CN108409307B - Neutron shielding foamed ceramic and preparation method thereof - Google Patents
Neutron shielding foamed ceramic and preparation method thereof Download PDFInfo
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- CN108409307B CN108409307B CN201810257493.5A CN201810257493A CN108409307B CN 108409307 B CN108409307 B CN 108409307B CN 201810257493 A CN201810257493 A CN 201810257493A CN 108409307 B CN108409307 B CN 108409307B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims abstract description 24
- 229940075613 gadolinium oxide Drugs 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 13
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 13
- 229920003064 carboxyethyl cellulose Polymers 0.000 claims abstract description 13
- 229920005646 polycarboxylate Polymers 0.000 claims abstract description 13
- 229920000193 polymethacrylate Polymers 0.000 claims abstract description 13
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 13
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 13
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 13
- 239000004927 clay Substances 0.000 claims abstract description 11
- 238000005470 impregnation Methods 0.000 claims abstract description 11
- 229920002635 polyurethane Polymers 0.000 claims abstract description 9
- 239000004814 polyurethane Substances 0.000 claims abstract description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims description 44
- 238000003801 milling Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000006260 foam Substances 0.000 claims description 10
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 10
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 9
- 229940075630 samarium oxide Drugs 0.000 claims description 9
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 9
- 239000002689 soil Substances 0.000 claims description 9
- 239000000440 bentonite Substances 0.000 claims description 8
- 229910000278 bentonite Inorganic materials 0.000 claims description 8
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000003628 erosive effect Effects 0.000 abstract description 17
- 239000000126 substance Substances 0.000 abstract description 7
- 238000007664 blowing Methods 0.000 abstract description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 239000003513 alkali Substances 0.000 description 11
- 230000035515 penetration Effects 0.000 description 11
- 230000007797 corrosion Effects 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 7
- 238000000576 coating method Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052570 clay Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
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Abstract
The invention relates to a neutron shielding foamed ceramic and a preparation method thereof, wherein zirconia micro powder and alumina micro powder, rare earth element oxide, ammonium polymethacrylate, sodium carboxymethylcellulose, ethanol and water are mixed uniformly to prepare slurry I; mixing gadolinium oxide micropowder, clay, aluminum oxide micropowder, polycarboxylate, sodium carboxyethyl cellulose, ethanol and water uniformly to prepare slurry II; soaking polyurethane sponge in the slurry I, blowing or centrifugally throwing the slurry by adopting compressed air, drying and preserving heat to obtain a foamed ceramic preform; then, carrying out vacuum impregnation on the foamed ceramic preform by using the slurry II, blowing compressed air or centrifugally throwing slurry, and drying; and finally, preserving the heat under certain conditions to obtain the neutron shielding foamed ceramic. The neutron shielding foamed ceramic prepared by the invention has the advantages of small volume density, high strength, excellent chemical erosion resistance and excellent neutron shielding performance.
Description
Technical Field
The invention relates to the technical field of foamed ceramics, in particular to neutron shielding foamed ceramics and a preparation method thereof.
Background
After the twenty-first century, with the rapid development of nuclear industry technology, neutron and neutron source technology is widely applied to industries such as energy, military industry, medical treatment, agriculture and the like. Brings about extremely destructive harm while benefiting the life of people. Neutrons can cause harm to the human body by ionization and excitation due to their strong penetrability. At present, the main radiation shielding materials mainly have the following problems: large mass and volume, low mechanical strength and poor resistance to acid and alkali attack. Therefore, the preparation of high-performance radiation protection materials has become an urgent problem to be solved today.
The foamed ceramic has the following characteristics: high porosity, small volume density, excellent chemical corrosion resistance, high mechanical strength and rigidity, strong thermal shock stability, large specific surface area and the like, and is widely applied to the preparation of high-performance filters, combustor homogenized media, catalyst carriers, heat insulation materials and the like. Meanwhile, the secondary coating process is adopted to treat the foamed ceramic, so that the physical and chemical properties of the foamed ceramic can be effectively improved, and the application range of the foamed ceramic in industry and life can be enlarged.
