CN108484208B - Mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation and preparation method thereof - Google Patents

Mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation and preparation method thereof Download PDF

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CN108484208B
CN108484208B CN201810186349.7A CN201810186349A CN108484208B CN 108484208 B CN108484208 B CN 108484208B CN 201810186349 A CN201810186349 A CN 201810186349A CN 108484208 B CN108484208 B CN 108484208B
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mullite
corundum
foamed ceramic
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CN108484208A (en
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贾文宝
汪瑜凡
陈若愚
金利民
黑大千
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention relates to a neutron shielding foamed ceramic for mullite/corundum-based spent fuel storage and transportation and a preparation method thereof, wherein firstly, sillimanite, alumina micro powder, kaolin, an additive, carboxyethyl cellulose, carboxymethyl cellulose, polycarboxylate, ethanol and deionized water are mixed uniformly to prepare slurry I; mixing gadolinium oxide micropowder, sillimanite, alumina micropowder, polyacrylate, ethanol and deionized water to obtain slurry II; soaking polyurethane sponge in the slurry I to prepare a foamed ceramic preform; and (3) carrying out vacuum impregnation on the foamed ceramic preform by using the slurry II, and treating to obtain a mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic blank, and finally obtaining the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic. The prepared mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation has the advantages of simple process, low cost, small volume density, high strength, high temperature resistance, excellent chemical erosion resistance and excellent neutron shielding performance.

Description

Mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation and preparation method thereof
Technical Field
The invention belongs to the technical field of foamed ceramics, and particularly relates to a mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation and a preparation method thereof.
Background
With the rapid development of science and technology, the application of nuclear energy and nuclear technology has been developed rapidly in recent years. The traditional neutron shielding material can not completely meet the protection requirements of nuclear power ships or movable radioactive sources, for example, the traditional lead-containing shielding material has poor neutron shielding effect and pollutes the environment to harm the health of human bodies; the shielding concrete has large volume, is difficult to move and has poor erosion resistance; the thermal neutron absorption performance of the boron element is decreased along with the reaction with neutrons. Therefore, the research and development of the radiation-proof material with small volume density, excellent physical property, good shielding effect and environmental friendliness is a problem to be solved urgently. The neutron absorption material adopted by the invention is gadolinium oxide micro powder. Gadolinium has an extremely high thermal neutron absorption cross section, and isotope absorption cross sections of gadolinium are Gd-155(60600b) and Gd-157(139000b), so that gadolinium is an excellent neutron absorption material.
The foamed ceramic has unique three-dimensional and curved-hole net-shaped framework structure, so that the foamed ceramic has the open porosity of 80-90%, and is light in weight and strong in mechanical property, so that the foamed ceramic is widely applied to the industries of aerospace, catalytic adsorption, fire resistance, heat insulation and the like. However, the foamed ceramics prepared by the organic foam impregnation method has poor mechanical properties due to the formation of hollow cell ribs by decomposition of polyurethane during calcination and a large number of defects on the surface of the ceramic-based cell ribs.
At present, technicians carry out intensive research and technical development for the preparation of high-performance radiation shielding materials and other problems:
the patent technology of "a neutron absorbing material and a preparation method thereof" (CN201510701250) discloses a composite material which is prepared from boron carbide, a neutron absorber, aluminum and an aluminum alloy and mainly aims at neutron shielding for spent fuel storage. The method improves the plasticity of the composite material on the basis of ensuring the neutron shielding efficiency to a certain extent, and improves the production efficiency. But its main drawbacks are: (1) the process is complex and the rate of finished products is low; (2) the corrosion resistance is not strong in wet storage; (3) the bulk density is high.
