respective one of multiple third bores 18 defined in the core. The thermal sensors 76 may be, for example, thermocouples. A controller 100 receives input from the thermal sensors 76, and controls the heating elements 74, to maintain the core 12 temperature at a predetermined level. The heating elements 74, thermal sensors 76, and exothermic reaction chamber 68 are each in thermal communication with the core 12. Thus, the heating elements 74, thermal sensors 76, and exothermic reaction chamber 68 are in thermal communication with each other via the core 12.
[0057] In some embodiments, a gas flow manifold 48 controls the pressure and flow of gases into and out of the exothermic reaction chamber 68, facilitating experimentation with various conditions and reaction triggering events. The controller 100 can provide high voltage (e.g., 5 kVDC) to an anode in the exothermic reaction chamber 68, and in some embodiments may superimpose an RF signal on the provided voltage.
[0058] When an exothermic reaction is triggered in the exothermic reaction chamber 68, the heat of the reaction is in part conducted away by the core 12, raising the temperature of the core 12. This rise in temperature is detected by one or more TEGs 20, which partially surround the core 12. Each TEG generates a voltage proportional to the temperature difference between a “hot side,” which is pressed against the core 12, and a“cold side,” which faces away from the core 12. Due to the high temperature of the core 12, heat sinks 30 are affixed to the cold side of the TEGs 20 to help cool the cold side, to maintain a thermal differential. In some embodiments, fans (not shown) direct convective cooling air over the fins of the heat sinks 30. In some embodiments, the entire calorimeter 10 may be placed in a refrigerated container. [0059] The“hot side” and“cold side” of a typical TEG are indicated by the manufacturer so as to assure proper orientation of the generator in use. For example, the cold sides of some manufactured TEGs have part numbers or other textual or graphical indications. The actual temperature of any given TEG side of course may vary according to its placement and use. In typical use, the“hot side” faces or thermally contacts a heat source or surface and the“cold side” faces away so as to cool radiantly or by thermal contact with a cooling device, structure, or flow. Thus, in use, the“hot side” typically has a higher temperature than the“cold side.” However, when not installed upon a heat source and in use, the hot and cold sides may be temperature equilibrated according to conditions of their environment. Nonetheless, the sides of a TEG can be described for nominal purposes herein as hot and cold sides without ambiguity according to the construction and expected use of the TEG, for example according to manufacturer specifications.
[0060] The above description of the structure and operation of the calorimeter 10 provides an overview of various embodiments of the present invention. Each of its constituent parts is disclosed in greater detail herein. Note that a benefit of the calorimeter 10 described herein is its flexibility of use. Accordingly, it is important to keep in mind that, in any given implementation and us, some or all of the features, parts, systems, components, and functions described herein may be present or utilized; while some features and elements described herein may be omitted in some implementations and uses.
[0061] FIG. 2 illustrates the core 12 of the calorimeter 10 as a metal block. The core 12 holds an exothermic reaction chamber 68 (FIG. 1) and optionally magnets 70 (FIG. 1). The core 12 can also hold heating elements 74 (FIG. 1) to heat the core 12, and thermal sensors 76 (FIG.
1) to monitor its temperature. The core 12 spreads heat evenly from the heating elements 74 around the exothermic reaction chamber 68 and magnets 70. Additionally, the core 12 quickly conducts excess heat from the exothermic reaction chamber 68 to the exterior surface of the core 12.
[0062] The core 12 may completely or partially cover or surround the exothermic reaction chamber 68 and magnets 70, and additionally has room for the heating elements 74 and thermal sensors 76. Accordingly, the size or dimensions of the core 12 may exceed dimensions of the exothermic reaction chamber 68 and magnets 70. However, the core 12 is not required to mimic the shape of the exothermic reaction chamber 68. In the illustrated embodiment of at least FIGS. 2-4, the core 12 is rectangular (other regular polygonal shape may also or alternatively be used), with flat sides to which the“hot side” of TEGs 20 may be affixed. In the embodiment depicted in FIG. 2, the core 12 has a rectangular block shape, with: a square cross-sectional profile, which may have sides dimensioned as approximately three inches; and a longitudinal dimension longer than the sides, for example a longitudinal length extending approximately one foot.