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 the neutron shielding material and the preparation process (ZL 201210156866) discloses a neutron shielding material prepared by mixing and stirring ultrahigh molecular weight polyethylene, a boron compound, stearic acid or stearate, a heavy metal material, a mildew preventive, a flame retardant and a coupling agent uniformly, heating to 100-200 ℃, putting into a mold, pressing for molding, pressing for cooling and demolding. The method reduces the production cost to a certain extent and improves the neutron shielding efficiency. But its main drawbacks are: (1) the mechanical properties are not high; (2) can not be used under the condition of high temperature; (3) the anti-erosion capability is weak; (4) the bulk density is high.
The patent technology of "a low-density neutron shielding material and a preparation method thereof" (CN 201710022555) discloses a low-density neutron shielding material prepared by mixing, freezing and drying a polymer solution or emulsion, a boron-containing compound and clay. The method reduces the production process and cost to a certain extent, and improves the production efficiency. But its main drawbacks are: (1) the high-temperature stability is weaker; (2) the mechanical strength is not high; (3) the erosion resistance is weak.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a neutron shielding foamed ceramic and a preparation method thereof.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a neutron shielding foamed ceramic is prepared by the following steps:
step one, mixing 35-55 parts by mass of zirconia micro powder and 45-55 parts by mass of alumina micro powder with 3-5 parts by mass of rare earth element oxide to obtain mixed powder I; adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 part by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically milling for 3-5 hours to obtain slurry I;
step two, mixing 15-45 parts by mass of gadolinium oxide micro powder, 20-35 parts by mass of clay and 20-32 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
step three, immersing the pretreated polyurethane sponge into the slurry I, injecting compressed air or centrifugally throwing slurry after impregnation, drying for 6-12 h at 70-110 ℃, heating to 600-850 ℃ at the speed of 1-2 ℃/min, and preserving heat for 0.5-1.5 h to obtain a foamed ceramic preform; then dipping the ceramic preform into the slurry II, vacuumizing until the residual pressure is 100-1500 Pa, maintaining the pressure for 10-30 min, spraying compressed air or centrifugally throwing the slurry, and drying at 80-110 ℃ for 6-24 h to obtain a neutron shielding foamed ceramic blank;
and step four, placing the neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 1350-1750 ℃ at the speed of 2-3 ℃/min in the air atmosphere, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the neutron shielding foamed ceramic.
The average grain diameter of the zirconia micro powder is less than or equal to 1 mu m.
The average grain diameter of the alumina micro powder is less than or equal to 2 mu m.
The rare earth element oxide is one or a mixture of yttrium oxide and samarium oxide, wherein the average grain diameter of the yttrium oxide and the samarium oxide is less than or equal to 5 mu m.
The average particle size of the gadolinium oxide micro powder is less than or equal to 5 mu m.
The clay is one of Fujian mud, bentonite and Suzhou soil, wherein the average grain diameter of the Fujian mud, the bentonite and the Suzhou soil is less than or equal to 20 mu m.
Compared with the prior art, the invention has the beneficial effects that:
firstly, uniformly mixing zirconia micro powder, alumina micro powder, rare earth element oxide, ammonium polymethacrylate, sodium carboxymethylcellulose, ethanol and water to prepare slurry I; mixing gadolinium oxide micropowder, clay, aluminum oxide micropowder, polycarboxylate, sodium carboxyethyl cellulose, ethanol and water uniformly to prepare slurry II; soaking polyurethane sponge in the slurry I, blowing or centrifugally throwing the slurry by adopting compressed air, drying and preserving heat to obtain a foamed ceramic preform; then, carrying out vacuum impregnation on the foamed ceramic preform by using the slurry II, blowing compressed air or centrifugally throwing slurry, and drying; and finally, preserving the heat under certain conditions to obtain the neutron shielding foamed ceramic.