The patent technology of 'neutron shielding material and preparation process' (ZL201210156866) discloses that ultra-high molecular weight polyethylene, boron compound, stearic acid or salt thereof, coupling agent and the like are mixed in a stirrer and stirred uniformly. Heating to 200 ℃ in a grinding tool, placing in a mould, pressurizing, molding, demoulding and cooling to obtain the neutron shielding material. The method reduces production cost and prolongs service life to a certain extent. But its main drawbacks are: (1) the mechanical properties are not high; (2) the use temperature is low; (3) the corrosion resistance is weak; (4) poor radiation aging resistance; (5) the bulk density is high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and prepare the mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation. The prepared mullite/corundum-based neutron shielding foamed ceramic for storage and transportation of spent fuel has the advantages of small volume density, high strength, excellent thermal shock resistance, high temperature resistance, strong corrosion resistance and good shielding effect on thermal neutrons, can be applied to a neutron field radiation environment, and is particularly suitable for storage of spent fuel, grillwork for transportation and container materials.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a neutron shielding foamed ceramic for storing and transporting mullite/corundum-based spent fuel comprises the following steps:
step one, mixing 50-70 parts by mass of sillimanite, 15-30 parts by mass of alumina micro powder, 10-20 parts by mass of kaolin and 3-5 parts by mass of additives to obtain mixed powder I; adding 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water into the mixed powder I, and performing ball milling for 1-1.5 hours to obtain slurry I;
step two, obtaining mixed powder II by using 20-50 parts by mass of gadolinium oxide micro powder, 15-30 parts by mass of aluminum oxide micro powder and 30-40 parts by mass of sillimanite, adding 0.3-1.6 parts by mass of polycarboxylate, 0.3-2 parts by mass of polyacrylate, 0.1-0.7 part by mass of ethanol and 25-50 parts by mass of deionized water into the mixed powder II, and mechanically ball-milling for 2-3 hours to obtain slurry II;
step three, soaking polyurethane sponge into the slurry I under a vacuum condition, extruding or centrifugally throwing the slurry after soaking, naturally drying for 12-24 hours to obtain a prefabricated green body, then carrying out vacuum soaking on the prefabricated green body by using the slurry II, blowing compressed air or centrifugally throwing the slurry after soaking, naturally drying, and baking for 12-24 hours at 70-100 ℃ to obtain a mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic blank;
and step four, placing the mullite/corundum-based fuel storage and transportation neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 230 ℃ at the speed of 2-3 ℃/min in the air atmosphere, heating to 700 ℃ at the speed of 0.5-1 ℃/min, then heating to 1450-1550 ℃ at the speed of 3 ℃/min, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic.
The chemical components of the sillimanite are as follows: SiO 2232 to 37wt% of Al2O361-65 wt%, TiO20.2 to 1.3wt%, CaO 0.3 to 1.5wt%, MgO 0.4 to 0.5wt%, and Na2O+K20.1-0.7 wt% of O and 1-3 wt% of loss on ignition; the average grain size of the sillimanite is less than or equal to 8 mu m.
The chemical components of the kaolin are as follows: : al (Al)2O340 to 50wt% of SiO245 to 55wt% of Fe2O30.5 to 2wt%, CaO 0.4 to 0.6wt%, MgO 0.2 to 0.4wt%, TiO20.5 to 1.0wt%, and 0.5 to 2.5wt% loss on ignition; the average particle size of the kaolin is less than or equal to 5 mu m.
The average grain size of the alumina micro powder is less than or equal to 5 mu m.
The additive is one or more of magnesium oxide micro powder, cerium oxide micro powder and zirconium oxide micro powder; the average particle size of the magnesium oxide micro powder, the cerium oxide micro powder and the zirconium oxide micro powder is less than or equal to 25 mu m.