[0063] As depicted in FIGS. 2 and 3, the core 12 has a number of longitudinally defined holes, or bores 14, 16, 18 drilled or otherwise formed therein. In the center of the core 12, the first bore 14 is of sufficient diameter to accommodate an exothermic reaction chamber 68 and magnets 70. Preferably, magnets 70 arrayed around the exothermic reaction chamber 68 make solid, constant contact with the inner walls of the first bore 14. The first bore 14 may be tapped to receive a threaded portion of the exothermic reaction chamber 68.
[0064] A plurality of second bores 16 - four, in the embodiment depicted in FIGS. 2 and 3 - is formed in the core 12, evenly spaced radially around the first bore 14. The second bores 16 are shown as positioned between the central first bore 14 and planar sides of the core 12. The second bores are sized, in diameter and depth, to accommodate heating elements 74. The heating elements 74 may comprise electrical resistive heating elements, which may be cylindrical in shape. In one embodiment, the plurality of second bores 16 may be formed all the way through the core 12, and two heating elements 74, each of which may be less than half the length of the core 12, may be inserted into the second bores 16 from either end of the core 12. In another embodiment, a plurality of second bores 16 is formed in the opposite end of the core 12, that are not aligned with the second bores 16 formed in the first end of the core 12. This may evenly heat the core 12. In one embodiment, the heating elements 74 are operative to heat the core 12 to 150° - 300° C. A suitable heating element 74 is model SWH16519-00 available from Watlow Electric Manufacturing Company, Inc. of St. Louis, Missouri.
[0065] A plurality of third bores 18 - also four, in the embodiment depicted in FIGS. 2 and 3 - is formed in the core 12, evenly spaced radially around the first bore 14, and generally disposed in between the plurality of second bores 16. The third bores 18 are shown as positioned between the central first bore 14 and comers of the core 12 defined at the junctions of the planar sides of the core 12. The third bores are sized, in diameter and depth, to accommodate thermal sensors 76. The thermal sensors 76 may be cylindrical in shape. The thermal sensor 76 are operative to monitor the temperature of the core 12. The second bores 16 may be formed deeply enough that, when installed, the most sensitive portion of the thermal sensors 76 are even with the center of the exothermic reaction chamber 68, where an exothermic reaction may be most likely to occur. The thermal sensors 76 in at least one embodiment are precise to 0.1° C and withstand temperatures up to 1100° C. A suitable thermal sensor for use is a thermocouple model TJ72-CASS-18U-6-CC-SB available from Omega Engineering, Inc. of Stamford, Connecticut.
[0066] FIG. 4 depicts the core 12 with TEGs 20 covering substantially the entirety of its external surface. The TEGs 20 in the illustrated embodiment are Seebeck effect devices, which output a DC voltage dependent on the difference in temperature between“hot” and“cold” sides of the device 20. Each TEG 20 has a positive and negative terminal. The TEGs may be all wired in series for additive voltage output - that is, the positive terminal of each TEG 20 is connected to the negative terminal of the next TEG 20, and the positive terminal of the last TEG 20 and the negative terminal of the first TEG 20 are connected to a calibrated multimeter or other data recording device. In other embodiments, the TEGs may be wired in parallel relation for additive current output. In yet other embodiments, the TEGs may be wired independently.
[0067] A suitable TEG 20 for the core 12, other than the top, is model TEG1-PB-12611-6.0, and a suitable TEG 20 for the top of the core 12 (shown highest in FIG. 4) is model TEG1-PB- 07110-25, both available from Thermal Electronics, Inc. of Lake Elsinore, California. These TEGs 20 can withstand up to 300° C.
[0068] The TEGs 20 are shown in FIG. 4 to cover substantially all of the exterior surface core 12, including the top (shown highest in FIG. 4) and bottom (lowest and obscured from view in the perspective view of FIG. 4). The TEGs 20 may be held firmly against the walls of the core 12 to obtain a consistent, optimal thermal conduction for thermal communication with the core 12.
[0069] Attachment of TEGs 20 to metal surfaces may be accomplished via thermally conductive adhesive, such as epoxy. However, as some epoxies may not remain an effective adhesive at the anticipated high operating temperatures of the calorimeter 10. Accordingly, mechanical attachment of the TEGs 20 to the core 12 may be implemented.
