CN105334138A - Molten salt impregnation experiment device for carbon material for molten salt reactor - Google Patents
Molten salt impregnation experiment device for carbon material for molten salt reactor Download PDFInfo
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- CN105334138A CN105334138A CN201510618392.2A CN201510618392A CN105334138A CN 105334138 A CN105334138 A CN 105334138A CN 201510618392 A CN201510618392 A CN 201510618392A CN 105334138 A CN105334138 A CN 105334138A
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- autoclave
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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Abstract
The invention discloses a molten salt impregnation experiment device for a carbon material for a molten salt reactor. The device includes an autoclave, a glove box, a well type atmosphere furnace, a gas path system, a hoisting device, and a sample lifting device; the well type atmosphere furnace is located below the glove box, and a furnace port is embedded in the glove box and is in sealing connection with a glove box bottom plate through a flange; the autoclave and the sample lifting device are located inside the glove box; the autoclave includes a kettle body and a kettle lid which are separable; the sample lifting device utilizes a screw lifting mechanism to separate molten salt and an experimental sample at a high temperature; the upper part of the glove box is provided with a visual box body which is in sealing connection with the glove box, and the hoisting device is arranged in the visual box body; the gas path system is arranged outside the glove box, is connected with the interior of the autoclave through a high temperature resistant pipeline, and is used for adjusting the air pressure inside the autoclave. Compared with the prior art, the molten salt impregnation experiment device can more safely and conveniently complete separation of the molten salt and the sample at the high temperature, can accurately adjust the experimental gas pressure, and obtains more accurate experimental results.
Description
Technical field
The present invention relates to high-temperature molten salt experimental provision, particularly relate to the fused salt infiltration experimental provision of a kind of MSR (moltensaltreactor, MSR) with carbon materials.
Background technology
MSR is the one of fission-type reactor, its Main Coolant is a kind of salt-mixture of molten state, keeps low-steam pressure when it can at high temperature work (can obtain the higher thermal efficiency), thus reduces mechanical stress, improve security, and lower than molten sodium cooling medium activity.Due to MSR have safe, efficient, be easy to miniaturization, to advantages such as environmental impact are less, it is studied as following Advanced Nuclear Energy Technology by countries in the world.
Structured material (mainly comprising alloy class large with the carbon materials two) needs used due to MSR contact with fused salt under high-temperature high-pressure state, due to the impact of fused salt, the change that the mechanics of material, thermal property will produce in various degree, and then may have an impact to the security of the serviceable life of material and reactor.Therefore, in order to ensure the security of MSR, must to MSR use the resistance to fused salt characteristic of structured material to carry out experimental study.
For metal alloy compositions, what usually pay close attention to is its corrosion behavior under high-temperature molten salt environment, and high-temperature molten salt corrosion test is the technical way understanding the salt corrosion of alloy high temperature resistant melt.But current each research unit adopts the experimental provision of designed, designed when doing high-temperature molten salt corrosion experiment, do not have unified industry standard and technical manual.Fig. 1 shows the basic structure of a kind of fused salt corrosion experimental provision conventional at present both at home and abroad.The experiment of this fused salt corrosion is carried out in graphite crucible, and sample is fixedly mounted on the graphite rod in graphite crucible.For ensureing that experiment is carried out in a closed environment, graphite crucible is placed in the metal can of 304 stainless steels.By metal can seal welding before experiment starts, experiment terminates, and when temperature of molten salt is cooled to about 500 DEG C, is inverted whole fused salt corrosion experimental provision, realizes being separated of fused salt and sample before fused salt is solidified.When temperature is down to room temperature, then metal can cutting is opened.Whole experimentation carries out in the glove box having argon shield gas above, in case fused salt absorbs water and causes corrosion data to be forbidden.