The average particle size of the gadolinium oxide micro powder is less than or equal to 10 mu m.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a neutron shielding foamed ceramic for mullite/corundum-based spent fuel storage and transportation and a preparation method thereof, wherein firstly, sillimanite, alumina micro powder, kaolin, an additive, carboxyethyl cellulose, carboxymethyl cellulose, polycarboxylate, ethanol and deionized water are mixed uniformly to prepare slurry I; mixing gadolinium oxide micropowder, sillimanite, alumina micropowder, polyacrylate, ethanol and deionized water to obtain slurry II; soaking polyurethane sponge in the slurry I, squeezing or centrifugally throwing the slurry, drying and preserving heat to obtain a foamed ceramic preform; then, carrying out vacuum impregnation, extrusion or centrifugal slurry throwing on the foamed ceramic preform by using the slurry II, naturally drying, and baking for 12-24 hours at the temperature of 70-100 ℃ to obtain a mullite/corundum-based spent fuel neutron shielding spent foamed ceramic blank for storage and transportation; and finally, preserving the heat for 2-5 hours under the conditions of air atmosphere and 1450-1550 ℃, and obtaining the mullite/corundum-based spent fuel neutron shielding foamed ceramic for storage and transportation.
The invention relates to a neutron shielding foamed ceramic for mullite/corundum-based spent fuel storage and transportation, which is prepared by adopting secondary coating and vacuum impregnation grouting technologies. The prefabricated slurry is coated on the surface of the mullite/corundum-based ceramic prefabricated body and inside the hollow pore ribs by the technology, so that the defects and the hollow pore ribs of the mullite/corundum-based foamed ceramic, which are generated by volatilization of the polyurethane sponge, can be repaired, and the mechanical property and the thermal shock stability of the mullite/corundum-based foamed ceramic are improved. Based on the fact that a large amount of ceramic slurry is adsorbed on the surface of the polyurethane sponge body after the first slurry hanging, the affinity between the surface of the foamed ceramic body and the inorganic slurry is improved, and therefore the adhesion amount of the slurry on the foamed ceramic body can be effectively improved through the second slurry hanging. Meanwhile, the slurry II is mainly prepared from gadolinium oxide micro powder, sillimanite and alumina micro powder, and the sillimanite is decomposed at high temperature to generate mullite and silicon dioxide to generate an expansion effect, so that the linear shrinkage generated by a sample calcined at high temperature can be offset, and the yield of the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic is improved; the thermal neutron absorption cross section of gadolinium oxide is far larger than that of other materials, so that the gadolinium oxide has extremely strong neutron absorption capacity, and the neutron shielding performance of gadolinium is dozens of times or even hundreds of times of that of the currently common B element. After preparing a foamed ceramic blank, calcining the foamed ceramic blank by a secondary slurry coating process, and then using Gd as gadolinium element2Si2O7And Al5Gd3O12The equal ceramic phase exists in the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic, and the volume density of the element gadolinium is about 0.05-0.065 g/cm3. By MCNP simulation, the volume density of gadolinium element is calculated to be 0.05g/cm3When the thickness of the foamed ceramic is 2cm, more than 99% of thermal neutrons can be shielded. Meanwhile, based on a 300mCi Am-Be neutron source in a laboratory, after polyethylene moderation treatment, the thermal neutron transmittance measured by the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic prepared by the method is lower than 5 percent, wherein the thickness of the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic is 2 cm. Through detection, the volume density of the neutron shielding foamed ceramic for storing and transporting the mullite/corundum-based spent fuel prepared by the invention is 0.3-0.6 g/cm3(ii) a The normal-temperature compressive strength is 1.49-2.53 MPa; the compressive strength of the sample after the alkali solution is washed and eroded for 15-20 h is 1.33-2.32 MPa. Therefore, the mullite/corundum-based neutron shielding foamed ceramic prepared by the method can meet the requirements of the spent fuel storage and transportation for long-term use, light weight and portability in China at present and in the future.
Therefore, the prepared mullite/corundum-based neutron shielding foamed ceramic for storage and transportation of spent fuel has the advantages of simple process, low cost, small volume density, high strength, high temperature resistance, excellent chemical erosion resistance and excellent neutron shielding performance.
Detailed Description
The invention is further described with reference to specific embodiments, which do not limit the scope of the invention.