The invention adopts the secondary coating and vacuum impregnation technology, and the shielding material-containing slurry II is coated on the surface of the foam ceramic prefabricated body by the secondary coating and vacuum impregnation technology, so that the slurry can be uniformly coated on the surface of a matrix and the inside of a hollow pore rib, but the surface and the inside of the foam ceramic matrix contain a large amount of shielding material Gd2O3Thereby remarkably improving the neutron shielding performance of the sample. Meanwhile, the defects and the hollow hole ribs of the foamed ceramic, which are generated by the volatilization of the polyurethane sponge, are repaired, so that the mechanical property and the erosion resistance of the foamed ceramic are improved.
Gadolinium oxide, clay and alumina micropowder are selected as main raw materials in the slurry II, the gadolinium oxide has a neutron absorption cross section far larger than that of other materials, so that the gadolinium oxide has extremely strong neutron moderating capability, and gadolinium oxide, alumina and silica react at high temperature to generate Gd2Si2O7And Al5Gd3O12And (3) equaling the ceramic phase. Because the clay contains low-melting phase substances, Gd can be promoted at a lower temperature2Si2O7And Al5Gd3O12When the ceramic phase is generated and the sample is densified, the shielding performance and the mechanical performance of the foamed ceramic are improved.
The neutron shielding foamed ceramic prepared by the invention is detected as follows: the bulk density is 0.3 to 0.6g/cm3(ii) a The normal-temperature compressive strength is 2.7-5.5 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 2.17-5.1 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 10% by adopting a 300mCi Am-Be neutron source.
Therefore, the neutron shielding foamed ceramic prepared by the invention has the advantages of small volume density, high strength, excellent chemical erosion resistance and excellent neutron shielding performance.
Detailed Description
The present invention will be further described with reference to the following specific examples.
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 average grain diameter of the zirconia micro powder is less than or equal to 1 mu m.
The average grain diameter of the alumina micro powder is less than or equal to 2 mu m.
The average grain diameter of the strontium oxide, the yttrium oxide and the samarium oxide is less than or equal to 5 mu m.
The average particle size of the gadolinium oxide micro powder is less than or equal to 5 mu m.
The average grain diameter of the Fujian mud, the bentonite and the Suzhou soil is less than or equal to 20 mu m.
Example 1
A neutron shielding foamed ceramic and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
step one, mixing 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder with 3-5 parts by mass of yttrium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethyl cellulose, 0.1-0.5 part by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically milling for 3-5 hours to obtain slurry I;
step two, mixing 15-25 parts by mass of gadolinium oxide micro powder, 30-35 parts by mass of Fujian mud and 28-32 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
step three, immersing the pretreated polyurethane sponge into the slurry I, injecting compressed air or centrifugally throwing slurry after impregnation, drying for 6-12 h at 70-110 ℃, heating to 600-850 ℃ at the speed of 1-2 ℃/min, and preserving heat for 0.5-1.5 h to obtain a foamed ceramic preform; then dipping the ceramic preform into the slurry II, vacuumizing until the residual pressure is 100-1500 Pa, maintaining the pressure for 10-30 min, spraying compressed air or centrifugally throwing the slurry, and drying at 80-110 ℃ for 6-24 h to obtain a neutron shielding foamed ceramic blank;
and step four, placing the neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 1350-1550 ℃ at the speed of 2-3 ℃/min in the air atmosphere, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the 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 2.7-3.5 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 2.17-3.15 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 10% by adopting a 300mCi Am-Be neutron source.
Example 2
A neutron foamed ceramic 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 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder, adding 1-2 parts by mass of strontium oxide and 2-3 parts by mass of samarium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 parts by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 25-35 parts by mass of gadolinium oxide micro powder, 10-20 parts by mass of Fujian mud, 10-15 parts by mass of bentonite and 24-28 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 2 is detected as follows: the bulk density is 0.31 to 0.43g/cm3(ii) a The normal-temperature compressive strength is 2.9-3.7 MPa; resisting scouring erosion of alkali solution for 15-20 hThe compressive strength of the rear sample is 2.6-3.5 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 5% by adopting a 300mCi Am-Be neutron source.