For the carbon materials (such as nuclear graphite, carbon-carbon composites etc.) that MSR uses, usual concern be the impregnation of high-temperature molten salt to carbon materials, therefore the actual motion environment of simulating MSR is needed to carry out high-temperature molten salt infiltration experiment to carbon materials, namely in specific experimental temperature, pressure and fused-salt medium, take out after there is the sample immersion fused salt certain hour of porosint, test the experiment of its fused salt infiltration amount.Do not have special fused salt infiltration experimental provision to be disclosed at present, researcher, when carrying out fused salt infiltration experiment, directly uses existing fused salt corrosion experimental provision, such as Fig. 1 shown device usually.But, when utilizing existing fused salt corrosion experimental provision to test to the fused salt infiltration carrying out carbon materials, the following shortcoming of ubiquity: (1) test limited sample; (2) being inverted metal can under high temperature with what realize fused salt and sample is separated dangerous property, and each experiment needs consumption metal can, and experimental cost is too high; (3) different from the fused salt corrosion characteristic of alloy, carbon materials can show different imbibing properties under different pressure, and existing fused salt corrosion experimental provision does not have pneumatic control system, cannot test along with the change of air pressure is on the impact of infiltration experimental result.
In summary, need one fused salt infiltration safely and effectively experimental provision badly, accurately can test the fused salt imbibing properties of MSR carbon materials.
Summary of the invention
Technical matters to be solved by this invention is to overcome prior art deficiency, a kind of fused salt infiltration experimental provision of MSR carbon materials is provided, saferly can complete being separated of fused salt and sample under high temperature easily, and can accurately regulate experiment air pressure, obtain experimental result more accurately.
The fused salt infiltration experimental provision of MSR carbon materials of the present invention comprises: autoclave, glove box, well formula atmosphere furnace, air-channel system, hanging apparatus, sample jacking gear; Described well formula atmosphere furnace is positioned at below glove box, and its fire door is embedded glove box and is tightly connected by flange and glove box base plate; Autoclave and sample jacking gear are positioned at glove box inside; Described autoclave comprises separable kettle and kettle cover; Described sample jacking gear comprises elevating screw, bracing frame, rotating nut, suspension ring, sample chamber, and wherein, the bottom of bracing frame is fixedly connected with autoclave kettle cover, and its top to be coordinated with rotating nut by threaded engagement mode and supports rotating nut; Elevating screw is through autoclave kettle cover, and both junction motive seals, the lower end of elevating screw is connected with the sample chamber for loading laboratory sample, the upper end of elevating screw is coordinated with rotating nut by threaded engagement mode, elevating screw oscilaltion can be driven by rotating rotating nut, thus being separated of fused salt and laboratory sample under realizing high temperature; Suspension ring are fixedly mounted on bracing frame, coordinate with hanging apparatus, for being elevated autoclave; Glove box top is provided with the visual casing sealing with glove box and be connected, and described hanging apparatus is installed in this visual casing; Described air-channel system is arranged at glove box outside, is communicated with autoclave by resistant to elevated temperatures pipeline, for regulating autoclave air pressure.
Further, described fused salt infiltration experimental provision also comprises cooling device, for preventing kettle cover and the at high temperature seal failure of kettle junction of autoclave, this cooling device comprises cooling-water machine and water collar, cooling-water machine is installed on glove box outside, water collar is installed on described well formula atmosphere furnace crossing inwall, and cooling-water machine is connected by stainless steel waterpipe with water collar, forms cooling water circulation loop.
Preferably, the motive seal of the junction of elevating screw and autoclave kettle cover is realized by filling flexible graphite, thus can obtain good motive seal performance.
Preferably, described elevating screw is the hollow structure of sealed bottom, is provided with temperature sensing component in its lower end hollow structure, thus can monitor the actual temperature of sample in sample chamber more accurately.
Preferably, described air-channel system comprises aerating system and pumped vacuum systems, can respectively to autoclave pressurization and vacuumizing, wherein, aerating system comprises the gas cylinder be communicated with autoclave, is filled with inert gas in gas cylinder, and pumped vacuum systems comprises the vacuum pump be communicated with autoclave.
