CN113061781B - Nickel-based composite material and molten salt reactor core structural member - Google Patents

Nickel-based composite material and molten salt reactor core structural member Download PDF

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CN113061781B
CN113061781B CN202110280872.8A CN202110280872A CN113061781B CN 113061781 B CN113061781 B CN 113061781B CN 202110280872 A CN202110280872 A CN 202110280872A CN 113061781 B CN113061781 B CN 113061781B
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yttrium oxide
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CN113061781A (en
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黄鹤飞
李�诚
雷冠虹
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Shanghai Institute of Applied Physics of CAS
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    • C—CHEMISTRY; METALLURGY
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    • B22—CASTING; POWDER METALLURGY
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
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    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
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    • G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
    • G21C3/42—Selection of substances for use as reactor fuel
    • G21C3/44—Fluid or fluent reactor fuel
    • G21C3/54—Fused salt, oxide or hydroxide compositions
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    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C5/00—Moderator or core structure; Selection of materials for use as moderator
    • G21C5/12—Moderator or core structure; Selection of materials for use as moderator characterised by composition, e.g. the moderator containing additional substances which ensure improved heat resistance of the moderator
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
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    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract

The invention discloses a nickel-based composite material, and belongs to the technical field of metal-based reinforced materials. The nickel-based composite material disclosed by the invention takes 17 wt.% of molybdenum and 79.5-82 wt.% of nickel as metal matrixes and takes 0.5-3 wt.% of nano yttrium oxide particles as reinforcements. According to the invention, by adding a proper amount of nano yttrium oxide particles into the nickel-molybdenum binary alloy, comprehensive strengthening effects such as dispersion strengthening containing the nano yttrium oxide particles and solid solution strengthening of molybdenum atoms can be formed, so that the mechanical strength of the matrix is greatly improved, and the obtained nickel-based composite material has excellent high-temperature strength property and fluoride salt corrosion resistance, especially excellent high-temperature irradiation resistance, and provides a new direction for the research of commercial molten salt reactor core structural member materials.

Description

Nickel-based composite material and molten salt reactor core structural member
Technical Field
The invention relates to the technical field of metal-based reinforced materials, in particular to a nickel-based composite material.
Background
The molten salt reactor is one of the most advanced fission reactors, can effectively realize thorium-uranium fuel circulation, thereby realizing the utilization of thorium energy to solve the problem that China faces the continuous increase of energy demand and CO2Double pressure for emission reduction. The service environment of high temperature, strong neutron irradiation and strong corrosivity in the molten salt reactor provides challenges for the alloy structural materials in the reactor. The U.S. department of energy deployed irp (integrated Research project) Research project initiated a fluoride salt cooled high temperature reactor (FHR) study, whose report statesIt is noted that the choice of structural materials in a molten salt pile is mainly based on the following points: high temperature strength, thermal conductivity, neutron irradiation resistance, corrosion resistance and nuclear engineering. Based on this, the common reactor alloy structural materials, such as various iron-based alloys used in light water reactor and high temperature gas cooled reactor, can not meet the requirement of molten salt reactor because iron is not resistant to fluoride molten salt corrosion. The united states spent a lot of manpower and money to develop structural materials for molten salt piles from the beginning of the 50's last century and finally developed INOR-8 alloy, which is commercially known as Hastelloy N alloy, by Oak Ridge National Laboratory (ORNL). This alloy was successfully used in the MSRE pilot stack of ORNL in the mid 1960 s. FHR nickel-based Hastelloy N alloys with excellent fluoride molten salt corrosion resistance are used as the primary candidate structural material for molten salt stacks. However, researchers in the mountain national laboratories of Ren et al indicate that Hastelloy N alloy can only operate below 704 ℃ at most, otherwise the thermal stability and high-temperature mechanical strength of the alloy are greatly reduced, which is far from meeting the requirement of commercial operation of a molten salt reactor at about 850 ℃.