[0070] The TEGs 20 may be attached directly to the core 12, such as by screws or other mechanical fasteners. However, the contact pressure by such attachment may change as the core 12 heated up. This may result in differing thermal conductivity due to changes in attachment pressure, which may damage the TEGs 20, which may be relatively fragile devices.
[0071] Accordingly, each TEG 20 may be biased against the core 12 with a constant force, such as by a mechanical spring. In one embodiment, TEG retention clips 22 are used to attach the TEGs 20 to the core 12. FIG. 5 depicts the TEGs 20 and the retention clips 22. As depicted in FIG. 6, to achieve a constant or predetermined bias force pressing the TEGs 20 against the core 12, a shoulder bolt 26 and Bellville washers 28 may be used. A Bellville washer 28, also known as a conical spring washer, is a spring having a frustoconical shape, and adapted to be used on mechanical fasteners as a washer. FIG. 6 depicts a shoulder bolt 26 disposed through a through-hole in a TEG retention clip 22, and into a threaded hole in the core 12. When the shoulder bolt 26 is tightened to the point that the bolt shoulder is flush with the face of the core 12, the head of the bolt 26 stops at a known distance d from the TEG retention clip 22. The dimensions of the retention clip 22 and shoulder bolt 26 may be selected such that when one or more Bellville washers 28 are interposed on the bolt between the retention clip 22 and the bolt head - that is, confined within the distance d - the washers 28 are compressed and generate a known force along the longitudinal axis of the bolt 26. This operates to bias the retention clip 22, and hence the TEG 20, against the core 12 with the known force. This force will remain substantially constant throughout the small range of distances d that may result from thermal expansion over the anticipated range of operating temperatures of the calorimeter 10. In some embodiments, a thermally conductive material 24, supplied by the TEG manufacturer, may be interposed between the TEG 20 and the core 12. In other embodiments, the hot side of each TEG 20 directly contacts the metal core 12. [0072] In general, Seebeck effect devices exhibit an inherently non-linear relationship between temperature differential and output voltage. By maintaining a constant attachment bias, and by operating within a limited temperature range, the devices may be limited to a more linear range. Additionally, different TEG 20 devices may be utilized for different anticipated operating temperatures of the calorimeter 10, to achieve such linearity. In any event, the calorimeter 10 must be well calibrated before an exothermic reaction is triggered, to account for discrepancies.
[0073] FIGS. 7 A, 7B, and 8 depict heat sinks 30 over the TEGs 20. The heat sinks 30 help the cold side of the TEGs 20 to maintain a constant, uniform temperature substantially cooler than that of the core 12 before, during, and after any exothermic reaction. The heat sinks 30 may cover substantially all of the cold sides of the TEGs 20 as illustrated in FIG. 8. In one embodiment, the heat sinks 30 are attached to the core 12 with compression screws. Of course, the compression screws must not go through any TEG 20, to prevent damage. In one
embodiment, the heat sinks 30 are formed from aluminum, due to its good thermal conductivity and ease of machining. However, the heat sinks 30 may be formed from other material. As with any heat sink, a large surface area exposed to the air increases thermal transfer efficacy.
Accordingly, the heat sinks may be formed with fins, increasing the surface area and allowing air flow between the fins. In one embodiment, the fins are oriented vertically, although this is not a requirement.
[0074] FIG. 9 depicts one or more fans 32 disposed and oriented to generate convective airflow over the heat sinks 30, preferably in the direction of the fins. This helps remove heat from the cool side of the TEGs 20, creating a greater thermal differential between the hot and cold sides. In one embodiment, four 12V DC brushless fans 32 are placed beneath the calorimeter 10, and oriented so as to maximize convective airflow over and between the fins of the heat sinks 30. Such fans are commonly used in computer housings to cool electronics.
[0075] FIG. 10 depicts the calorimeter 10 - including the exothermic reaction chamber 68, metal core 12, TEGs 20, heat sinks 30, and convective airflow fans 32 - disposed in a
refrigerated container 34. In one embodiment, container 34 has a glass (or other transparent) door 36 for observing the calorimeter 10 during an experiment. By reducing the temperature of ambient air providing the convective airflow, the cool side of the TEGs 20 is further lowered, and maintained at a constant temperature, against which changes in the temperature of the core 12 may be measured by changes in the TEG 20 output voltage.
