CN111349805A - High-temperature structure function integrated Mg (Al) B2And B4C-co-enhanced aluminum-based neutron absorption material and preparation method thereof - Google Patents
High-temperature structure function integrated Mg (Al) B2And B4C-co-enhanced aluminum-based neutron absorption material and preparation method thereof Download PDFInfo
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- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0057—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
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- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/08—Metals; Alloys; Cermets, i.e. sintered mixtures of ceramics and metals
Abstract
The invention discloses a high-temperature structure function integrated Mg (Al) B2And B4A C-co-enhanced aluminum-based neutron absorption material and a preparation method thereof belong to the technical field of neutron absorption materials and aluminum-based composite materials. The method optimizes the composition of the matrix alloy by B4Pre-oxidizing C particles to increase the wettability of the C particles, heating, pressurizing to a specified density, slowly heating to control in-situ reaction, re-pressurizing to realize densification, and regulating the density after twice pressurization and the heating speed in the in-situ reaction to control the content and uniform distribution of a liquid phase in the sintering process so as to prepare the high-temperature structure function integrationA sub-absorbent material. The invention controls the liquid phase content in the hot pressing sintering process through corresponding hot pressing temperature and heating speed regulation and control, so that the interface reaction is continuously, controllably and thoroughly carried out until the Mg element is exhausted and the liquid phase disappears finally, and the instantaneous liquid phase reaction sintering process is completed. In the obtained material, nano Mg (Al) B2The dispersion is distributed in the matrix, and the high-temperature performance of the material is obviously enhanced.
Description
Technical Field
The invention relates to the technical field of neutron absorption materials and aluminum-based composite materials, in particular to a high-temperature structure function integrated Mg (Al) B2And B4C co-enhanced aluminum-based neutron absorption material and a preparation method thereof.
Background
During the operation of nuclear reactors, nuclear fuel is constantly converted into spent fuel, i.e., spent nuclear fuel. The spent fuel has higher radioactivity, and the safe development of nuclear power requires a reliable spent fuel storage technology. The spent fuel needs neutron absorption materials for shielding protection in the transportation and storage processes, and meanwhile, the reaction is maintained in a subcritical safety state. The current storage method is to use a neutron absorbing material, usually B, which maintains the subcritical state of the spent fuel, in combination with a structural material4The C/Al neutron absorbing material is arranged in the stainless steel plate interlayer. The poor heat conducting capacity of the stainless steel is not beneficial to the heat dissipation of the spent fuel storage device, and water needs to be introduced for cooling, so that the storage device is difficult to maintain, and the safety and reliability of the long-term use of the storage device are reduced. Therefore, more reliable dry storage techniques are needed for spent fuel storage. However, spent fuel dry storage devices are in a high temperature state for long periods of time, normal B4C/Al does not have good high-temperature strength, so that the structural function integrated aluminum-based neutron absorbing material with high temperature resistance and neutron absorbing capacity needs to be developed.
The nanoscale ceramic particles can achieve higher enhancement efficiency in aluminum matrices than do the microscale enhancement phases. The existing data are searched and found, and few reports are reported on the research of the high-temperature-resistant aluminum-based neutron absorption material. Patent application number 201611079600.7' high-temperature structure function integrated B4In the preparation method of the C/Al neutron absorption material, the prepared material has enough high-temperature strength at high temperature, but the preparation process thereofIn order to introduce enough alumina, the flake aluminum needs to be ball milled to be extremely thin, and the grains of the prepared material are too fine, so that the high-temperature and room-temperature plasticity of the material is extremely poor, and the hot working such as extrusion, rolling and the like is very difficult. In addition, the sheet aluminum powder has poor fluidity, so that densification is difficult to realize during sintering, and defects such as holes and the like are easy to occur. Furthermore, the flake aluminum powder has a very low apparent density, making it difficult to prepare large-sized bulk materials. The patent with the application number of CN201711291924.1 discloses a preparation method of a boron carbide reinforced aluminum-based neutron absorption material with integrated high-temperature structure and function, which uses alumina on the surface of superfine aluminum powder with higher cost to reinforce the high-temperature strength of the material and also faces the defect of difficult sintering of the aluminum powder. There are also patents CN201910212249.1, CN201910212574.8 and CN201910212574.8, the preparation process of which requires the use of ball milling of nanoparticles into a matrix, and the process is dangerous and time-consuming, and more importantly, not conducive to large-scale industrial production.