Further, nickel has a large neutron absorption cross section, and thus is likely to react with neutrons to generate helium, which in turn forms helium bubbles in the nickel-based alloy. The following damage was caused to the alloy: the great accumulation of helium bubbles at the grain boundary can reduce the bonding force between alloy grain boundaries, and cause direct embrittlement of the material; helium bubbles formed inside alloy crystal grains can pin the dislocation lines to move freely, so that the alloy is hardened and embrittled; helium bubble formation can also cause swelling of the material, which in turn affects the service properties of the alloy. The helium embrittlement problem of nickel-base alloys is also specified in the report of ORNL and there is a clear objection in the paper to the use of nickel-base alloys at the core. Per Peterson states that for liquid fuel thorium-based molten salt reactors, the problem of helium embrittlement of reactor vessels made of Hastelloy N alloy will directly affect the service life of the reactor. In terms of core components, the deficiencies of the Hastelloy N alloy in high temperature strength and resistance to intense neutron irradiation have become a limitation for the development of molten salt reactors from experimental reactors to commercial reactors. In recent years, researchers indicate that carbon-based composite materials are used for replacing Hastelloy N alloys, and the good high-temperature strength and neutron irradiation resistance of the carbon-based composite materials can meet the requirements of commercial molten salt reactors. However, the connectivity and processability of carbon-based composite materials are in question, and the related technologies need to be solved. Based on the above situation, it is very necessary to search a new alloy structural material which can satisfy the structural requirements of the molten salt reactor core to promote the development of the molten salt reactor structural material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a nickel-based composite material which has excellent thermal stability, high-temperature mechanical strength, fluoride salt corrosion resistance and helium brittleness resistance, and can meet the performance indexes required by a molten salt reactor core structural member.
The invention specifically adopts the following technical scheme to solve the technical problems:
the nickel-based composite material takes 17 wt.% of molybdenum and 79.5-82 wt.% of nickel as metal matrixes and 0.5-3 wt.% of nano yttrium oxide particles as reinforcements.
Preferably, the size of the nano yttrium oxide particles is 2-20 nanometers.
Preferably, the nickel-based composite material is prepared by a powder metallurgy method.
Further preferably, the powder metallurgy method is as follows:
step 1, mixing the pure nickel powder, the pure molybdenum powder, the nano yttrium oxide particles and the stearic acid according to the weight ratio of 79.5-82 wt.% -17 wt.% -0.5-3 wt.%: 1wt.% of the components are mixed evenly;
step 2, performing ball milling on the mixture obtained in the step 1, and pressing the mixture into a prefabricated body;
and 3, carrying out vacuum or inert atmosphere protection sintering on the prefabricated body, wherein the sintering temperature range is 1100-1175 ℃, the heat preservation time is 10-15 minutes, and the temperature rise and temperature reduction speed ranges are 80-100 ℃/minute and 35-40 ℃/minute respectively.
And 4, annealing heat treatment is carried out on the sintered preform.
Preferably, the ball milling is carried out by using a planetary ball mill, and the ball milling time is 2-24 hours. As a preferred scheme, ball milling is carried out in a stainless steel tank containing 1:1 mixed stainless steel balls with diameters of 6mm and 10mm respectively, and the ball-to-material ratio is 5-10: 1.
Preferably, the treatment process of the annealing heat treatment specifically comprises the following steps: and (3) preserving the heat for 10-50 minutes at the temperature of 1100 ℃, and then cooling in air.
Preferably, the average particle size of the pure nickel powder and the pure molybdenum powder is 2-10 microns.
Preferably, the ball-milled mixture is pressed into a preform with a pressure of 20 MPa.
Preferably, the nickel-based composite material is applied in a high temperature molten salt environment.
The following technical solutions can also be obtained according to the same inventive concept:
the molten salt reactor core structure is made of the nickel-based composite material in any one technical scheme.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the nano yttrium oxide particle reinforcement is added into the nickel-molybdenum binary alloy, so that comprehensive strengthening effects such as dispersion strengthening containing nano yttrium oxide particles, solid solution strengthening of molybdenum atoms and the like are formed; therefore, the mechanical strength of the pure nickel is greatly improved, the better plasticity is maintained, and the mechanical strength and the molten salt corrosion resistance of the alloy are greatly superior to those of the existing Hastelloy N and other high-temperature alloys; more importantly, the interfaces of the nano yttrium oxide particles and the matrix are stable He capture sites, and helium generated by irradiation in the material can be captured around the particles, so that embrittlement caused by helium diffusion to grain boundaries is prevented, swelling caused by helium bubble growth is avoided, and the high-temperature irradiation resistance of the material is effectively improved.
