CN108409307A - A kind of neutron shield foamed ceramics and preparation method thereof - Google Patents

A kind of neutron shield foamed ceramics and preparation method thereof Download PDF

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CN108409307A
CN108409307A CN201810257493.5A CN201810257493A CN108409307A CN 108409307 A CN108409307 A CN 108409307A CN 201810257493 A CN201810257493 A CN 201810257493A CN 108409307 A CN108409307 A CN 108409307A
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quality
foamed ceramics
parts
slurry
neutron shield
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CN108409307B (en
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贾文宝
陈若愚
金利民
汪瑜凡
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 present invention relates to a kind of neutron shield foamed ceramicses and preparation method thereof, and first by zirconium oxide micro mist and alumina powder, rare earth oxide, ammonium polymethacrylate, sodium carboxymethylcellulose, second alcohol and water mixing, slurry I is made；By gadolinium oxide micro mist, clay, alumina powder, polycarboxylate, sodium hydroxyethlcellulose, second alcohol and water mixing, slurry II is made；Polyurethane sponge is impregnated in slurry I, is starched using compressed air spraying or centrifugal drying, dry, heat preservation obtains foamed ceramics precast body；Then vacuum impregnation, compressed air spraying or centrifugal drying slurry are carried out to foamed ceramics precast body with slurry II, it is dry；Finally kept the temperature under certain condition to get neutron shield foamed ceramics.The chemerosiveness resistent and neutron shield performance that the bulk density of neutron shield foamed ceramics prepared by the present invention is small, intensity is high, excellent.

Description

A kind of neutron shield foamed ceramics and preparation method thereof
Technical field
The present invention relates to foamed ceramics technical fields, and in particular to a kind of neutron shield foamed ceramics and preparation method thereof.
Background technology
Into after 21st century, with the fast development of nuclear industry technology, neutron and neutron source technology are widely used In the industries such as the energy, military project, medical treatment and agricultural.While benefiting people's life, the harm of very disruptive is also brought. Neutron to human body by ionizing and exciting with very strong penetrability due to that can generate harm.Currently, main radiation shield material Material is primarily present problems with：Quality and volume is larger, mechanical strength is not high and antiacid alkali erosiveness is poor.Therefore, it prepares high The radiation protection material of performance has become current urgent problem to be solved.
Foamed ceramics is due to following characteristic：High porosity, bulk density are small, resistant to chemical etching excellent, mechanical strong It spends and is widely used in the advantages that rigidity height, stronger thermal shock resistance and large specific surface area and prepares high-performance filtration Device, burner homogenize medium, catalyst carrier and heat-barrier material etc..At the same time, it is made pottery to foam using secondary coating processes Porcelain, which carries out processing, can effectively promote the physicochemical property of foamed ceramics and expand its use scope in industry and life.
Technical staff is to conduct in-depth research and technological development the problems such as preparing high-performance radiation-shielding material at present：
The patented technology of " neutron shielding material and preparation process " (ZL201210156866) discloses a kind of with superelevation point Sub- weight northylen, boron compound, stearic acid or stearate, heavy metal material, mould inhibitor, fire retardant, coupling agent are kneaded stirring Uniformly, it by being heated to 100~200 DEG C, is placed in mold, is press-formed, pressurization is cooling, demoulding prepares neutron shielding material. This method reduces production cost and improves neutron shield efficiency to a certain extent.But its major defect is：(1) mechanicalness It can not be high；(2) it can not use under hot conditions again；(3) corrosion resistance is weaker；(4) bulk density is larger.
The patented technology of " a kind of low-density neutron shielding material and preparation method thereof " (CN201710022555), discloses One kind is dried through mixed freezing with polymer solution or lotion, boron-containing compound and clay and prepares low-density neutron shielding material. This method reduces production technology and cost to a certain extent, and improves production efficiency.But its major defect is：(1) High-temperature stability is weaker；(2) mechanical strength is not high；(3) corrosion resistance is weak.