[0076] Other methods of cooling the cold side of the TEGs 20 are contemplated. In one embodiment, water or other fluid may be sprayed on the calorimeter 10 in a low humidity environment to take advantage of evaporative cooling. In one embodiment water or other fluid may be circulated over the surface of the calorimeter 10 in tubes or pipes with high thermal conductivity. In one embodiment, the calorimeter 10 may be immersed in an ice bath or fluid that is circulated through a chiller to maintain a constant low temperature. In general, any means of cooling the cooling the cold side of the TEGs 20 may be utilized.
[0077] FIG. 11 depicts the calorimeter 10 with the exothermic reaction chamber 68 installed within, and thus not visible in FIG. 11, in the first bore 14. A sealing nut 40 is attached. A safe high voltage connector 42 protrudes from the sealing nut 40, and a gas flow tube 44 connects to the interior of the reaction chamber 68. FIG. 12 is an enlarged view of the gas flow tube 44, and an electrical connector 46, which may for example receive an RF signal. Although not depicted in FIGS. 11 or 12, electrical connections to the heating elements 74 and thermocouples 76, as well as both ends of the TEGs 20, will exit the top of the calorimeter 10. A heat sink 30 may be fitted to the top, with provisions for these connectors to protrude through it.
[0078] FIG. 13 depicts a gas flow manifold 48, which facilitates implementation and investigation of triggering events for an exothermic reaction in the exothermic reaction chamber 68. The manifold attaches to the gas flow tube 44 (Figs. 11, 12) at nut 50. A port 52 allows a pressure meter to be attached, to monitor the pressure (vacuum) in the exothermic reaction chamber 68. A port 54 allows for attachment to a vacuum pump, to evacuate the exothermic reaction chamber 68 to 106-10 7 Torr prior to introducing hydrogen gas.
[0079] In the illustrated embodiment, a particular gas flow valve 56 selectively isolates the port 54 from other elements of the manifold 48 after the desired vacuum is achieved. Additional gas flow valves 56 selectively close to isolate respective supply gas storage chambers 60 from the manifold 48 or open to permit the entry of respective gases from the gas storage chambers 60. The gas flow valves 56 may be electronically actuated, and hence may be controlled by software executing on a processor. In other embodiments, the valves 56 may be manually actuated.
[0080] A mass flow controller 58 permits precise amounts of gas - stored, in one
embodiment, in supply gas storage chambers 60 - to pass into the exothermic reaction chamber 68, once a desired vacuum has been achieved in the chamber 68. In one embodiment, one supply gas storage chamber 60 stores“light” hydrogen gas (H), and the other stores“heavy” hydrogen gas (deuterium). Gas flow valves 56 isolate the supply gas storage chambers 60, and selectively allow gas to flow from one or the other through the mass flow controller 58 into the exothermic reaction chamber 68. [0081] In one embodiment, after an exothermic reaction has been observed by a rise in the temperature of the core 12, as detected by the TEG 20 output, gas in the exothermic reaction chamber 68 may be sampled for analysis, such as by mass spectroscopy. For example, the presence of 4He nuclei may indicate that a nuclear fusion reaction occurred in the exothermic reaction chamber 68.
[0082] Accordingly, the illustrated embodiment of the gas flow manifold 48 of FIG. 13 includes a sample gas storage chamber 62 for collection of gas from the exothermic reaction chamber 68. The sample gas storage chamber 62 may be evacuated to a vacuum, along with the exothermic reaction chamber 68, by opening both of two sample gas valves 64 during the vacuum pump operation. The sample gas valves 64 are then closed as one or more supply gases are introduced and an exothermic reaction is triggered in the exothermic reaction chamber 68. Following an indication of a reaction (i.e., thermal rise), the sample gas valves 64 may both be opened, and the pressure differential will transfer gas from the exothermic reaction chamber 68 into the sample gas storage chamber 62. At this point, both sample gas valves 64 may be closed, and a linking connector 66 therebetween, illustrated as a connection nut that can be loosened, can be used to release the connection between the first sample gas valve 64, on the manifold side of the linking connector 66, and the second sample gas valve 64, on the sample gas storage chamber 62 side of the linking connector 66. Upon release of the linking connector 66, the first sample gas valve 64 remains connected to the manifold 48, and the second sample gas valve 64 remains connected to the sample gas storage chamber 62. This permits the sample gas storage chamber 62 to be removed from the manifold 48 and subsequently be attached to instrumentation such as a mass spectrometer for testing of the collected gas. Thus, the first and second sample gas valves 64, and the linking connector 66 interposed therebetween, serve as a coupling interposed between the sample gas storage chamber 62 and the gas flow manifold 48.