Drawings
FIG. 1 shows the microstructure of a nano-yttrium oxide particle-reinforced nickel-based composite material, wherein (a) shows the microstructure of a composite material prepared with a ball milling time of 2 hours; (b) the microstructure of the composite material is prepared with ball milling time of 4 hours; (c) the microstructure of the composite material is prepared with ball milling time of 8 hours;
FIG. 2 shows a nano yttrium oxide particle reinforced nickel-based composite materialCompared with the helium embrittlement resistance of Hastelloy N alloy, wherein SRIs Hastelloy N at 700 deg.C 5 x 106ions/cm2Volume percent of helium bubbles under irradiation dose, S1-1Preparation of composite materials for ball milling time of 2 hours at 700 ℃ 5 x 106ions/cm2Volume percent of helium bubbles under irradiation dose, S2-1Preparation of composite with a ball milling time of 4 hours at 700 ℃ 5 x 106ions/cm2Volume percent of helium bubbles under irradiation dose, S3-1For the preparation of a composite material with a ball milling time of 8 hours at 700 ℃ 5 x 106ions/cm2Volume percent helium bubble under irradiation dose;
FIG. 3 shows the yield strength and tensile strength of the composite material ball milled for 4 hours at different yttria levels;
FIG. 4 is a comparison of the cross-sectional shapes of the nano-yttria particle reinforced nickel-based composite material and Hastelloy N alloy corroded in FLiNaK salt at 650 ℃ for 100 hours.
Detailed Description
Although nickel-based alloys have been explored for use in molten salt reactors as early as the sixties of the last century, nickel has a large neutron absorption cross section and is likely to react with neutrons to produce helium, which forms helium bubbles inside the nickel-based alloys. The great accumulation of helium bubbles at the grain boundary can reduce the bonding force between alloy grain boundaries, and cause direct embrittlement of the material; helium bubbles formed inside alloy crystal grains can pin the dislocation lines to move freely, so that the alloy is hardened and embrittled; helium bubble formation can also cause swelling of the material, which in turn affects the service properties of the alloy. The helium embrittlement problem of nickel-base alloys is also specified in the report of ORNL and there is a clear objection in the paper to the use of nickel-base alloys at the core. Per Peterson states that for liquid fuel thorium-based molten salt reactors, the problem of helium embrittlement of reactor vessels made of Hastelloy N alloy will directly affect the service life of the reactor. How to solve the problem of helium brittleness is the key of the application of the nickel-based alloy in the future commercial molten salt pile structural materials.
Through a large amount of experimental researches, the inventor finds that a nickel-based composite material which takes 0.5-3 wt.% of nano yttrium oxide particles as a reinforcement and 17 wt.% of molybdenum and 79.5-82 wt.% of nickel as a metal matrix can form comprehensive strengthening effects such as dispersion strengthening containing the nano yttrium oxide particles, solid solution strengthening of molybdenum atoms and the like, so that the mechanical strength of the matrix is greatly improved, and the obtained nickel-based composite material has excellent thermal stability, high-temperature mechanical strength, fluoride salt corrosion resistance and helium brittleness resistance and can sufficiently meet the requirements of the reactor core environment of a molten salt reactor on structural materials.
The nano yttrium oxide particle reinforced nickel-based composite material provided by the invention can be prepared by adopting the existing or future process methods, such as the existing solid dispersion method, the existing spray deposition method, the existing liquid infiltration method, the existing in-situ composite method and the like. The invention takes the dispersion effect, the process maturity, the production cost and other factors of the reinforcing base in the composite material into comprehensive consideration, and the composite material is preferably prepared by adopting a powder metallurgy method, so that on one hand, a bulk composite material with excellent performance can be obtained, and on the other hand, the preparation cost is lower and the material performance is more stable.