In order to avoid repetition, the technical parameters to be related in this specific embodiment are described in a unified manner as follows, which will not be described in the embodiments:
the main chemical components of the sillimanite are as follows: SiO 2232 to 37wt% of Al2O361-65 wt%, TiO20.2 to 1.3wt%, CaO 0.3 to 1.5wt%, MgO 0.4 to 0.5wt%, and Na2O+K20.1-0.7 wt% of O and 1-3 wt% of loss on ignition; the average grain size of the sillimanite is less than or equal to 8 mu m.
The kaolin comprises the following main chemical components: a. thel2O340 to 50wt% of SiO245 to 55wt% of Fe2O30.5 to 2wt%, CaO 0.4 to 0.6wt%, MgO 0.2 to 0.4wt%, TiO20.5 to 1.0wt%, and a loss on ignition of 0.5 to 2.5 wt%; the average particle size of the kaolin is less than or equal to 5 mu m.
The average particle size of the alumina micro powder is less than or equal to 5 mu m.
The average particle size of the magnesium oxide micro powder, the cerium oxide micro powder and the zirconium oxide micro powder is less than or equal to 25 mu m.
The average particle size of the gadolinium oxide micro powder is less than or equal to 10 mu m.
Example 1
A neutron shielding foamed ceramic for mullite/corundum-based spent fuel storage and transportation and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
step one, mixing 50-60 parts by mass of sillimanite, 22-30 parts by mass of alumina micro powder and 10-20 parts by mass of kaolin with 3-5 parts by mass of cerium oxide to obtain mixed powder I, adding 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water into the mixed powder I, and performing ball milling for 1-1.5 hours to obtain slurry I;
step two, obtaining mixed powder II by using 20-30 parts by mass of gadolinium oxide micro powder, 15-30 parts by mass of aluminum oxide micro powder and 30-40 parts by mass of sillimanite, adding 0.3-1.6 parts by mass of polycarboxylate, 0.3-2 parts by mass of polyacrylate, 0.1-0.7 parts by mass of ethanol and 25-50 parts by mass of deionized water into the mixed powder II, and mechanically milling for 2-3 hours to obtain slurry II;
step three, soaking polyurethane sponge into the slurry I under a vacuum condition, injecting compressed air or centrifugally throwing slurry after soaking, naturally drying for 12-24 hours to obtain a prefabricated green body, then performing vacuum soaking on the prefabricated green body by using the slurry II, injecting compressed air or centrifugally throwing slurry after soaking, naturally drying, and baking for 12-24 hours at 70-100 ℃ to obtain a mullite/corundum-based neutron shielding foamed ceramic body;
and step four, placing the mullite/corundum-based fuel storage and transportation neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 230 ℃ at the speed of 2-3 ℃/min in the air atmosphere, heating to 700 ℃ at the speed of 0.5-1 ℃/min, then heating to 1450-1550 ℃ at the speed of 3 ℃/min, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the mullite/corundum-based fuel storage and transportation neutron shielding foamed ceramic.
The neutron shielding foamed ceramic prepared in the embodiment 1 is detected as follows: the bulk density is 0.3 to 0.42g/cm3(ii) a The normal-temperature compressive strength is 1.9-2.53 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 1.57-2.32 MPa; after the 300mCi Am-Be neutron source is subjected to polyethylene moderation treatment, the ratio of the thermal neutron flux detected by a He-3 detector to the neutron flux without the shielding material, namely the transmittance, is lower than 5%.
Example 2
A neutron shielding foamed ceramic for storing and transporting mullite/corundum-based spent fuel and a preparation method thereof. The preparation method shown in this example is the same as that of example 1 except for the first step and the second step.
Step one, 50-60 parts by mass of sillimanite, 22-30 parts by mass of alumina micro powder, 10-20 parts by mass of kaolin, 1-2 parts by mass of magnesium oxide and 2-3 parts by mass of zirconium oxide are mixed to obtain mixed powder I, 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water are added into the mixed powder I, and ball milling is carried out for 1-1.5 hours to obtain slurry I.