The document "Enhancing high-temperature string of B4C-6061Al neutronabsorber material by in-situ Mg(Al)B2Journal of Nuclear Materials, 2019; 526: 151788 report, B4The C particles can react with Mg in 6061 aluminum matrix to generate nano Mg (Al) B2Particles (MgB)2A certain amount of Mg atoms are replaced by Al atoms), so that the high-temperature performance of the material is improved. However, the content of Mg in a 6061 aluminum matrix is very low (1 wt.%), and elements such as Si and Cu do not have obvious high-temperature reinforcing effect in the material system, so that the high-temperature strength of the material is not enough to meet the actual engineering requirements. If the content of Mg element in the raw material is increased, if the conventional 'heating-pressurizing-cooling' sintering process is still used, a large amount of liquid phase appears in the hot pressing process, and Mg (Al) B is generated in the sintering process2The particles are too large in size and agglomerated, the reinforcing efficiency is low, and due to the fact that liquid sinks under the action of gravity, components are not uniform and even liquid leaks can be caused; on the other hand, if the sintering temperature is lowered, the reaction does not proceed sufficiently, and Mg (Al) B in the final material2The content of particles is small, and a large amount of magnesium element remains, so that the high-temperature strength of the material is insufficient.
Disclosure of Invention
In order to solve the problem of B existing in the prior art4C/Al material having insufficient high-temperature strength or high-temperature B resistance4The invention aims to provide a Mg (Al) B with high-temperature structure and function integration, which has the problems of poor plasticity, difficult processing or high cost of C/Al2And B4The method optimizes the components of matrix alloy, provides a process of heating-pressurizing to specified density, slowly heating to control in-situ reaction and pressurizing again to realize densification, and controls the content and uniform distribution of a liquid phase in a sintering process by specifying the density after pressurizing twice and the heating speed in the in-situ reaction, thereby preparing the neutron absorbing material with high-temperature structure and function integration.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
high-temperature structure function integrated Mg (Al) B2And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material comprises the following steps:
(1) b is to be4Pre-oxidizing the particles C;
(2) mixing the aluminum-magnesium alloy matrix powder with pre-oxidized B4C, uniformly mixing the particles, and putting the formed mixed material into a die for cold pressing;
(3) heating to (Ts-30 ℃) to Ts with a heating speed of S1, wherein Ts is the solidus temperature of the aluminum-magnesium alloy matrix, and then applying a pressure F1 to ensure that the density of the mixed material in the die reaches more than 85%;
(4) lowering the pressure to F2 while decreasing the rate of temperature increase to S2; in the process, only a small amount of liquid phase appears in the matrix after the temperature is raised to the solidus temperature Ts of the aluminum-magnesium alloy matrix, the instantaneous liquid phase reaction sintering process is started, and the nano Mg (Al) B is generated in situ through interface reaction2；
(5) Keeping the pressure at F2 and the heating speed at S2; in the process, along with the progress of the interface reaction, the temperature is slowly increased, and the consumption of Mg element in the matrix gradually increases the solidus temperature of the matrix alloy, so that a proper amount of liquid phase in the matrix is kept to continuously exist, and the interface reaction can be continuously carried out;
(6) stopping when Mg element in the matrix is exhausted and the liquid phase disappearsHeating, and applying pressure F1 again to make the density reach 100%, finally obtaining nano Mg (Al) B2And micron B4C co-reinforcing aluminum-based neutron absorption material billet;
(7) carrying out hot processing on the billet obtained in the step (6) to obtain the Mg (Al) B with the high-temperature structure and function integration2And B4C co-reinforced aluminum-based neutron absorbing material.
In the step (1), the pre-oxidation is carried out in an air atmosphere at 500-600 ℃ for 30-90 min.