Among them, the preferable powder metallurgy method is specifically as follows:
step 1, mixing the pure nickel powder, the pure molybdenum powder, the nano yttrium oxide particles and the stearic acid according to the weight ratio of 79.5-82 wt.% -17 wt.% -0.5-3 wt.%: 1wt.% of the components are mixed evenly;
step 2, performing ball milling on the mixture obtained in the step 1, and pressing the mixture into a prefabricated body;
and 3, carrying out vacuum or inert atmosphere protection sintering on the prefabricated body, wherein the sintering temperature range is 1100-1175 ℃, the heat preservation time is 10-15 minutes, and the temperature rise and temperature reduction speed ranges are 80-100 ℃/minute and 35-40 ℃/minute respectively.
And 4, annealing heat treatment is carried out on the sintered preform.
In the powder metallurgy process, the particle size of the pure nickel powder and the pure molybdenum powder is preferably 2-10 microns, the purity is more than 99.6 wt.%, the particle size of the nano yttrium oxide powder is preferably 2-20 nanometers, and the purity is more than 99.9 wt.%.
Ball milling, which is a key process of the powder metallurgy process, has a large impact on the performance of the final product (fig. 1 shows the microstructure of the composite material prepared at different ball milling times), so the ball milling process parameters should be optimized. The invention preferably uses a planetary ball mill to perform ball milling in a stainless steel tank containing 1:1 mixed stainless steel balls with diameters of 6mm and 10mm respectively, wherein the ball-material ratio is-10: 1, and the ball milling time is 2-24 hours. And (3) filling the material powder which is subjected to ball milling and sieving into a die cavity, and performing compression molding to obtain a preform, wherein the compression molding pressure is preferably 20 MPa.
The sintering process is also the core process of powder metallurgy, and the process parameters directly determine the properties of the finished product. The preferred sintering process of the present invention is specifically as follows: at a vacuum degree of 10-3～10-5And (3) carrying out spark plasma sintering under the bar, gradually raising the temperature and the pressure to 1100-1175 ℃ and 40-60 MPa at the temperature raising speed of 100 ℃/min and the pressure raising speed of 1.6MPa/min, carrying out heat preservation and pressure maintaining for 10 minutes, immediately relieving the pressure, and circularly cooling to the room temperature through cooling water within 30 minutes.
The preferred annealing heat treatment process of the invention is as follows: and (3) preserving the heat for 10-50 minutes at the temperature of 1100 ℃, and then cooling in air.
In order to obtain the optimal process parameters, the invention also carries out a large number of experiments to find out the influence of the content of yttrium oxide and the ball milling time on the performance of the composite material. The results of the experiment are shown in fig. 3 and table 1.
TABLE 1 yield strength, tensile strength and elongation of the composite material at different ball milling times
Yield strength (MPa) Tensile strength (MPa) Elongation (%)
2 hours ball milling 710 959 19.7
Ball milling for 4 hours 1023 1193 10.4
Ball milling for 6 hours 1066 1181 6.7
The public can select appropriate process parameters according to the above experimental data to obtain the composite material of the present invention with corresponding properties.
In order to verify the high-temperature irradiation characteristic, particularly the helium brittleness resistance of the composite material, a composite material sample prepared by the process is taken to perform a high-temperature irradiation experiment: performing helium ion implantation high-temperature irradiation on the composite material and the Hastelloy N sample at 700 ℃ by using a series accelerator, wherein the irradiation dose is 5E16 ion/cm2. Fig. 2 gives statistics on helium bubble information at the maximum depth of injection for composite and Hastelloy N samples. Where the volume fraction of helium bubbles was counted, it was found that the volume fraction of helium bubbles in the composite was smaller than in the Hastelloy N sample. The effect of the helium bubbles on the composite material is much less even in the areas where the helium bubbles appear the most. In addition, as shown in fig. 4, in the aspect of molten salt corrosion performance, when the composite material and the Hastelloy N sample are subjected to molten salt corrosion under the same condition (corrosion in FLiNaK salt at 650 ℃ for 100 hours), the composite material of the invention has no obvious cracks and holes, maintains structural integrity, and has better molten salt corrosion resistance than Hastelloy N alloy. In conclusion, the composite material of the invention has the helium brittleness resistance and the corrosion resistance far exceeding those of the common nickel-based alloyCan and still perform well under the strong irradiation environment, which is enough to meet the requirements of stronger irradiation and corrosive operation environment of the commercial molten salt reactor in the future.