Step two, mixing 30-40 parts by mass of gadolinium oxide micro powder, 15-30 parts by mass of aluminum oxide micro powder and 30-40 parts by mass of sillimanite to obtain mixed powder II, adding 0.3-1.6 parts by mass of polycarboxylate, 0.3-2 parts by mass of polyacrylate, 0.1-0.7 parts by mass of ethanol and 25-50 parts by mass of deionized water into the mixed powder II, and mechanically milling for 2-3 hours to obtain slurry II;
example 2 preparation ofThe prepared neutron shielding foamed ceramic is detected as follows: the bulk density is 0.31 to 0.46g/cm3(ii) a The normal-temperature compressive strength is 1.83-2.31 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 1.56-2.28 MPa; after the 300mCi Am-Be neutron source is subjected to polyethylene moderation treatment, the ratio of the thermal neutron flux detected by a He-3 detector to the neutron flux without the shielding material, namely the transmittance, is lower than 5%.
Example 3
A neutron shielding foamed ceramic for storing and transporting mullite/corundum-based spent fuel and a preparation method thereof. The preparation method shown in this example is the same as that of example 1 except for the first step and the second step.
Step one, mixing 50-60 parts by mass of sillimanite, 22-30 parts by mass of alumina micro powder and 10-20 parts by mass of kaolin with 3-5 parts by mass of cerium oxide to obtain mixed powder I, adding 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water into the mixed powder I, and performing ball milling for 1-1.5 hours to obtain slurry I.
Step two, mixing 40-50 parts by mass of gadolinium oxide micro powder, 15-30 parts by mass of aluminum oxide micro powder and 30-40 parts by mass of sillimanite to obtain mixed powder II, adding 0.3-1.6 parts by mass of polycarboxylate, 0.3-2 parts by mass of polyacrylate, 0.1-0.7 parts by mass of ethanol and 25-50 parts by mass of deionized water into the mixed powder II, and mechanically milling for 2-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 3 is detected as follows: the bulk density is 0.27 to 0.53g/cm3(ii) a The normal-temperature compressive strength is 1.79-2.33 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 1.49-2.15 MPa; after the 300mCi Am-Be neutron source is subjected to polyethylene moderation treatment, the ratio of the thermal neutron flux detected by a He-3 detector to the neutron flux without the shielding material, namely the transmittance, is lower than 1%.
Example 4
A neutron shielding foamed ceramic for storing and transporting mullite/corundum-based spent fuel and a preparation method thereof. The preparation method shown in this example is the same as that of example 1 except for the first step.
Step one, 60-70 parts by mass of sillimanite, 15-22 parts by mass of alumina micro powder, 10-20 parts by mass of kaolin, 1-2 parts by mass of magnesium oxide and 2-3 parts by mass of zirconium oxide are mixed to obtain mixed powder I, 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water are added into the mixed powder I, and ball milling is carried out for 1-1.5 hours to obtain slurry I.
The neutron shielding foamed ceramic prepared in the embodiment 4 is detected as follows: the bulk density is 0.38-0.44 g/cm3(ii) a The normal-temperature compressive strength is 1.57-2.20 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 1.39-2.02 MPa; after the 300mCi Am-Be neutron source is subjected to polyethylene moderation treatment, the ratio of the thermal neutron flux detected by a He-3 detector to the neutron flux without the shielding material, namely the transmittance, is lower than 5%.
Example 5
A neutron shielding foamed ceramic for storing and transporting mullite/corundum-based spent fuel and a preparation method thereof. The preparation method shown in this example is the same as that of example 2 except for the first step.
Step one, 60-70 parts by mass of sillimanite, 15-22 parts by mass of alumina micro powder and 10-20 parts by mass of kaolin plus 3-5 parts by mass of cerium oxide are mixed to obtain mixed powder I, 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water are added into the mixed powder I, and ball milling is carried out for 1-1.5 hours to obtain slurry I.