Example 3
A neutron shielding foamed ceramic 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 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder, adding 1-2 parts by mass of strontium oxide and 1-2 parts by mass of yttrium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 parts by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 35-45 parts by mass of gadolinium oxide micro powder, 20-25 parts by mass of Suzhou soil and 20-24 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 3 is detected as follows: the bulk density is 0.33 to 0.45g/cm3(ii) a The normal-temperature compressive strength is 3.1-4.1 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 2.7-3.8 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 1% by adopting a 300mCi Am-Be neutron source.
Example 4
A neutron shielding foamed ceramic and a preparation method thereof. The preparation method comprises the following steps:
step one, mixing 45-55 parts by mass of zirconia micro powder and 45-50 parts by mass of alumina micro powder with the addition of 3-4.5 parts by mass of samarium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 part by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 15-25 parts by mass of gadolinium oxide micro powder, 30-35 parts by mass of Suzhou soil and 28-32 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
step three, immersing the pretreated polyurethane sponge into the slurry I, injecting compressed air or centrifugally throwing slurry after impregnation, drying for 6-12 h at 70-110 ℃, heating to 600-850 ℃ at the speed of 1-2 ℃/min, and preserving heat for 0.5-1.5 h to obtain a foamed ceramic preform; then dipping the ceramic preform into the slurry II, vacuumizing until the residual pressure is 100-1500 Pa, maintaining the pressure for 10-30 min, spraying compressed air or centrifugally throwing the slurry, and drying at 80-110 ℃ for 6-24 h to obtain a neutron shielding foamed ceramic blank;
and step four, placing the neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 1550-1650 ℃ at the speed of 2-3 ℃/min in the air atmosphere, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the neutron shielding foamed ceramic.
The neutron shielding foamed ceramic prepared in the embodiment 4 is detected as follows: the bulk density is 0.4 to 0.49g/cm3(ii) a The normal-temperature compressive strength is 3.7-4.8 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 3.5-4.6 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 10% by adopting a 300mCi Am-Be neutron source.
Example 5
A neutron shielding foamed ceramic and a preparation method thereof. The preparation method shown in this example is the same as that of example 4 except for the first step and the second step.
Step one, mixing 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder, adding 1-2 parts by mass of strontium oxide and 2-3 parts by mass of yttrium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 parts by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 25-35 parts by mass of gadolinium oxide micro powder, 10-20 parts by mass of Suzhou soil, 10-15 parts by mass of bentonite and 24-28 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 5 is detected as follows: the bulk density is 0.4 to 0.49g/cm3(ii) a The normal-temperature compressive strength is 3.7-4.8 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 3.5-4.6 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 5% by adopting a 300mCi Am-Be neutron source.
Example 6
A neutron shielding foamed ceramic and a preparation method thereof. The preparation method shown in this example is the same as that of example 4 except for the first step and the second step.
Step one, mixing 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder, adding 1-2 parts by mass of samarium oxide and 1-2 parts by mass of yttrium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 parts by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 35-45 parts by mass of gadolinium oxide micro powder, 20-25 parts by mass of Fujian mud and 20-24 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 6 is detected as follows: the bulk density is 0.42 to 0.51g/cm3(ii) a The normal-temperature compressive strength is 3.6-4.5 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 3.2-4.3 MPa; shielding foamed ceramic (thickness of 2 cm) by 300mCi Am-Be neutron source) The penetration rate of thermal neutrons is less than 1 percent when the irradiation is carried out.