Owing to have employed above-mentioned technical solution, the fused salt infiltration experimental provision of carbon materials of the present invention effectively can be avoided fused salt water suction under normal temperature, heated up and the problem that is oxidized occurs in the whole process such as cooling, experiment air pressure can be regulated easily and flexibly according to actual application environment, and solve experiment terminate rear fused salt and sample safe separating at high temperature, thus provide condition for the fused salt infiltration amount of testing carbon materials more exactly, so that launch the fused salt imbibing properties research of carbon materials more scientificly.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of existing fused salt corrosion experimental provision;
Fig. 2 is the one-piece construction schematic diagram of a fused salt of the present invention infiltration experimental provision preferred embodiment;
Fig. 3 is the structural representation of preferred embodiment mesohigh still;
Fig. 4 is the structural representation of sample jacking gear in preferred embodiment;
Fig. 5 is the structural representation of air-channel system in preferred embodiment;
Fig. 6 is the structural representation of cooling device in preferred embodiment;
Fig. 7 is the structural representation of well formula atmosphere furnace in preferred embodiment;
Fig. 8 is the structural representation of glove box in preferred embodiment;
In figure, each label implication is as follows:
1, autoclave, 2, sample jacking gear, 3, air-channel system, 4, cooling device, 5, well formula atmosphere furnace, 6, glove box, 7, hanging apparatus, 101, kettle, 102, kettle cover, 103, heat resisting pipe, 201, carbon materials sample, 202, sample chamber, 203, elevating screw, 204, bracing frame, 205, rotating nut, 206, suspension ring, 207, thermopair, 301, vacuum pump, 302, tensimeter, 303-1 ~ 303-4, gas-tpe fitting, 304, reduction valve, 305, gas circuit panel, 306, gas cylinder, 307, connecting pipe, 401, water collar, 402, cooling-water machine, 403, stainless steel water inlet pipe, 501, body of heater, 502, burner hearth, 503, flange, 504, the stainless steel Inlet and outlet water mouth of pipe, 505, heater wire exports, 506, thermopair, 601, main box, 602, control panel, 603, transfer chamber, 604, cleaning system, 605, visual casing.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described in detail:
Fig. 2 shows the one-piece construction of a fused salt of the present invention infiltration experimental provision preferred embodiment.As shown in Figure 1, this device comprises autoclave 1, sample jacking gear 2, air-channel system 3, cooling device 4, well formula atmosphere furnace 5, glove box 6 and hanging apparatus 7.As shown in the figure, well formula atmosphere furnace 5 is positioned at below glove box 6, and its fire door is embedded glove box 6 and is tightly connected by flange and glove box 6 base plate; It is inner that autoclave 1 and sample jacking gear 2 are positioned at glove box 6; Hanging apparatus 7 is fixedly installed in a visual casing on glove box 6, and this visual casing and glove box 6 are tightly connected; It is outside that air-channel system 3 is arranged at glove box 6, is communicated with, for regulating the air pressure inside of autoclave 1 by resistant to elevated temperatures pipeline with autoclave.
Fig. 3 shows the basic structure of the present embodiment mesohigh still 1, and as shown in the figure, it comprises separable kettle 101 and kettle cover 102.Wherein, kettle 102 flange is designed with the groove of placing graphite O-ring seal, kettle cover 102 is roman flat plate cover, fixedly mounts sample jacking gear 2 above it.Kettle cover 102 is designed with the heat resisting pipe 103 for ventilating, heat resisting pipe 103 one end passes in still, and the other end is connected with air-channel system 3.Kettle 101, kettle cover 102 are connected by the uniform kingbolt of circumference, fastening nuts.Kettle cover 102 and sample jacking gear 2 coupling part adopt metal covering tongue and groove method for designing and bolt, fastening nuts mode to seal.
Fig. 4 shows the basic structure of sample jacking gear 2 in the present embodiment, and as shown in the figure, sample jacking gear 2 comprises elevating screw 203, bracing frame 204, rotating nut 205 and suspension ring 206; Wherein, one end of elevating screw 203 is connected with sample chamber 202, loads carbon materials sample 201 to be tested in sample chamber 202.The other end of elevating screw 203 is coordinated with rotating nut 205 by threaded engagement mode, drives elevating screw 203 oscilaltion by rotating rotating nut 205, thus being separated of fused salt and sample under realizing high temperature.Elevating screw 203 hollow in the present embodiment, sealed bottom, for placing thermopair 207, thus can carry out measuring accurately in real time to the temperature of sample chamber 202.Elevating screw 203 is through autoclave kettle cover 102 center simultaneously, fills the soft graphite being used for motive seal in both junctions.Bracing frame 204 is for supporting sample jacking gear 2, and bottom is connected with kettle cover 102, and top to be coordinated with rotating nut 205 by threaded engagement mode and supports rotating nut 205.Suspension ring 206 are fixedly mounted on bracing frame 204 both sides, coordinate with hanging apparatus 6, for being elevated autoclave 1.