The neutron shielding foamed ceramic prepared in the embodiment 5 is detected as follows: the bulk density is 0.31 to 0.47g/cm3(ii) a The normal-temperature compressive strength is 1.49-2.01 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali solution is 1.33-1.97 MPa; 300mCi Am-Be neutron source, passing through polyethyleneAfter the alkene is subjected to moderation treatment, the ratio of the thermal neutron flux detected by a He-3 detector to the neutron flux without the shielding material, namely the transmittance, is lower than 5%.
Example 6
A neutron shielding foamed ceramic for storing and transporting mullite/corundum-based spent fuel and a preparation method thereof. The preparation method shown in this example is the same as that of example 3 except for the first step.
Step one, 60-70 parts by mass of sillimanite, 15-22 parts by mass of alumina micro powder, 10-20 parts by mass of kaolin, 1-2 parts by mass of magnesium oxide and 2-3 parts by mass of zirconium oxide are mixed to obtain mixed powder I, 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water are added into the mixed powder I, and ball milling is carried out for 1-1.5 hours to obtain slurry I.
The neutron shielding foamed ceramic prepared in the embodiment 6 is detected as follows: the bulk density is 0.43 to 0.62g/cm3(ii) a The normal-temperature compressive strength is 1.62-2.36 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 1.53-2.12 MPa; after the 300mCi Am-Be neutron source is subjected to polyethylene moderation treatment, the ratio of the thermal neutron flux detected by a He-3 detector to the neutron flux without the shielding material, namely the transmittance, is lower than 1%.
The invention relates to a neutron shielding foamed ceramic for mullite/corundum-based spent fuel storage and transportation, which is prepared by adopting secondary coating and vacuum impregnation grouting technologies. The prefabricated slurry is coated on the surface of the mullite/corundum-based ceramic prefabricated body and inside the hollow pore ribs by the technology, so that the defects and the hollow pore ribs of the mullite/corundum-based foamed ceramic, which are generated by volatilization of the polyurethane sponge, can be repaired, and the mechanical property and the thermal shock stability of the mullite/corundum-based foamed ceramic are improved. Based on the fact that a large amount of ceramic slurry is adsorbed on the surface of the polyurethane sponge body after the first slurry hanging, the affinity between the surface of the foamed ceramic body and the inorganic slurry is improved, and therefore the adhesion amount of the slurry on the foamed ceramic body can be effectively improved through the second slurry hanging. Meanwhile, the slurry II is prepared from gadolinium oxide micropowder, sillimanite and oxygenThe alumina micropowder is used as a main raw material, and mainly because the sillimanite is decomposed at high temperature to generate mullite and silicon dioxide to generate an expansion effect which can offset the linear shrinkage generated by a sample calcined at high temperature and improve the yield of the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic; the thermal neutron absorption cross section of gadolinium oxide is far larger than that of other materials, so that the gadolinium oxide has extremely strong neutron absorption capacity, and the neutron shielding performance of gadolinium is dozens of times or even hundreds of times of that of the currently common B element. After preparing a foamed ceramic blank, calcining the foamed ceramic blank by a secondary slurry coating process, and then using Gd as gadolinium element2Si2O7And Al5Gd3O12The equal ceramic phase exists in the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic, and the volume density of the element gadolinium is about 0.05-0.065 g/cm3. By MCNP simulation, the volume density of gadolinium element is calculated to be 0.05g/cm3When the thickness of the foamed ceramic is 2cm, more than 99% of thermal neutrons can be shielded. Meanwhile, based on a 300mCi Am-Be neutron source in a laboratory, after polyethylene moderation treatment, the thermal neutron transmittance measured by the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic prepared by the method is lower than 5 percent, wherein the thickness of the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic is 2 cm. Through detection, the volume density of the neutron shielding foamed ceramic for storing and transporting the mullite/corundum-based spent fuel prepared by the invention is 0.3-0.6 g/cm3(ii) a The normal-temperature compressive strength is 1.49-2.53 MPa; the compressive strength of the sample after the alkali solution is washed and eroded for 15-20 h is 1.33-2.32 MPa. Therefore, the mullite/corundum-based neutron shielding foamed ceramic prepared by the method can meet the requirements of the spent fuel storage and transportation for long-term use, light weight and portability in China at present and in the future.