Example 7
A neutron shielding foamed ceramic and a preparation method thereof. The preparation method comprises the following steps:
step one, mixing 45-55 parts by mass of zirconia micro powder and 45-50 parts by mass of alumina micro powder with 3-5 parts by mass of strontium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethyl cellulose, 0.1-0.5 part by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically milling for 3-5 hours to obtain slurry I;
step two, mixing 15-25 parts by mass of gadolinium oxide micro powder, 30-35 parts by mass of bentonite and 28-32 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
step three, immersing the pretreated polyurethane sponge into the slurry I, injecting compressed air or centrifugally throwing slurry after impregnation, drying for 6-12 h at 70-110 ℃, heating to 600-850 ℃ at the speed of 1-2 ℃/min, and preserving heat for 0.5-1.5 h to obtain a foamed ceramic preform; then dipping the ceramic preform into the slurry II, vacuumizing until the residual pressure is 100-1500 Pa, maintaining the pressure for 10-30 min, spraying compressed air or centrifugally throwing the slurry, and drying at 80-110 ℃ for 6-24 h to obtain a neutron shielding foamed ceramic blank;
and step four, placing the neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 1650-1750 ℃ at the speed of 2-3 ℃/min in the air atmosphere, preserving the heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the neutron shielding foamed ceramic.
The neutron shielding foamed ceramic prepared in the embodiment 7 is detected as follows: the bulk density is 0.45-0.52 g/cm3(ii) a The normal-temperature compressive strength is 4.3-4.9 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 3.2-4.3 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 10% by adopting a 300mCi Am-Be neutron source.
Example 8
A neutron shielding foamed ceramic and a preparation method thereof. The preparation process shown in this example is the same as that of example 7 except for the first and second steps.
Step one, mixing 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder, adding 1-2 parts by mass of strontium oxide and 2-3 parts by mass of samarium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 parts by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 25-35 parts by mass of gadolinium oxide micro powder, 10-20 parts by mass of Suzhou soil, 10-15 parts by mass of Fujian mud and 24-28 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 7 is detected as follows: the bulk density is 0.49-0.57 g/cm3(ii) a The normal-temperature compressive strength is 4.5-5.2 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 4.2-4.9 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 5% by adopting a 300mCi Am-Be neutron source.
Example 9
A neutron shielding foamed ceramic and a preparation method thereof. The preparation process shown in this example is the same as that of example 7 except for the first and second steps.
Step one, mixing 35-45 parts by mass of zirconia micro powder and 50-55 parts by mass of alumina micro powder, adding 1-2 parts by mass of strontium oxide and 1-2 parts by mass of yttrium oxide to obtain mixed powder I, adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 parts by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically ball-milling for 3-5 hours to obtain slurry I;
step two, mixing 35-45 parts by mass of gadolinium oxide micro powder, 20-25 parts by mass of Fujian mud and 20-24 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
the neutron shielding foamed ceramic prepared in the embodiment 9 is detected as follows: the bulk density is 0.51 to 0.6g/cm3(ii) a The normal-temperature compressive strength is 4.7-5.5 MPa; the compressive strength of the sample after 15-20 h of erosion and corrosion of the alkali-resistant solution is 4.6-5.2 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 1% by adopting a 300mCi Am-Be neutron source.
The invention adopts secondary coating and vacuum impregnation technology. Coating the slurry II containing the shielding material on the surface of the foam ceramic prefabricated part by secondary coating and vacuum impregnation technology, so that the slurry can be uniformly coated on the surface of the matrix and the inside of the hollow pore ribs, but the surface and the inside of the foam ceramic matrix contain a large amount of Gd shielding material2O3Thereby remarkably improving the neutron shielding performance of the sample. Meanwhile, the defects and the hollow hole ribs of the foamed ceramic, which are generated by the volatilization of the polyurethane sponge, are repaired, so that the mechanical property and the erosion resistance of the foamed ceramic are improved.