Fig. 5 shows the air-channel system 3 in preferred embodiment, and as shown in the figure, it comprises vacuum pump 301, tensimeter 302, gas-tpe fitting 303-1 ~ 303-4, reduction valve 304 and connecting pipe 307.Wherein tensimeter 302, gas-tpe fitting 303 and reduction valve 304 are fixedly installed on gas circuit panel 305, install and operation to facilitate.Air-channel system 3 is divided into aerating system and pumped vacuum systems, can pressurize to autoclave 1 respectively and vacuumize.Wherein aerating system inert gas enters autoclave 1 by gas-tpe fitting 303-2, reduction valve 304, gas-tpe fitting 303-3, tensimeter 302 and connecting pipe 307 successively from gas cylinder 306; Pumped vacuum systems is vacuumized by vacuum pump 301, gas-tpe fitting 303-1, tensimeter 302 and connecting pipe 307 pairs of autoclaves 1 successively, and gas-tpe fitting 303-4 is used for autoclave 1 and exits.
Fig. 6 shows the basic structure of cooling device 4 in preferred embodiment, and it is for preventing kettle cover 102 and the at high temperature seal failure of kettle 101 junction of autoclave 1.Comprise water collar 401 and cooling-water machine 402, cooling device 4 also has the stainless steel water inlet pipe 403 connecting water collar 401 and cooling-water machine 402, makes water collar 401 and cooling-water machine 402 form a recirculated water path.
Fig. 7 shows the basic structure of the well formula atmosphere furnace 5 used in preferred embodiment, it comprises body of heater 501, burner hearth 502 and flange 503, and well formula atmosphere furnace 5 also has the stainless steel Inlet and outlet water mouth of pipe 504 for connecting water collar 401 and cooling-water machine 402, heater wire outlet 505 and thermopair 506.Well formula atmosphere furnace 5 is periodic operating, adopts housing integration sealing, the sealing of bottom cover plate employing high temperature silicon rubber cushion.Flange 503 and glove box 6 are tightly connected, and make autoclave 1 be placed in inert atmosphere in glove box 6.Heater wire is drawn by side heat line outlet 505, and thermopair 506 is arranged on bottom well formula atmosphere furnace 5, leads to outside stove, and heater wire and thermopair 506 use teflon seal respectively, prevents furnace atmosphere and stove to be interlinked to the outside.
Fig. 8 shows the basic structure of institute's use glove box 6 in preferred embodiment, and it comprises main box 601, control panel 602, transfer chamber 603 and cleaning system 604.Control panel 602 can control pressure and water oxygen content in main box 601, and fused salt infiltration experiment is carried out in an inert atmosphere.Cleaning system 604 for purifying the atmosphere in main box 601, to ensure that water Control for Oxygen Content is at below 1ppm.In addition, the upper end of main box 601 is provided with the visual casing 605 for installing hanging apparatus 7, and this visual casing 605 seals with main box 601 and is connected.
Below by an experiment embodiment, concrete use procedure of the present invention is described:
For avoiding fused salt corrosion metal, cause experimental data inaccurate and facilitate fused salt to extract, fused salt infiltration experiment is placed in graphite crucible to be carried out.First sample jacking gear 2 is risen to highest point before experiment, a certain amount of fused salt is put into graphite crucible, then graphite crucible is placed in autoclave 1.By ready carbon materials sample 201(as graphite material, pyrocarbon coating material, carbon-carbon composites, composite material of silicon carbide etc.) put into sample chamber 202, by screwed tight mode, sample chamber is fixedly connected with sample jacking gear.After carbon materials sample 201 installs, tighten autoclave 1, start experiment.Experimental procedure is roughly as follows:
1. vacuumize
Air-channel system 3 is communicated with autoclave 1, closes gas-tpe fitting 303-3, open gas-tpe fitting 303-1 and open vacuum pump 301, autoclave 1 is vacuumized (experimentally demand can carry out pumpback several times).