In the step (2), the aluminum magnesium alloy matrix powder is formed by mixing elemental Al powder and elemental Mg powder, or the aluminum magnesium alloy matrix powder is Al-Mg alloying powder, or the aluminum magnesium alloy matrix powder is formed by mixing elemental Al powder, elemental Mg powder and Al-Mg alloying powder; b is4C particles are micron-sized and have the size of 1-30 mu m; the mixing mode is mechanical mixing or ball milling mixing; in the mixed material B45-35 wt% of C particles, 2-10 wt% of Mg, and not more than 9/14 × B4And C, particle mass.
In the step (3), the temperature rise speed S1 is 10-20 ℃/min, and the pressure F1 is greater than 30 MPa.
In the step (4), the sintering manner used is hot-pressing sintering (atmosphere or vacuum condition), hot isostatic pressing or spark ion beam sintering.
In the steps (4) - (5), the temperature rise speed S2 is 0.1-2 ℃/min, and the pressure F2 is kept at 7-20 MPa in the temperature rise process.
In the step (6), the temperature at which the temperature increase is stopped is less than 660 ℃.
In the step (7), the hot working is performed by an extrusion, forging or rolling process, and the hot working temperature is 350-.
The design mechanism of the invention is as follows:
the invention provides a method for generating Mg (Al) B by using instantaneous liquid phase sintering and in-situ reaction2A preparation method of a nanoparticle-enhanced neutron absorption material. By the pair B4Pre-oxidation of the C particles to form a layer B on the surface2O3Increasing its surface roughness, thereby increasing its wettability with the liquid phase and promoting interfacial reactions. The time and temperature of the pre-oxidation are specified because too low a pre-oxidation level does not have a significant effect, while too high a pre-oxidation level leads to the formation of B2O3In excess, a large amount of MgO in the final material is detrimental to the material properties. Different from the conventional sintering process of heating-pressurizing-cooling, the invention adopts the process of heating-pressurizing to specified density, slowly heating to control in-situ reaction and pressurizing again to realize densification. For the first pressurization, the minimum compactness is specified in order to prepare for the in situ reaction containing the liquid phase. In this case, if the degree of densification is less than a predetermined value, the liquid phase sinks to form an uneven final material while the temperature is further raised. In the process of slow-speed temperature-rise in-situ reaction, the pressure is reduced to a proper range, so that liquid phase is not extruded, and the specific temperature rise speed is used, so that liquid leakage, uneven material components or generated Mg (Al) B caused by excessive liquid phase can be avoided2Too coarse and agglomerated particles. With the temperature rising, the in-situ reaction generates nano Mg (Al) B2The particles, Mg element, are consumed so that the solidus line of the material also rises continuously. Therefore, when the liquid phase increasing speed caused by temperature rise is basically equal to the liquid phase decreasing speed caused by reaction consumption of Mg element, the reaction can be continuously, controllably and thoroughly carried out on the premise of avoiding the appearance of excessive liquid phase in the sintering process until the Mg element is finally exhausted and the liquid phase disappears, and finally, the solid phase sintering is carried out when the pressure is increased again to finish densification, namely the transient liquid phase reaction sintering process is finished. And nano Mg (Al) B generated2Extremely stable in aluminum and difficult to further coarsen in the presence of only a small amount of liquid phase, so Mg (Al) B in the final material2The particles are fine and dispersed, and the high-temperature strengthening effect is strong.
The invention has the beneficial effects that:
1. the high-temperature structural function integrated neutron absorption material obtained by the method of the invention and the traditional B4Compared with the traditional B neutron absorption material, the C/Al neutron absorption material has excellent mechanical properties at high temperature, for example, the strength can reach 150MPa at 375 ℃, and the C/Al neutron absorption material is more excellent than the traditional B neutron absorption material4The C/Al neutron absorbing material has the advantages of high strength of 70-100 MPa and simultaneously hasGood plasticity, no need of additional equipment, and no excessive cost increase, and can realize the remarkable improvement of the high-temperature strength of the material.
2. By the pair B4The particle C is pre-oxidized to a proper degree, so that the wettability of the particle and the liquid phase can be effectively improved, the liquid phase can be more fully contacted with the particle, the interface reaction can be promoted, and the reaction product is more uniform.