Gadolinium oxide, clay and alumina micropowder are selected as main raw materials in the slurry II, the gadolinium oxide has a neutron absorption cross section far larger than that of other materials, so that the gadolinium oxide has extremely strong neutron moderating capability, and gadolinium oxide, alumina and silica react at high temperature to generate Gd2Si2O7And Al5Gd3O12And (3) equaling the ceramic phase. Because the clay contains low-melting phase substances, Gd can be promoted at a lower temperature2Si2O7And Al5Gd3O12When the ceramic phase is generated and the sample is densified, the shielding performance and the mechanical performance of the foamed ceramic are improved.
The neutron shielding foamed ceramic prepared by the invention is detected as follows: the bulk density is 0.3 to 0.6g/cm3(ii) a The normal-temperature compressive strength is 2.7-5.5 MPa; resistance to erosion by alkaline solution 1After 5-20 h, the compressive strength of the sample is 2.17-5.1 MPa; the penetration rate of thermal neutrons of the shielding foamed ceramics (the thickness is 2 cm) is less than 10% by adopting a 300mCi Am-Be neutron source.
Therefore, the neutron shielding foamed ceramic prepared by the invention has the advantages of small volume density, high strength, 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 (6)
1. A neutron shielding ceramic foam, characterized in that: the preparation steps are as follows:
step one, mixing 35-55 parts by mass of zirconia micro powder and 45-55 parts by mass of alumina micro powder with 3-5 parts by mass of rare earth element oxide to obtain mixed powder I; adding 0.5-2.0 parts by mass of ammonium polymethacrylate, 0.2-1.6 parts by mass of sodium carboxymethylcellulose, 0.1-0.5 part by mass of ethanol and 20-46 parts by mass of water into the mixed powder I, and mechanically milling for 3-5 hours to obtain slurry I;
step two, mixing 15-45 parts by mass of gadolinium oxide micro powder, 20-35 parts by mass of clay and 20-32 parts by mass of alumina micro powder to obtain mixed powder II; adding 0.2-1.7 parts by mass of polycarboxylate, 0.1-0.7 part by mass of sodium carboxyethyl cellulose, 0.1-0.7 part by mass of ethanol and 25-52 parts by mass of water into the mixed powder II, and mechanically milling for 1-3 hours to obtain slurry II;
step three, immersing the pretreated polyurethane sponge into the slurry I, injecting compressed air or centrifugally throwing slurry after impregnation, drying for 6-12 h at 70-110 ℃, heating to 600-850 ℃ at the speed of 1-2 ℃/min, and preserving heat for 0.5-1.5 h to obtain a foamed ceramic preform; then dipping the ceramic preform into the slurry II, vacuumizing until the residual pressure is 100-1500 Pa, maintaining the pressure for 10-30 min, spraying compressed air or centrifugally throwing the slurry, and drying at 80-110 ℃ for 6-24 h to obtain a neutron shielding foamed ceramic blank;
and step four, placing the neutron shielding foamed ceramic blank into a high-temperature furnace, heating to 1350-1750 ℃ at the speed of 2-3 ℃/min in the air atmosphere, preserving heat for 2-5 h, and cooling to room temperature along with the furnace to obtain the neutron shielding foamed ceramic.
2. The neutron shielding ceramic foam of claim 1, wherein: the average grain diameter of the zirconia micro powder is less than or equal to 1 mu m.
3. The neutron shielding ceramic foam of claim 1, wherein: the average grain diameter of the alumina micro powder is less than or equal to 2 mu m.
4. The neutron shielding ceramic foam of claim 1, wherein: the rare earth element oxide is one or a mixture of yttrium oxide and samarium oxide, wherein the average grain diameter of the yttrium oxide and the samarium oxide is less than or equal to 5 mu m.
5. The neutron shielding ceramic foam of claim 1, wherein: the average particle size of the gadolinium oxide micro powder is less than or equal to 5 mu m.
6. The neutron shielding ceramic foam of claim 1, wherein: the clay is one of Fujian mud, bentonite and Suzhou soil, wherein the average grain diameter of the Fujian mud, the bentonite and the Suzhou soil is less than or equal to 20 mu m.
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-
2018
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