[0083] In another embodiment, an entrance port to an instrument may replace the gas storage chamber 62, and the analysis of sample gas performed in“real time.” Real time gas sample analysis can be used to monitor the progress of an exothermic reaction in the reaction chamber 68. The analysis may be focused on detecting an indication that a reaction is actually taking place. The analysis can also be used as feedback to control the reaction. In the embodiment depicted in FIG. 13, the sample gas valves 64 are manually actuated; in other embodiments, they may be electronically actuated and controlled by software executing on a processor. By programming the processor, gas samples can be extracted at a pre-determined time interval by a pre-determined amount. The gas samples can be used to detect one or more signature gases. For example, the content of a sample can be analyzed to determine how much reactant gas, e.g., deuterium gas, has been consumed or how much resultant gas, e.g., 4He, has been produced. In some embodiments, the amount of helium detected in the gas sample may indicate whether the reaction rate is slowing down or will slow down imminently. The reaction rate can be accelerated or moderated based on the amount of helium detected in the samples to maintain a desired reaction rate. For example, to increase the reaction rate, the mass flow controller 58 can be controlled to allow more gas supply to flow from the gas storage chambers 60 into the reaction chamber 68.
[0084] In some embodiments, instead of analyzing gas samples, other types of real time data analysis can be performed, for instance, energetic particle detection, radio frequency (RF) detection, and optical signal detection. [0085] In some embodiments, the gas samples extracted in real time may be analyzed to detect energetic particles. In some embodiments, energetic particle detection can be carried out by placing detectors around the calorimeter 10.
[0086] In some embodiments, one or more ports may be added to facilitate RF detection. Additionally or alternatively, an optical window may be introduced on the calorimeter 10 to allow optical signals to pass through. Often, optical signals are reliable indicators of how a reaction is progressing.
[0087] In other embodiments, more than two supply gas storage chambers 60 may be provided, and/or more than one sample gas storage chamber 62 may be provided, as desired or required for a given experiment. A suitable supply/sample gas storage chamber is the HydroStik lO-liter canister available from Jameco Electronics of Belmont, California.
[0088] FIG. 14 depicts an exothermic reaction chamber 68, according to one embodiment, which may function as a gas reaction chamber. The reaction chamber 68 includes the sealing nut 40 and gas flow tube 44. In one embodiment, one or more generally toroidal magnets 70 surround the reaction chamber 68. One feature of the reaction chamber 68 is a flange 72 on the end opposite the sealing nut 40 - that is, the end of the reaction chamber 68 that is inserted into the first bore 14 in the core 12. The flange 72 acts to retain the magnets 70 as the reaction chamber 68 is removed from the core 12. The flange also allows the end of the reaction chamber 68 to be attached and sealed by orbital welding, yielding a stronger and more robust chamber 68.
[0089] FIG. 15 depicts a functional block diagram of a complete and functional calorimeter 10, according to embodiments of the present invention. The exothermic reaction chamber 68 comprises a metal container 78 plated with a layer of gold 82 and a layer of palladium 84, and contains an anode 86. A lid 88 seals the exothermic reaction chamber 68, with a gas flow pass- through 90. A Teflon cap or spacer 92 insulates the anode 86 in the small region on which the metal container 78 is not plated with gold 82 and palladium 84, to prevent arcing between the anode 86 and this portion of the metal container 78 under very high voltage. In one embodiment, one or more magnets surround the exothermic reaction chamber 68. The exothermic reaction chamber 68, and the magnets if used, are disposed in a central bore of the core 12. A feature 80 between the container 78 and core 12 represents, in various embodiments, one or more of: one or magnets, and a thermally conductive material.
