CN112358308A - Oxide composite nuclear fuel pellet and preparation method thereof - Google Patents
Oxide composite nuclear fuel pellet and preparation method thereof Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- G21C3/58—Solid reactor fuel Pellets made of fissile material
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- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention provides a preparation method of an oxide composite nuclear fuel pellet, belonging to the technical field of nuclear material preparation. The method comprises the following steps: 1) preparing mixed powder: oxide nuclear fuel powder and filler powder are put into a ball milling tank, and zirconium dioxide grinding balls are added for mixing and ball milling; 2) and (3) pressing and forming: carrying out compression molding on the mixed powder after ball milling, and demoulding to obtain an oxide composite nuclear fuel blank; 3) flash burning: electrifying the oxide composite nuclear fuel blank, applying a constant electric field at two ends of the blank, simultaneously raising the temperature, and carrying out flash combustion when the flash combustion temperature is met; the current is 0-700mA/mm2The constant current of the power supply is 0-300V/cm in field intensity, the flash temperature is 25-1000 ℃, and the flash time is 0-600 s; flash firing is finishedAnd then, cooling and demoulding to obtain the oxide composite nuclear fuel pellet. The invention applies constant direct current electric fields at two ends of the blank by using a flash firing technology, can obviously reduce the sintering temperature of uranium dioxide or thorium dioxide, shortens the sintering time and improves the density of the material.
Description
Technical Field
The invention belongs to the technical field of nuclear material preparation, and particularly relates to an oxide composite nuclear fuel pellet and a preparation method thereof.
Background
Uranium dioxide (UO)2) The fuel is the most widely applied nuclear fuel of commercial nuclear reactors at present, has excellent thermal, chemical and irradiation stability and good compatibility with cladding materials, and is an ideal nuclear fuel. However, the low thermal conductivity of the fuel pellets, which is an important factor limiting the performance of nuclear reactors due to the property of phonon heat transfer, has become an important factor in nuclear accident. Thus, UO is improved2The thermal conductivity of the fuel pellets is an effective means of improving the safety of nuclear power plants. At present by mixing UO2Compounded with heat-conducting filler (such as beryllium oxide, silicon carbide, etc.) with high heat conductivity to improve UO2The main technical approach of material thermal conductivity. The existing uranium dioxide composite core block is generally sintered under the condition of heat preservation for 5-10h at the temperature of more than 1700 ℃, and the energy consumption is high.
Thorium dioxide can be used as fuel of a breeder reactor, and nuclear fuel self-sustaining or near-breeding can be realized in a thermal neutron reactor; in fast reactors, a large amount of value can be added. The thorium-uranium mixed fuel is an important fuel system of a thorium circulating high-temperature gas cooled reactor and can also be applied to a light water value-added reactor or a pressurized heavy water reactor. The manufacturing method of the thorium dioxide or uranium-thorium mixed fuel pellet is basically the same as that of the uranium dioxide pellet, but the sintering temperature is higher, and the heat preservation time is longer.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity oxide composite nuclear fuel pellet and a preparation method thereof, aiming at solving the problems of poor thermal conductivity and low preparation efficiency of the existing oxide composite nuclear fuel pellet, adopting a flash combustion technology to improve sintering efficiency and optimize a material organization structure.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the oxide composite nuclear fuel pellet is characterized by comprising the following steps:
1) preparing mixed powder: oxide nuclear fuel powder and filler powder are put into a ball milling tank, and zirconium dioxide grinding balls are added for mixing and ball milling;
2) and (3) pressing and forming: carrying out compression molding on the mixed powder after ball milling, and demoulding to obtain an oxide composite nuclear fuel blank; wherein the molding pressure is 2-10Mpa, and the pressure maintaining time is 2-5 min; then, carrying out green pressing by adopting isostatic cool pressing at the pressure of 100-300Mpa for 1-20 min;
3) flash burning: electrifying the obtained oxide composite nuclear fuel blank, applying a constant electric field at two ends of the blank, simultaneously raising the temperature, and carrying out flash combustion when the flash combustion temperature is reached; wherein the electrified current density is 0-700mA/mm2The field intensity is 0-300V/cm, the flash temperature is 25-1000 ℃, and the flash time lasts 0-600 s; and after flash burning is finished, cooling and demolding to obtain the oxide composite nuclear fuel pellet.
Further, the oxide powder is thorium dioxide powder with the particle size of 20nm-5 mu m or uranium dioxide powder with the particle size of 20nm-5 mu m.
Further, the filler powder is one or more of metal molybdenum, silicon carbide, diamond, beryllium oxide, graphene, graphite and carbon nanotubes.