Therefore, the prepared mullite/corundum-based neutron shielding foamed ceramic for storage and transportation of spent fuel has the advantages of simple process, low cost, small volume density, high strength, high temperature resistance, excellent chemical erosion resistance and excellent neutron shielding performance.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.

Claims (4)

1. A mullite/corundum-based neutron shielding foamed ceramic for spent fuel storage and transportation is characterized in that: the preparation method comprises the following steps:
step one, mixing 50-70 parts by mass of sillimanite, 15-30 parts by mass of alumina micro powder, 10-20 parts by mass of kaolin and 3-5 parts by mass of additives to obtain mixed powder I; adding 0.3-2.1 parts by mass of carboxyethyl cellulose, 0.3-1.5 parts by mass of carboxymethyl cellulose, 0.2-1.2 parts by mass of polycarboxylate, 0.1-1.5 parts by mass of ethanol and 20-45 parts by mass of deionized water into the mixed powder I, and performing ball milling for 1-1.5 hours to obtain slurry I;
step two, obtaining mixed powder II by using 20-50 parts by mass of gadolinium oxide micro powder, 15-30 parts by mass of aluminum oxide micro powder and 30-40 parts by mass of sillimanite, adding 0.3-1.6 parts by mass of polycarboxylate, 0.3-2 parts by mass of polyacrylate, 0.1-0.7 part by mass of ethanol and 25-50 parts by mass of deionized water into the mixed powder II, and mechanically ball-milling for 2-3 hours to obtain slurry II;
step three, soaking polyurethane sponge into the slurry I under a vacuum condition, extruding or centrifugally throwing the slurry after soaking, naturally drying for 12-24 hours to obtain a prefabricated green body, then carrying out vacuum soaking on the prefabricated green body by using the slurry II, blowing compressed air or centrifugally throwing the slurry after soaking, naturally drying, and baking for 12-24 hours at 70-100 ℃ to obtain a mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic blank;
putting the mullite/corundum-based fuel storage and transportation neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 230 ℃ at the speed of 2-3 ℃/min in the air atmosphere, heating to 700 ℃ at the speed of 0.5-1 ℃/min, then heating to 1450-1550 ℃ at the speed of 3 ℃/min, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the mullite/corundum-based spent fuel storage and transportation neutron shielding foamed ceramic;
the chemical components of the sillimanite are as follows: SiO 2232 to 37wt% of Al2O361-65 wt%, TiO20.2 to 1.3wt%, CaO 0.3 to 1.5wt%, MgO 0.4 to 0.5wt%, and Na2O+K20.1-0.7 wt% of O and 1-3 wt% of loss on ignition; the average grain size of the sillimanite is less than or equal to 8 mu m;
the chemical components of the kaolin are as follows: al (Al)2O340 to 50wt% of SiO245 to 55wt% of Fe2O30.5 to 2wt%, CaO 0.4 to 0.6wt%, MgO 0.2 to 0.4wt%, TiO20.5 to 1.0wt%, and 0.5 to 2.5wt% loss on ignition; the average particle size of the kaolin is less than or equal to 5 mu m.
2. The mullite/corundum-based spent fuel handling neutron shielding ceramic foam according to claim 1, wherein: the average grain size of the alumina micro powder is less than or equal to 5 mu m.
3. The mullite/corundum-based spent fuel handling neutron shielding ceramic foam according to claim 1, wherein: the additive is one or more of magnesium oxide micro powder, cerium oxide micro powder and zirconium oxide micro powder; the average particle size of the magnesium oxide micro powder, the cerium oxide micro powder and the zirconium oxide micro powder is less than or equal to 25 mu m.
4. The mullite/corundum-based spent fuel handling neutron shielding ceramic foam according to claim 1, wherein: the average particle size of the gadolinium oxide micro powder is less than or equal to 10 mu m.
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