Invention content
The present invention is directed to overcome prior art defect, it is therefore an objective to provide a kind of neutron shield foamed ceramics and its preparation side Method, with the corrosion resistance and neutron shield that the neutron shield foamed ceramics volume density of this method preparation is small, intensity is high, excellent Energy.
To achieve the above object, technical solution provided by the invention is：
A kind of neutron shield foamed ceramics, preparation process are as follows：
Step 1: by the alumina powder of the zirconium oxide micro mist and 45~55 parts of quality of 35~55 parts of quality, additional 3~5 The rare earth oxide mixing of part quality, obtains mixed powder I；The poly- methyl of 0.5~2.0 part of quality is added into mixed powder I again Ammonium acrylate, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, the ethyl alcohol of 0.1~0.5 part of quality and 20~46 parts of quality Slurry I is made in water, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 15~45 parts of quality, the oxygen of the clay of 20~35 parts of quality, 20~32 parts of quality Change the mixing of aluminium micro mist, obtains mixed powder II；Again into mixed powder II be added 0.2~1.7 part of quality polycarboxylate, 0.1~0.7 part The sodium hydroxyethlcellulose of quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, system Obtain slurry II；
Step 3: pretreated polyurethane sponge is immersed in slurry I, compressed air spraying or centrifugal drying after dipping Slurry is warming up to 600~850 DEG C in 70~110 DEG C of dry 6~12h, then with the rate of 1~2 DEG C/min, keeps the temperature 0.5~1.5h, Obtain foamed ceramics precast body；Then ceramics preparative body is impregnated into slurry II, be evacuated to residual compression be 100~ 10~30min of pressurize when 1500Pa, compressed air sprays or centrifugal drying slurry, and 80~110 DEG C of dryings 6~for 24 hours, obtain neutron screen Cover foamed ceramics green body；
Step 4: by the neutron shield foamed ceramics green body merging high temperature furnace, under air atmosphere, with 2~3 DEG C/speed of min rises to 1350~1750 DEG C, keeps the temperature 2~5h, room temperature is cooled to the furnace to get to neutron shield foamed ceramics.
Average grain diameter≤1 μm of the zirconium oxide micro mist.
Average grain diameter≤2 μm of the alumina powder.
The rare earth oxide is one or more mixing in strontium oxide strontia, yttrium oxide or samarium oxide, wherein Strontium oxide strontia, yttrium oxide and samarium oxide average grain diameter≤5 μm.
Average grain diameter≤5 μm of the gadolinium oxide micro mist.
The clay is one kind in Fujian mud, bentonite and Suzhou soil, and wherein Fujian mud, bentonite and Suzhou soil is flat Equal grain size≤20 μm.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is first by zirconium oxide micro mist and alumina powder, rare earth oxide, ammonium polymethacrylate, carboxymethyl Slurry I is made in sodium cellulosate, second alcohol and water mixing；By gadolinium oxide micro mist, clay, alumina powder, polycarboxylate, carboxyethyl Slurry II is made in sodium cellulosate, second alcohol and water mixing；Polyurethane sponge is impregnated in slurry I, using compressed air spraying or Person's centrifugal drying is starched, dry, and heat preservation obtains foamed ceramics precast body；Then vacuum is carried out to foamed ceramics precast body with slurry II Dipping, compressed air spraying or centrifugal drying slurry, it is dry；Finally kept the temperature under certain condition to get neutron shield foamed ceramics.
The present invention uses secondary coating and Vacuum infusion techniques, will contain shielding by secondary coating and Vacuum infusion techniques Material paste II is coated to foamed ceramics precast body surface, and slurry can be made to be evenly coated in inside matrix surface and hollow hole muscle, But a large amount of shielding material Gd is contained in foamed ceramics matrix surface and inside2O3And then it is obviously improved the neutron shield of sample Energy.At the same time, foamed ceramics hole muscle is repaired because of defect and hollow hole muscle caused by polyurethane sponge volatilization, is improved The mechanical performance and erosion-resisting characteristics of foamed ceramics.