3. Compared with the conventional sintering process of heating-pressurizing-cooling, the method of the invention comprises twice pressurizing, pressurizing to the density of the material favorable for liquid phase reaction at low temperature, slowly heating for in-situ reaction to generate nano Mg (Al) B2And (3) granules. The liquid phase content in the hot pressing process is controlled by controlling the sintering temperature and the heating rate, namely the actual solidus line of the material is gradually increased along with the consumption of Mg element by the interface reaction, so that the sintering temperature is gradually increased, a small amount of liquid phase exists in the heating process, the interface reaction is continuously, stably and fully carried out, and a large amount of fine and dispersed nano Mg (Al) B2And (3) granules. Finally, Mg element is exhausted, the liquid phase disappears, the densification of the material is completed by pressurizing again, and the instantaneous liquid phase reaction sintering process is completed. Finally obtaining nano Mg (Al) B2The structural function integrated neutron absorption material is in dispersion distribution and has good high-temperature performance.
4. Compared with the existing preparation method of the structural function integrated neutron absorption material, the method does not use flake aluminum powder or superfine aluminum powder, does not need a ball milling process, and has low cost and high safety. The powder has high apparent density, good sintering property, compact material and simple and convenient preparation process, can realize large-scale industrial preparation, has good formability and processability, is suitable for the fields of spent fuel dry storage, transportation and the like, and can carry out large-scale industrial production.
5. The process is simple and easy to implement, and can be applied to the fields of dry storage and transportation of the spent fuel of the nuclear power station needing the lasting high-temperature strength and other engineering.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
At 550 ℃ in air to B4Pre-oxidizing the C particles for 45 min. 355g of aluminum powder and B are weighed4125g of C particles and 20g of Mg powder are mixed, and the solidus of the Al-Mg alloy with the composition is about 570 ℃ by inquiring a phase diagram. Heating to 550 deg.C at 15 deg.C/min, applying pressure to 88% density, reducing pressure to 15MPa, heating to 640 deg.C at 1 deg.C/min, increasing pressure again to 100% density, and stopping heating. The sintered ingots were hot extruded at 450 ℃ into a strip sheet at an extrusion ratio of 16: 1. The extruded strip was annealed at 450 ℃ for 8 hours to obtain the final profile.
The final material component is represented by B4C、Mg(Al)B2A structural-functional integrated neutron absorbing material taking pure Al as a matrix as a reinforcing phase, and about 7 wt.% of nano-scale Mg (Al) B2The particles are dispersed in the matrix. The material is subjected to load transfer strengthening and effective pinning of grain boundaries and dislocation, so that the material with good strong plastic matching is obtained.
High-temperature structure function integration B manufactured by adopting the embodiment4Mechanical properties of the C/Al neutron absorbing material at room temperature: the yield strength is 256MPa, the tensile strength is 365MPa, and the elongation is 6%. Mechanical properties at 375 ℃: the yield strength is 116MPa, the tensile strength is 135MPa, and the elongation is 9%.
Comparative example 1
At 550 ℃ in air to B4Pre-oxidizing the C particles for 45 min. 355g of aluminum powder and B are weighed4125g of C particles and 20g of Mg powder. And carrying out vacuum hot-pressing sintering after cold pressing until the density is 60%. The temperature is raised to 550 ℃ at a speed of 15 ℃/min, then raised to 640 ℃ at a speed of 1 ℃/min, and the heating is stopped. The sintered ingots were hot extruded at 450 ℃ into a strip sheet at an extrusion ratio of 16: 1. The extruded strip was annealed at 450 ℃ for 8 hours to obtain the final profile.
Because the density is too low before sintering, the low-melting-point liquid sinks towards each other under the action of gravity, so that the final material components are extremely non-uniform, and the lower material Mg (Al) B2There are significantly more particles than upper. At the same time, the strength of the material is also very uneven.