Further, the mass ratio of the oxide nuclear fuel powder to the filler powder is 85-97: 15-3.
Further, the mass ratio of the sum of the mass of the oxide powder and the filler powder to the grinding balls is 1: 3-15; the ball milling speed is 50-300r/min, and the ball milling time is 2-24 h.
Further, a grinding medium is added in the ball milling process, and the grinding medium is ethanol.
Further, the flash combustion atmosphere is one of air, hydrogen, a hydrogen-argon mixture, nitrogen and a hydrogen-nitrogen mixture.
An oxide composite nuclear fuel pellet is prepared by the method.
The flash combustion of the oxide composite nuclear fuel blank according to the present invention can be realized by the flash combustion system as shown in fig. 1, but other systems or devices can be used as long as the effect of applying an electric field to both ends of the blank while the sintering temperature is raised can be realized. The flash system shown in fig. 1 includes: the sintering device, the power supply, the data recording unit, the control unit and the junction box; the power supply is preferably a direct current power supply with a digital control function, the data recording unit is preferably a digital multimeter, the control unit is preferably a computer, the computer can control the sintering device and the power supply, the sintering device is preferably a tube furnace or a box-type resistance furnace, a sintering chamber is arranged in the sintering device, and the electrodes and the platinum wires or the platinum sheets are located in the sintering chamber.
The electrode penetrates through the sintering device through a platinum wire to be connected with an external lead, a ceramic insulating sleeve is arranged outside the platinum wire to be insulated with the shell of the sintering device, the lead is connected with a power supply through a junction box, and the data recording unit is connected with the electrode through the junction box; the power supply is connected with the control unit to realize the control of parameters such as voltage, current and the like of the power supply; the data recording unit is connected with the control unit, and records the measured voltage and current signals in the control unit, and the control unit simultaneously controls the sintering device. The sintering device, the power supply, the data recording unit, the control unit and each part and function of the junction box and the connection mode can be realized by adopting conventional products in the prior art and combining with the conventional known technology in the field.
In the sintering chamber, the sample is contacted with an electrode, and the electrode is connected with a platinum wire and led out of the sintering chamber to be connected with a lead. According to the shape of the sample, the connection mode of the electrode and the sample can be four, as shown in fig. 2: (a) the sheet electrodes clamp the sample from the left end and the right end and are suspended in the sintering chamber; (b) the flaky electrode contacts the sample from top to bottom, and high-temperature clamps can be arranged on the top and bottom of the electrode to ensure the contact between the sample and the electrode; (c) stick-shaped electrodes penetrate through small holes at two ends of the dog bone-shaped sample and are suspended in the sintering chamber; (d) electrodes were wound around both ends of the stick sample.
The sintering operation of the flash firing system is as follows: connecting two ends of the blank with electrodes, firstly setting a temperature-raising program of a sintering device, then starting the sintering device to raise the temperature, simultaneously starting a power supply to apply an electric field at two ends of the blank, observing current and voltage changes in real time in the sintering process, and recording the current and voltage changes in real time by a data recording unit.
Compared with the prior art, the invention has the following beneficial effects:
the preparation of the prior sintered uranium dioxide pellet, thorium dioxide chip or thorium-uranium mixed fuel pellet needs pressureless sintering for more than 5-8 hours at the temperature of 1700-1800 ℃ so as to achieve the compactness of more than 95%. The sintering temperature required for the preparation of uranium dioxide pellets, thorium dioxide chips, or thorium-uranium mixed fuel pellets by existing field-assisted sintering techniques such as spark plasma sintering is still above 1600 ℃, and the sintering hold time is also typically 15 to 30 minutes. Excessively high sintering temperatures and long holding times generally cause the uranium dioxide or thorium dioxide particles to grow to micron-sized dimensions, which in turn leads to a reduction in their usability. The invention uses a flash combustion technology and applies a constant direct current electric field, can obviously reduce the sintering temperature of the uranium dioxide or the thorium dioxide, shortens the sintering time of a thorium dioxide chip or a thorium-uranium mixed fuel pellet, can effectively refine the crystal grains of the composite material and regulate and control the phase structure and microstructure, improves the density of the material, and meets the use requirement.