It is primary raw material that gadolinium oxide, clay and alumina powder are selected in slurry II, mainly due in gadolinium oxide Sub- absorption cross-section is much larger than other materials and then has extremely strong moderation of neutrons ability, and gadolinium oxide and aluminium oxide and dioxy SiClx is reacted at high temperature generates Gd2Si2O7And Al5Gd3O12Equal ceramic phases.Due to containing eutectic phase substance in clay, It can promote Gd at a lower temperature2Si2O7And Al5Gd3O12Equal ceramic phases generate and sample densification, improve foamed ceramics Shielding properties and mechanical performance.
Neutron shield foamed ceramics prepared by the present invention, after testing：Bulk density is 0.3~0.6g/cm3；Room temperature pressure resistance Intensity is 2.7~5.5MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 2.17~5.1MPa；Using 300mCi Am-Be neutron sources carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and are less than 10%.
Therefore, the resistance to chemical attack that the bulk density of the neutron shield foamed ceramics that prepared by the present invention is small, intensity is high, excellent Property and neutron shield performance.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
To avoid repeating, the technical parameter Unify legislation to be first related to present embodiment is as follows, in embodiment It will not repeat：
Average grain diameter≤1 μm of the zirconium oxide micro mist.
Average grain diameter≤2 μm of the alumina powder.
The strontium oxide strontia, yttrium oxide and samarium oxide average grain diameter≤5 μm.
Average grain diameter≤5 μm of the gadolinium oxide micro mist.
The Fujian mud, bentonite and Suzhou soil average grain diameter≤20 μm.
Embodiment 1
A kind of the step of neutron shield foamed ceramics and preparation method thereof, the preparation method is：
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 3~5 The yttrium oxide mixing of part quality, obtains mixed powder I, then be added into mixed powder I 0.5~2.0 part of quality ammonium polymethacrylate, The sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality ethyl alcohol and 20~46 parts of quality water, mechanical ball 3~5h is ground, slurry I is made；
Step 2: by the gadolinium oxide micro mist of 15~25 parts of quality, the Fujian mud of 30~35 parts of quality, 28~32 parts of quality Alumina powder mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 into mixed powder II again The sodium hydroxyethlcellulose of part quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, Slurry II is made；
Step 3: pretreated polyurethane sponge is immersed in slurry I, compressed air spraying or centrifugal drying after dipping Slurry is warming up to 600~850 DEG C in 70~110 DEG C of dry 6~12h, then with the rate of 1~2 DEG C/min, keeps the temperature 0.5~1.5h, Obtain foamed ceramics precast body；Then ceramics preparative body is impregnated into slurry II, be evacuated to residual compression be 100~ 10~30min of pressurize when 1500Pa, compressed air sprays or centrifugal drying slurry, and 80~110 DEG C of dryings 6~for 24 hours, obtain neutron screen Cover foamed ceramics green body；
Step 4: by the neutron shield foamed ceramics green body merging high temperature furnace, under air atmosphere, with 2~3 DEG C/speed of min rises to 1350~1550 DEG C, 2~5h is kept the temperature, is made pottery to get to neutron shield foam cooling to room temperature with the furnace Porcelain.
Neutron shield foamed ceramics prepared by the present embodiment 1, after testing：Bulk density is 0.3~0.42g/cm3；Often Warm compressive resistance is 2.7~3.5MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 2.17~ 3.15MPa；300mCi Am-Be neutron sources are used to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) small In 10%.
Embodiment 2
A kind of neutron foamed ceramics and preparation method thereof.Preparation method shown in the present embodiment in addition to step 1 and step 2, Remaining is same
Embodiment 1.