According to the invention, a proper amount of nano yttrium oxide particles are utilized to reinforce the nickel-molybdenum binary alloy, and a corresponding preparation process is assisted, so that the obtained nickel-based composite material has excellent high-temperature strength property and fluoride salt corrosion resistance, especially excellent high-temperature irradiation property, the technical bias that the nickel-based alloy cannot be used for the reactor core of the molten salt reactor is broken, and a new direction is pointed out for the research of structural member materials of the reactor core of the molten salt reactor. The nano yttrium oxide particle reinforced nickel-based composite material can be widely applied to high-temperature molten salt environments such as molten salt reactors, particularly can meet the application requirements of extremely strict performance requirements such as molten salt reactor core structural members, has higher reliability and longer service life, and can also be applied to other similar high-temperature irradiation environments.

Claims (11)

1. A nickel-based composite material is used for a molten salt reactor core structure and is characterized in that molybdenum and nickel are used as metal matrixes, nano yttrium oxide particles are used as reinforcements, and the proportion of the molybdenum, the nickel and the nano yttrium oxide particles is 17 wt.%: 79.5-82 wt.%: 0.5-3 wt.%.
2. The nickel-based composite material of claim 1, wherein the nano yttrium oxide particles have a size of 2 to 20 nm.
3. The nickel-based composite of claim 1, wherein the nickel-based composite is prepared by a powder metallurgy process.
4. The nickel-based composite material according to claim 3, wherein the powder metallurgy method is as follows:
step 1, mixing pure nickel powder, pure molybdenum powder, nano yttrium oxide particles and stearic acid according to the weight ratio of 79.5-82 wt% to 17 wt% to 0.5-3 wt%: 1wt.% of the components are mixed evenly;
step 2, performing ball milling on the mixture obtained in the step 1, and pressing the mixture into a prefabricated body;
step 3, carrying out vacuum or inert atmosphere protection sintering on the prefabricated body, wherein the sintering temperature range is 1100-1175 ℃, the heat preservation time is 10-15 minutes, and the temperature rise and temperature reduction speed ranges are 80-100 ℃/minute and 35-40 ℃/minute respectively;
and 4, annealing heat treatment is carried out on the sintered preform.
5. The nickel-based composite material according to claim 4, wherein the ball milling is performed using a planetary ball mill for 2 to 24 hours.
6. The nickel-based composite material as claimed in claim 5, wherein the ball milling is carried out in a stainless steel tank containing 1:1 mixed stainless steel balls with diameters of 6mm and 10mm respectively, and the ball-to-material ratio is 5-10: 1.
7. The nickel-based composite material according to claim 4, wherein the annealing heat treatment comprises the following specific treatment processes: and (3) preserving the heat for 10-50 minutes at the temperature of 1100 ℃, and then cooling in air.
8. The nickel-based composite material according to claim 4, wherein the pure nickel powder and the pure molybdenum powder have an average particle size of 2 to 10 μm.
9. The nickel-base composite of claim 4 wherein the ball milled mixture is pressed into a preform using a pressure of 20 MPa.
10. The nickel-based composite material according to any one of claims 1 to 9, wherein the nickel-based composite material is applied to a high-temperature molten salt environment.
11. A molten salt reactor core structure, characterized in that the material is the nickel-based composite material as claimed in any one of claims 1 to 10.
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EP2327807A1 (en) * 2008-08-20 2011-06-01 National University Corporation Hokkaido University Oxide-dispersion-strengthened alloy
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