Comparative example 2
At 550 ℃ in air to B4C granuleThe pellets were pre-oxidized for 45 min. 355g of aluminum powder and B are weighed4125g of C particles and 20g of Mg powder. Heating to 550 deg.C at 15 deg.C/min, applying pressure to 100% under 40MPa, maintaining the pressure, heating at 1 deg.C/min, heating to 640 deg.C, and stopping heating. The sintered ingots were hot extruded at 450 ℃ into a strip sheet at an extrusion ratio of 16: 1. The extruded strip was annealed at 450 ℃ for 8 hours to obtain the final profile.
As the pressure is overlarge in the temperature rise process, the liquid phase in the material is extruded out, and the final material has uneven components and properties.
Comparative example 3
355g of aluminum powder and B are weighed4125g of C particles and 20g of Mg powder are mixed and then sintered by vacuum hot pressing. Heating to 580 deg.C, holding for 2 hr, and pressurizing to complete densification. The sintered ingots were hot extruded at 450 ℃ into a strip sheet at an extrusion ratio of 16: 1. The extruded strip was annealed at 450 ℃ for 8 hours to obtain the final profile.
The final material component is represented by B4C particles and very little Mg (Al) B2The particles are reinforced phase, Al-Mg alloy is used as matrix, in the course of sintering, interface reaction can make Mg element be consumed, solidus line be raised, liquid phase be disappeared, interface reaction can be stopped, so that it only has a very small quantity of nano-grade Mg (Al) B2The particles are dispersed in the matrix. Has no obvious strengthening effect on the material.
The composite material manufactured by adopting the comparative example has the following mechanical properties at room temperature: the yield strength is 176MPa, the tensile strength is 235MPa, and the elongation is 15%. The yield strength is 42MPa, the tensile strength is 48MPa and the elongation is 52 percent at 375 ℃.
Comparative example 4
At 550 ℃ in air to B4Pre-oxidizing the C particles for 45 min. 355g of aluminum powder and B are weighed4125g of C particles and 20g of Mg powder are mixed, and the compactness is pressed to 90% by using isostatic cool pressing and then is sintered by hot pressing in vacuum. Directly heating to 640 ℃ at a speed of 15 ℃/min by a conventional sintering process, preserving heat for 3h, and stopping heating.
Preparation B using this example4When the C/Al neutron absorbing material is used, a large amount of liquid phase flows out in the sintering process, and the material components and the performance are unstable.
Comparative example 5
375g and B of 6061 aluminum alloy powder are weighed4125g of C particles are mixed. And (3) pressing the density to 90% by using cold isostatic pressing, and then carrying out vacuum hot-pressing sintering. And (3) pressing the density to 90% by using cold isostatic pressing, and then carrying out vacuum hot-pressing sintering. The temperature is raised to 550 ℃ at a speed of 15 ℃/min, then raised to 640 ℃ at a speed of 1 ℃/min, and the heating is stopped. The sintered ingots were hot extruded at 450 ℃ into a strip sheet at an extrusion ratio of 16: 1. The extruded strip was annealed at 450 ℃ for 8 hours to obtain the final profile.
The final material component is represented by B4C. Small amount of Mg (Al) B2In order to strengthen the phase, the matrix component is mainly Al, and in addition, a small amount of Si and Cu elements which are not beneficial to the high-temperature performance are contained.
B produced by this example4Mechanical properties of the C/Al neutron absorbing material at room temperature: the yield strength is 220MPa, the tensile strength is 315MPa, and the elongation is 8%. The yield strength is 55MPa, the tensile strength is 62MPa and the elongation is 43 percent at 375 ℃.
Example 2
At 550 ℃ in air to B4Pre-oxidizing the C particles for 45 min. 345g of aluminum powder and B are weighed4125g of C particles and 30g of Mg powder are mixed. And (3) pressing the density to 90% by using cold isostatic pressing, and then carrying out vacuum hot-pressing sintering. Heating to 530 deg.C at 15 deg.C/min, heating to 640 deg.C at 1.5 deg.C/min, and applying pressure to complete densification. The sintered ingot was rolled into a strip at 450 ℃ with a deformation ratio of 10: 1. The strip was annealed at 450 ℃ for 8 hours to obtain the final profile.