[0090] A plurality of heating elements 74 are disposed in second bores 16, and operate to heat the core 12 to a predetermined temperature (e.g., 150° - 300° C). A plurality of
thermocouples 76 are disposed in third bores 18, and operative to monitor the temperature of the core 12, allowing for a closed-loop control system to maintain the core 12 at a steady, predetermined temperature.
[0091] When the reaction chamber 68 is evacuated to a vacuum and the desired form of hydrogen gas is introduced in the desired quantity, such as by utilizing the manifold 48 (Fig. 13), an exothermic reaction is triggered. In one embodiment, the trigger may comprise the application of high voltage (e.g., 5 kV) at low current between the anode 86 and metal container 78 (grounded to act as cathode). In another embodiment, the trigger may comprise the high DC voltage with an RF signal superimposed, e.g., at a resonant frequency.
[0092] Because the trigger voltage generates a very low current, very little power is input to the system by triggering the exothermic reaction. For example, in one embodiment the triggering power may be 0.1 W. Accordingly, virtually the entirety of any temperature rise of the core 12 may be attributed to an exothermic reaction in the exothermic reaction chamber 68. Such a thermal rise is detected by monitoring the output voltage of the gas storage chambers 60 TEGs 20, which may be series connected, and which may cover substantially the entirety of the external surface of the core 12. Note that the TEG retention clips 22 and thermal transfer material 24 (Fig. 6) may be used in the calorimeter 10 in FIG. 15. The TEGs 20 are covered by heat sinks 30 to aid in cooling the cold side of the TEGs 20. In some embodiments, cooling is further supplemented by convective airflow and/or a refrigerated ambient environment. By maintaining a large temperature differential between the hot and cold sides of the TEGs 20, any rise in temperature of the core 12 is detected and reflected in the TEG 20 output voltage.
[0093] In this manner, excess heat from an exothermic reaction in the exothermic reaction chamber 68 may be detected, quantified, and carefully measured. The occurrence of an exothermic reaction may thus be definitively proven. By utilizing the features provided by the gas flow manifold 48, numerous variations of experimental parameters may easily be explored, and the reaction product gases analyzed. The calorimeter 10 is scalable, and may be modified to operate at higher temperatures than those specified herein. Any operating temperature, voltage value, vacuum level, or other parameter specifically disclosed herein is exemplary only, and not limiting.
[0094] The present invention may, of course, be carried out in other ways than those specifically set forth herein without departing from essential characteristics of the invention. The present embodiments are to be considered in all respects as illustrative and not restrictive, and all changes coming within the meaning and equivalency range of the appended claims are intended to be embraced therein.

Claims

CLAIMS What is claimed is:
1. A calorimeter operative to measure heat from an exothermic reaction, comprising: a core comprising a thermally conductive material;
a first bore defined in the core and operative to hold a reaction chamber;
one or more second bores defined in the core, each second bore operative to hold a heating element;
one or more third bores defined in the core, each third bore operative to hold a thermal sensor; and
a plurality of thermoelectric generators, each operative to generate an output voltage in response to the temperature of the core, each thermoelectric generator having a hot side and a cold side, the hot side of each thermoelectric generator being in thermal communication with the core.
2. The calorimeter of claim 1, wherein the core comprises a copper block.
3. The calorimeter of any preceding claim, wherein the one or more second bores comprise a plurality of second bores defined in the core evenly spaced radially around the first bore.
4. The calorimeter of any preceding claim, wherein the one or more third bores comprise a plurality of third bores defined in the core are evenly spaced radially around the first bore.
5. The calorimeter of any preceding claim, wherein the thermoelectric generators comprise Seebeck effect thermoelectric generators operative in a hot side temperature range from 120° C to 160° C.
6. The calorimeter any preceding claim, further comprising a thermally conductive material interposed between each thermoelectric generator and the core.
7. The calorimeter any preceding claim, wherein the thermoelectric generators at least partially cover an outer surface of the core.
8. The calorimeter of any preceding claim, wherein each thermoelectric generator is
connected to the core with a retention clip.
9. The calorimeter of any preceding claim, wherein the thermoelectric generators are biased towards the core with a predetermined force.