Drawings
FIG. 1 is a schematic diagram of a flash system;
FIG. 2 shows the connection between the sample and the electrode in the sintering chamber
FIG. 3 is a UO prepared in example 12-a microscopic morphology of SiC whisker composite pellets;
FIG. 4 is a UO prepared in example 22-carbon nanotube composite pellet micro-morphology;
FIG. 5 is ThO prepared in example 32-carbon nanotube composite pellet micro-morphology.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
With UO2Nanometer powder (the particle diameter of the powder is about 100nm) and SiC whiskers (the length of the whiskers is about 9 microns, the diameter is about 1 micron) are used as raw materials, the silicon carbide whiskers account for 5 percent by mass, and the total amount of the raw materials is 50 g;
putting the raw material powder into a ball milling tank, adding zirconium dioxide grinding balls and 20mL of ethanol, and ball milling and mixing for 20 hours at the rotating speed of 100 r/min.
After mixing, heating, stirring and drying the slurry at the temperature of 90 ℃; and (3) putting the dried mixed powder into a hard alloy die for compression molding, pressing into a blank with the mass of about 2g under the axial pressure of 4MPa, and then pressing into a blank by adopting isostatic cool pressing at the pressure of 100-300MPa and the pressure maintaining time of 1-20 min.
Placing the blank after cold isostatic pressing into a sintering device of a flash combustion system, introducing nitrogen, connecting electrodes at two ends of the blank, starting a power supply (applying a constant electric field at two ends of the blank) to sinter while raising the temperature of the sintering device, wherein the field intensity is 150V/cm, and the current density is 150mA/mm2When the temperature is increased to 800 ℃, flash burning occurs, and UO with compact structure can be obtained within 60s2-SiC composite pellets. And after flash burning is finished, cooling and demolding to obtain the oxide composite nuclear fuel pellet. The temperature rise parameters of the sintering device are as follows: heating to 800 deg.C at 10 deg.C/min, maintaining for 60s, and cooling at 10 deg.C/min.
Imaging UO with secondary electrons of scanning electron microscope2The microscopic morphology of the-SiC whisker composite pellet is characterized, and the result is shown in FIG. 3: the compactness is over 95 percent.
Example 2
With UO2Nano powder (the particle size of the powder is about 1 mu m) and carbon nano tube powder (the particle size of the powder is about 100nm) are taken as raw materials, the mass fraction of the carbon nano tube is 3 percent, and the total amount of the raw materials is 50 g;
putting the raw material powder into a ball milling tank, adding zirconium dioxide grinding balls and 20mL of ethanol, and ball milling and mixing for 15h at the rotating speed of 100 r/min.
After mixing, heating, stirring and drying the slurry at the temperature of 90 ℃; and (3) putting the dried mixed powder into a hard alloy die for compression molding, pressing into a biscuit with the mass of about 2g under the axial pressure of 4MPa, and pressing into the biscuit under the pressure of 150MPa by adopting cold isostatic pressing for 20 min.
Placing the blank after cold isostatic pressing into a sintering device of a flash combustion system, connecting electrodes at two ends of the blank, starting a power supply (applying a constant electric field at two ends of the blank) while raising the temperature of the sintering device, wherein the field strength is 200V/cm, and the current density is 200mA/mm2When the temperature rises to 650 ℃, flash burning occurs, and UO with compact structure can be obtained within 60s2-SiC composite pellets. And after flash burning is finished, cooling and demolding to obtain the oxide composite nuclear fuel pellet. The temperature rise parameters of the sintering device are as follows: heating to 650 deg.C at 10 deg.C/min, maintaining for 60s, and cooling at 10 deg.C/min.
Imaging UO with secondary electrons of scanning electron microscope2Characterization of the microscopic morphology of the carbon nanotube composite pellets, the results are shown in fig. 4: the compactness is over 95 percent.
Example 3
By ThO2The particle size of the powder is about 200nm and the carbon nano tube powder (the particle size of the powder is about 100nm) are taken as raw materials, the mass fraction of the carbon nano tube is 10 percent, and the total amount of the raw materials is 40 g;
putting the raw material powder into a ball milling tank, adding zirconium dioxide grinding balls and 15mL of ethanol, and ball milling and mixing for 15h at the rotating speed of 150 r/min.
After mixing, heating, stirring and drying the slurry at the temperature of 90 ℃; and carrying out compression molding on the dried mixed powder, pressing into a biscuit with the mass of about 2g under the axial pressure of 4MPa, and then pressing the biscuit into a compact by adopting cold isostatic pressing under the pressure of 200MPa and the pressure maintaining time of 10 min.
Placing the blank after cold isostatic pressing into a sintering device of a flash combustion system, introducing hydrogen, connecting electrodes at two ends of the blank, starting a power supply (applying a constant electric field at two ends of the blank) while raising the temperature of the sintering device, wherein the field strength is 300V/cm, and the current density is 200mA/mm2When the temperature is raised to 700 ℃, the flash burning is carried out, and ThO with compact structure can be obtained within 60s2And (3) a core block. The temperature rise parameters of the sintering device are as follows: heating to 700 deg.C at 10 deg.C/min, maintaining for 60s, and cooling at 10 deg.C/min.