The final material component is represented by B4C、Mg(Al)B2The structural-function integrated neutron absorption material taking pure Al as a matrix as a reinforcing phase has about 11.5 wt.% of nano-scale Mg (Al) B2The particles are distributed in the matrix. The material is subjected to load transfer strengthening and effective pinning of grain boundaries and dislocation, so that the material with good strong plastic matching is obtained.
High-temperature structure function integration B manufactured by adopting the embodiment4Mechanical properties of the C/Al neutron absorbing material at room temperature: the yield strength is 326MPa, the tensile strength is 420MPa, and the elongation is 4%. The yield strength is 134MPa, the tensile strength is 150MPa and the elongation is 7 percent at 375 ℃.
The above embodiments are described for the purpose of illustrating the features and advantages of the present invention, and are not intended to limit the scope of the claims.
Claims (9)
1. High-temperature structure function integrated Mg (Al) B2And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: the method comprises the following steps:
(1) b is to be4Pre-oxidizing the particles C;
(2) mixing the aluminum-magnesium alloy matrix powder with pre-oxidized B4C, uniformly mixing the particles, and putting the formed mixed material into a die for cold pressing;
(3) heating to (Ts-30 ℃) to Ts with a heating speed of S1, wherein Ts is the solidus temperature of the aluminum-magnesium alloy matrix, and then applying a pressure F1 to ensure that the density of the mixed material in the die reaches more than 85%;
(4) lowering the pressure to F2 while decreasing the rate of temperature increase to S2; in the process, only a small amount of liquid phase appears in the matrix after the temperature is raised to the solidus temperature Ts of the aluminum-magnesium alloy matrix, the instantaneous liquid phase reaction sintering process is started, and the nano Mg (Al) B is generated in situ through interface reaction2；
(5) Keeping the pressure at F2 and the heating speed at S2; in the process, along with the progress of the interface reaction, the temperature is slowly increased, and the consumption of Mg element in the matrix gradually increases the solidus temperature of the matrix alloy, so that a proper amount of liquid phase in the matrix is kept to continuously exist, and the interface reaction can be continuously carried out;
(6) stopping heating after the Mg element in the matrix is exhausted and the liquid phase disappears, applying pressure F1 again to make the density reach 100%, and finally obtaining nano Mg (Al) B2And micron B4C co-reinforcing aluminum-based neutron absorption material billet;
(7) carrying out hot processing on the billet obtained in the step (6) to obtain the Mg (Al) B with the high-temperature structure and function integration2And B4C co-reinforced aluminum-based neutron absorbing material.
2. The chair of claim 1Temperature structure function integrated Mg (Al) B2And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the step (1), the pre-oxidation is carried out in an air atmosphere at 500-600 ℃ for 30-90 min.
3. High temperature structural and functional integration Mg (Al) B as claimed in claim 12And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the step (2), the aluminum magnesium alloy matrix powder is formed by mixing Al elemental powder and Mg elemental powder, or the aluminum magnesium alloy matrix powder is Al-Mg alloying powder, or the aluminum magnesium alloy matrix powder is formed by mixing Al elemental powder, Mg elemental powder and Al-Mg alloying powder; b is4C particles are micron-sized and have the size of 1-30 mu m; the mixing mode is mechanical mixing or ball milling mixing; in the mixed material B45-35 wt% of C particles, 2-10 wt% of Mg, and not more than 9/14 × B4And C, particle mass.
4. High temperature structural and functional integration Mg (Al) B as claimed in claim 12And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the step (3), the temperature rising speed S1 is 10-20 ℃/min, and the pressure F1 is greater than 30 MPa.
5. High temperature structural and functional integration Mg (Al) B as claimed in claim 12And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the step (4), the sintering mode is hot-pressing sintering (atmosphere or vacuum condition), hot isostatic pressing or spark ion beam sintering.
6. High temperature structural and functional integration Mg (Al) B as claimed in claim 12And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the steps (4) - (5), the temperature rising speed S2 is 0.1-2 ℃/min, and the pressure F2 is kept at 7-20 MPa in the temperature rising process.
7. High temperature structural and functional integration Mg (Al) B as claimed in claim 12And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the step (6), the temperature at which the temperature rise is stopped is less than 660 ℃.