2. heat
From temp controlled meter or temperature control panel input temp parameter.For being more conducive to temperature-controlled precision, the thermopair 506 in well formula atmosphere furnace 5 is set to temperature controlling mode, and in autoclave 1, thermopair 207 is displays temperature pattern.Experimentally temperature adjustment electric thermo-couple temperature.
3. drive cooling system
Open cold radiator cooler 4 while heating, cools autoclave 1, causes autoclave 1 to leak to prevent flange 102 place O-ring seal to lose efficacy.Cooling water temperature is set according to demand, to ensure cooling effect.
4. preacceleration inflation
After being heated to experiment design temperature, sample immerses before fused salt, and experimentally demand is to autoclave 1 preacceleration inflation or vacuumize.Be pressurised into manual adjustments, first close gas-tpe fitting 303-1, open gas-tpe fitting 303-2 and 303-3, open reduction valve 304 and be adjusted to required pressure, then ventilate.After being adjusted to set pressure, closing gas-tpe fitting 303-2, unscrew reduction valve 304.If vacuumize, with reference to above-mentioned steps 1.
5. pressurize
Be warming up to experiment temperature required after, fall sample jacking gear 2, carbon materials sample 201 be immersed in fused salt completely.Twist rotating nut 205 with spanner, drive sample jacking gear 2 to decline, until in the complete submergence fused salt of sample.Experimentally demand pressurization, pressurization steps is with reference to above-mentioned steps 4.After pressurization, close gas-tpe fitting 303-3, make equipment set be in air-tight state.Experiment starts and is incubated.
6. sample
After experiment terminates, carbon materials sample 201 is separated with fused salt.Twist rotating nut 205 with spanner, drive sample jacking gear 2 to rise, until sample is separated completely with fused salt, then lower the temperature.Because temperature decline autoclave 1 still internal gas pressure also declines thereupon, for avoiding pressure drop in temperature-fall period to have an impact to experimental result, need to autoclave 1 pressurize.Concrete steps, for closing gas-tpe fitting 303-1, are opened gas-tpe fitting 303-2 and 303-2, and reduction valve 304 are adjusted to required pressure, then keep aeration status.After being down to room temperature, experiment terminates.
Utilize the present invention to carry out the fused salt infiltration experiment of MSR carbon materials, there is safe and reliable, that experimental precision is high, experimental cost is low advantage, there is good application prospect.In addition, the present invention also can be used for the fused salt corrosion experiment of MSR alloy material.
Claims (7)
1. the fused salt infiltration experimental provision of MSR carbon materials, is characterized in that, comprising: autoclave, glove box, well formula atmosphere furnace, air-channel system, hanging apparatus, sample jacking gear; Described well formula atmosphere furnace is positioned at below glove box, and its fire door is embedded glove box and is tightly connected by flange and glove box base plate; Autoclave and sample jacking gear are positioned at glove box inside; Described autoclave comprises separable kettle and kettle cover; Described sample jacking gear comprises elevating screw, bracing frame, rotating nut, suspension ring, sample chamber, and wherein, the bottom of bracing frame is fixedly connected with autoclave kettle cover, and its top to be coordinated with rotating nut by threaded engagement mode and supports rotating nut; Elevating screw is through autoclave kettle cover, and both junction motive seals, the lower end of elevating screw is connected with the sample chamber for loading laboratory sample, the upper end of elevating screw is coordinated with rotating nut by threaded engagement mode, elevating screw oscilaltion can be driven by rotating rotating nut, thus being separated of fused salt and laboratory sample under realizing high temperature; Suspension ring are fixedly mounted on bracing frame, coordinate with hanging apparatus, for being elevated autoclave; Glove box top is provided with the visual casing sealing with glove box and be connected, and described hanging apparatus is installed in this visual casing; Described air-channel system is arranged at glove box outside, is communicated with autoclave by resistant to elevated temperatures pipeline, for regulating autoclave air pressure.