Scanning electron microscope secondary electron imaging for ThO2Characterization of the microscopic morphology of the carbon nanotube composite pellets, the results are shown in fig. 5: the compactness is over 95 percent, and the grain size is about 1 mu m.
The effects of examples 1 to 3 can also be achieved by replacing the filler powder (carbon nanotubes, SiC) in examples 1 to 3 with one or more of molybdenum metal, diamond, beryllium oxide, graphene, graphite, and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. The preparation method of the oxide composite nuclear fuel pellet is characterized by comprising the following steps:
1) preparing mixed powder: oxide nuclear fuel powder and filler powder are put into a ball milling tank, and zirconium dioxide grinding balls are added for mixing and ball milling;
2) and (3) pressing and forming: carrying out compression molding on the mixed powder after ball milling, and demoulding to obtain an oxide composite nuclear fuel blank; wherein the molding pressure is 2-10Mpa, and the pressure maintaining time is 2-5 min; then, carrying out green pressing by adopting isostatic cool pressing at the pressure of 100-300Mpa for 1-20 min;
3) flash burning: electrifying the obtained oxide composite nuclear fuel blank, applying a constant electric field at two ends of the blank, simultaneously raising the temperature, and carrying out flash combustion when the flash combustion temperature is reached; wherein the current density is 0-700
mA/mm2The field intensity is 0-300V/cm, the flash temperature is 25-1000 ℃, and the flash time lasts 0-600 s; and after flash burning is finished, cooling and demolding to obtain the oxide composite nuclear fuel pellet.
2. A method for the production of an oxide composite nuclear fuel pellet as claimed in claim 1, characterized in that the oxide powder is thorium dioxide powder with a particle size of 20nm to 5 μm or uranium dioxide powder with a particle size of 20nm to 5 μm.
3. The method for preparing an oxide composite nuclear fuel pellet as claimed in claim 1, wherein the filler powder is one or more of molybdenum metal, silicon carbide, diamond, beryllium oxide, graphene, graphite and carbon nanotubes.
4. A method for the preparation of oxide composite nuclear fuel pellets according to claim 1, characterized in that the mass ratio of oxide nuclear fuel powder to filler powder is between 85 and 97: 15-3.
5. The method for preparing an oxide composite nuclear fuel pellet as claimed in claim 1, wherein the ball milling rotation speed is 50-300r/min and the ball milling time is 2-24 h.
6. A method for the preparation of oxide composite nuclear fuel pellets according to claim 1, characterized in that a grinding medium is also added during the ball milling process, the grinding medium being ethanol.
7. The method for producing an oxide composite nuclear fuel pellet according to claim 1, wherein the flash atmosphere is one of air, hydrogen-argon mixture, nitrogen, and hydrogen-nitrogen mixture.
8. An oxide composite nuclear fuel pellet, characterized in that it is obtained by the process according to any of the claims from 1 to 7.
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Cited By (4)
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| CN113683422A (en) * | 2021-09-03 | 2021-11-23 | 中国工程物理研究院材料研究所 | Large-grain UO2Ceramic fuel and preparation method and application thereof |
| CN114477966A (en) * | 2021-12-22 | 2022-05-13 | 北京理工大学 | Preparation method of fine-grain oxide ceramic |
| CN114907100A (en) * | 2022-05-19 | 2022-08-16 | 中国科学院长春应用化学研究所 | Instantaneous synthesis process of Ba-matrix sub-conductor electrolyte |
| US11705249B2 (en) | 2021-05-11 | 2023-07-18 | Clean Core Thorium Energy Llc | Thorium-based fuel design for pressurized heavy water reactors |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11705249B2 (en) | 2021-05-11 | 2023-07-18 | Clean Core Thorium Energy Llc | Thorium-based fuel design for pressurized heavy water reactors |
| US11929183B2 (en) | 2021-05-11 | 2024-03-12 | Clean Core Thorium Energy Llc | Thorium-based fuel design for pressurized heavy water reactors |
| CN113683422A (en) * | 2021-09-03 | 2021-11-23 | 中国工程物理研究院材料研究所 | Large-grain UO2Ceramic fuel and preparation method and application thereof |
| CN114477966A (en) * | 2021-12-22 | 2022-05-13 | 北京理工大学 | Preparation method of fine-grain oxide ceramic |
| CN114907100A (en) * | 2022-05-19 | 2022-08-16 | 中国科学院长春应用化学研究所 | Instantaneous synthesis process of Ba-matrix sub-conductor electrolyte |
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