8. High temperature structural and functional integration Mg (Al) B as claimed in claim 12And B4The preparation method of the C-co-enhanced aluminum-based neutron absorption material is characterized by comprising the following steps of: in the step (7), the hot working adopts an extrusion, forging or rolling process, and the hot working temperature is 350-.
9. A high temperature structurally functional integrated Mg (Al) B prepared by the method of any one of claims 1 to 82And B4The C co-enhanced aluminum-based neutron absorption material is characterized in that: the aluminum-based neutron absorbing material is made of nano Mg (Al) B2Particles and B4The C particles are uniformly distributed in the aluminum matrix.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112853139A (en) * | 2021-01-18 | 2021-05-28 | 武汉理工大学 | Preparation method of iron-aluminum intermetallic compound porous material |
| CN113458394A (en) * | 2021-05-20 | 2021-10-01 | 中国工程物理研究院材料研究所 | Homogeneous boron carbide/aluminum composite material with high boron carbide content and preparation method thereof |
| CN114538447A (en) * | 2022-03-22 | 2022-05-27 | 哈尔滨工业大学 | Low-cost rapid B4C powder surface modification method for inhibiting B4C/Al composite material interface brittle phase |
| CN114703389A (en) * | 2022-03-09 | 2022-07-05 | 哈尔滨工业大学 | Low stress shaping B4Preparation method of C/Al composite material section bar |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5433214A (en) * | 1977-08-18 | 1979-03-10 | Sumitomo Light Metal Ind | Structural aluminum alloy materials having good neutron barrier effect and corrosion resistivity |
| CN104164601A (en) * | 2014-08-13 | 2014-11-26 | 扬州峰明金属制品有限公司 | Multielement-reinforced heat-resistant magnesium alloy and manufacturing method thereof |
| CN106811613A (en) * | 2015-11-30 | 2017-06-09 | 北京有色金属研究总院 | A kind of high-volume fractional B4C mixes enhanced aluminum matrix composite and its preparation technology with Si particles |
| CN108130438A (en) * | 2017-12-08 | 2018-06-08 | 中国科学院金属研究所 | A kind of preparation method of thermal structure function integration boron carbide enhancing aluminium base neutron absorber material |
-
2020
- 2020-03-23 CN CN202010206265.2A patent/CN111349805B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5433214A (en) * | 1977-08-18 | 1979-03-10 | Sumitomo Light Metal Ind | Structural aluminum alloy materials having good neutron barrier effect and corrosion resistivity |
| CN104164601A (en) * | 2014-08-13 | 2014-11-26 | 扬州峰明金属制品有限公司 | Multielement-reinforced heat-resistant magnesium alloy and manufacturing method thereof |
| CN106811613A (en) * | 2015-11-30 | 2017-06-09 | 北京有色金属研究总院 | A kind of high-volume fractional B4C mixes enhanced aluminum matrix composite and its preparation technology with Si particles |
| CN108130438A (en) * | 2017-12-08 | 2018-06-08 | 中国科学院金属研究所 | A kind of preparation method of thermal structure function integration boron carbide enhancing aluminium base neutron absorber material |
Non-Patent Citations (1)
| Title |
|---|
| Y.N. ZAN ET AL: "Enhancing high-temperature strength of B4C-6061Al neutron absorber material by in-situ Mg(Al)B2", 《JOURNAL OF NUCLEAR MATERIALS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112853139A (en) * | 2021-01-18 | 2021-05-28 | 武汉理工大学 | Preparation method of iron-aluminum intermetallic compound porous material |
| CN113458394A (en) * | 2021-05-20 | 2021-10-01 | 中国工程物理研究院材料研究所 | Homogeneous boron carbide/aluminum composite material with high boron carbide content and preparation method thereof |
| CN114703389A (en) * | 2022-03-09 | 2022-07-05 | 哈尔滨工业大学 | Low stress shaping B4Preparation method of C/Al composite material section bar |
| CN114538447A (en) * | 2022-03-22 | 2022-05-27 | 哈尔滨工业大学 | Low-cost rapid B4C powder surface modification method for inhibiting B4C/Al composite material interface brittle phase |
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