10. The calorimeter of any preceding claim, wherein the thermoelectric generators are affixed to the core with shoulder bolts and spring washers, such that the spring washers are operative to apply a predetermined force biasing the thermoelectric generators against the core when the shoulder bolts are fully advanced.
11. The calorimeter of any preceding claim, further comprising one or more heat sinks in thermal communication with respective cold sides of the thermoelectric generators.
12. The calorimeter of claim 11, further comprising one or more fans operative to direct convective airflow over the heat sinks.
13. The calorimeter of any preceding claim, further comprising a refrigerated housing
operative to contain the calorimeter in an environment having a predetermined ambient temperature.
14. The calorimeter of any preceding claim, further comprising a gas flow manifold operative to supply one or more gases to a reaction chamber in the first bore, the gas flow manifold comprising:
a mass flow controller operative to control the flow of one or more supply gases into the reaction chamber at a predetermined rate;
one or more supply gas storage chambers in gas flow relationship with the mass flow controller;
one or more supply gas valves, each interposed between a respective supply gas storage chamber and the mass flow controller and operative to selectively isolate the supply gas storage chamber from the mass flow controller; and
a port in gas flow relationship with the reaction chamber and operative to connect to a vacuum pump.
15. The calorimeter of claim 14, wherein the mass flow controller and the one or more supply gas valves are actuated electronically under the control of software executing on a processor.
16. The calorimeter of any one of claims 14 and 15, wherein the gas flow manifold is further operative to sample gas from the reaction chamber, and further comprises a sample gas storage chamber removably connected to the gas flow manifold and in gas flow relationship with the reaction chamber.
17. The calorimeter of claim 16, wherein the gas flow manifold further comprises a coupling interposed between the sample gas storage chamber and the manifold, the coupling comprising:
first and second sample gas valves; and
a linking connector interposed between the first and second sample gas valves; wherein when the first and second sample gas valves are open, gas is operative to flow from the reaction chamber into the sample gas storage chamber; and wherein when the first and second sample gas valves are closed, the second valve and sample gas storage chamber may be removed from the manifold at the linking connector.
18. The calorimeter of claim 17, wherein the first and second sample gas valves are manually actuated.
19. The calorimeter of claim 17 wherein the first and second sample gas valves are actuated electronically under the control of software executing on a processor.
20. The calorimeter of any preceding claim, further comprising:
a cylindrical gas reaction chamber operative to house an exothermic reaction;
one or more toroidal magnets positioned around the gas reaction chamber;
a gas flow connector at one end of the gas reaction chamber to connect to a gas flow manifold in gas flow relationship; and
a flange at another end of the gas reaction chamber operative to retain the magnets around the gas reaction chamber.
21. The calorimeter of any preceding claim, wherein the gas from the reaction chamber is sampled in real time.
22. The calorimeter of any preceding claim, wherein the gas from the reaction chamber is analyzed for one or more signature gases.
23. The calorimeter of any preceding claim, wherein the gas sample from the reaction
chamber is analyzed for energetic particle detection or radio frequency detection.
24. The calorimeter of any preceding claim, further comprising an optical window for detecting an optical signal.
PCT/US2018/066288 2017-12-18 2018-12-18 Calorimeter for low energy nuclear reaction experiments WO2019126206A1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140003460A1 (en) * 2011-03-11 2014-01-02 Alliance For Sustainable Energy, Llc Calorimeters for testing energy storage systems and power electronics methods of making the same and methods of use
US20140177669A1 (en) * 2012-12-24 2014-06-26 Schlumberger Technology Corporation Method for determining adsorption heat and wetting heat of a surface and a measuring cell of a calorimeter
US20170227480A1 (en) * 2016-02-05 2017-08-10 Waters Technologies Corporation Calorimeter With Diffusion-Bonded Block

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140003460A1 (en) * 2011-03-11 2014-01-02 Alliance For Sustainable Energy, Llc Calorimeters for testing energy storage systems and power electronics methods of making the same and methods of use
US20140177669A1 (en) * 2012-12-24 2014-06-26 Schlumberger Technology Corporation Method for determining adsorption heat and wetting heat of a surface and a measuring cell of a calorimeter
US20170227480A1 (en) * 2016-02-05 2017-08-10 Waters Technologies Corporation Calorimeter With Diffusion-Bonded Block

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