2. as claimed in claim 1 fused salt infiltration experimental provision, it is characterized in that, also comprise cooling device, for preventing kettle cover and the at high temperature seal failure of kettle junction of autoclave, this cooling device comprises cooling-water machine and water collar, and cooling-water machine is installed on glove box outside, and water collar is installed on described well formula atmosphere furnace fire door inwall, cooling-water machine is connected by stainless steel waterpipe with water collar, forms cooling water circulation loop.
3. as claimed in claim 1 fused salt infiltration experimental provision, it is characterized in that, the motive seal of the junction of elevating screw and autoclave kettle cover is realized by filling flexible graphite.
4. as claimed in claim 1 fused salt infiltration experimental provision, it is characterized in that, described elevating screw is the hollow structure of sealed bottom, is provided with temperature sensing component in its lower end hollow structure.
5. as claimed in claim 4 fused salt infiltration experimental provision, it is characterized in that, described temperature sensing component is thermopair.
6. as claimed in claim 1 fused salt infiltration experimental provision, it is characterized in that, described air-channel system comprises aerating system and pumped vacuum systems, can respectively to autoclave pressurization and vacuumizing, wherein, aerating system comprises the gas cylinder be communicated with autoclave, is filled with inert gas in gas cylinder, and pumped vacuum systems comprises the vacuum pump be communicated with autoclave.
7. as claimed in claim 1 fused salt infiltration experimental provision, it is characterized in that, also comprising the graphite crucible for holding fused salt.
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CN106769450A (en) * | 2016-11-29 | 2017-05-31 | 中国科学院上海应用物理研究所 | Fused salt environmental mechanicses performance testing device, system and method |
CN108231224A (en) * | 2018-01-17 | 2018-06-29 | 中国科学院上海应用物理研究所 | A kind of analogy method of nuclear material in molten salt reactor |
CN108492894A (en) * | 2018-03-06 | 2018-09-04 | 哈尔滨工程大学 | A kind of safe cooling device of fused salt |
CN110333180A (en) * | 2019-07-02 | 2019-10-15 | 中国科学院上海硅酸盐研究所 | High-temperature molten salt environment simulator and method |
CN111879911A (en) * | 2020-06-15 | 2020-11-03 | 中国原子能科学研究院 | Experimental device for static compatibility of liquid metal |
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CN106769450A (en) * | 2016-11-29 | 2017-05-31 | 中国科学院上海应用物理研究所 | Fused salt environmental mechanicses performance testing device, system and method |
CN106769450B (en) * | 2016-11-29 | 2019-05-03 | 中国科学院上海应用物理研究所 | Fused salt environmental mechanics performance testing device, system and method |
CN108231224A (en) * | 2018-01-17 | 2018-06-29 | 中国科学院上海应用物理研究所 | A kind of analogy method of nuclear material in molten salt reactor |
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CN108492894A (en) * | 2018-03-06 | 2018-09-04 | 哈尔滨工程大学 | A kind of safe cooling device of fused salt |
CN110333180A (en) * | 2019-07-02 | 2019-10-15 | 中国科学院上海硅酸盐研究所 | High-temperature molten salt environment simulator and method |
CN111879911A (en) * | 2020-06-15 | 2020-11-03 | 中国原子能科学研究院 | Experimental device for static compatibility of liquid metal |
CN112814652A (en) * | 2021-01-13 | 2021-05-18 | 江苏联友科研仪器有限公司 | Visual model cauldron for ultralow gas permeability |
CN112700895A (en) * | 2021-01-25 | 2021-04-23 | 中国科学院上海应用物理研究所 | High-temperature molten salt stirring test device |
CN112700895B (en) * | 2021-01-25 | 2022-08-12 | 中国科学院上海应用物理研究所 | High-temperature molten salt stirring test device |
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US12012827B1 (en) | 2023-09-11 | 2024-06-18 | Natura Resources LLC | Nuclear reactor integrated oil and gas production systems and methods of operation |
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