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 1~2 The strontium oxide strontia of part quality and the samarium oxide mixing of 2~3 parts of quality, obtain mixed powder I, then 0.5~2.0 part is added into mixed powder I The ethyl alcohol and 20 of the ammonium polymethacrylate of quality, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality Slurry I is made in the water of~46 parts of quality, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 25~35 parts of quality, the Fujian mud of 10~20 parts of quality, 10~15 parts of quality The alumina powder mixing of bentonite, 24~28 parts of quality, obtains mixed powder II；0.2~1.7 part of matter is added into mixed powder II again The ethyl alcohol and 25~52 parts of matter of the polycarboxylate of amount, the sodium hydroxyethlcellulose of 0.1~0.7 part of quality, 0.1~0.7 part of quality Slurry II is made in the water of amount, 1~3h of mechanical ball mill；
Neutron shield foamed ceramics prepared by the present embodiment 2, after testing：Bulk density is 0.31~0.43g/cm3；Often Warm compressive resistance is 2.9~3.7MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 2.6~3.5MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 5%.
Embodiment 3
A kind of neutron shield foamed ceramics and preparation method thereof.Preparation method shown in the present embodiment removes step 1 and step 2 Outside, remaining is the same as embodiment 1.
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 1~2 The strontium oxide strontia of part quality and the yttrium oxide mixing of 1~2 part of quality, obtain mixed powder I, then 0.5~2.0 part is added into mixed powder I The ethyl alcohol and 20 of the ammonium polymethacrylate of quality, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality Slurry I is made in the water of~46 parts of quality, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 35~45 parts of quality, the Suzhou soil of 20~25 parts of quality, 20~24 parts of quality Alumina powder mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 into mixed powder II again The sodium hydroxyethlcellulose of part quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, Slurry II is made；
Neutron shield foamed ceramics prepared by the present embodiment 3, after testing：Bulk density is 0.33~0.45g/cm3；Often Warm compressive resistance is 3.1~4.1MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 2.7~3.8MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 1%.
Embodiment 4
A kind of neutron shield foamed ceramics and preparation method thereof.The step of preparation method is：
Step 1: by the alumina powder of the zirconium oxide micro mist and 45~50 parts of quality of 45~55 parts of quality, additional 3~ The samarium oxide mixing of 4.5 parts of quality, obtains mixed powder I, then the polymethylacrylic acid of 0.5~2.0 part of quality is added into mixed powder I Ammonium, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality ethyl alcohol and 20~46 parts of quality water, machinery Slurry I is made in 3~5h of ball milling；
Step 2: by the gadolinium oxide micro mist of 15~25 parts of quality, the Suzhou soil of 30~35 parts of quality, 28~32 parts of quality Alumina powder mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 into mixed powder II again The sodium hydroxyethlcellulose of part quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, Slurry II is made；
Step 3: pretreated polyurethane sponge is immersed in slurry I, compressed air spraying or centrifugal drying after dipping Slurry is warming up to 600~850 DEG C in 70~110 DEG C of dry 6~12h, then with the rate of 1~2 DEG C/min, keeps the temperature 0.5~1.5h, Obtain foamed ceramics precast body；Then ceramics preparative body is impregnated into slurry II, be evacuated to residual compression be 100~ 10~30min of pressurize when 1500Pa, compressed air sprays or centrifugal drying slurry, and 80~110 DEG C of dryings 6~for 24 hours, obtain neutron screen Cover foamed ceramics green body；
Step 4: by the neutron shield foamed ceramics green body merging high temperature furnace, under air atmosphere, with 2~3 DEG C/speed of min rises to 1550~1650 DEG C, 2~5h is kept the temperature, is made pottery to get to neutron shield foam cooling to room temperature with the furnace Porcelain.
Neutron shield foamed ceramics prepared by the present embodiment 4, after testing：Bulk density is 0.4~0.49g/cm3；Often Warm compressive resistance is 3.7~4.8MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 3.5~4.6MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 10%.
Embodiment 5
A kind of neutron shield foamed ceramics and preparation method thereof.Preparation method shown in the present embodiment removes step 1 and step 2 Outside, remaining is the same as embodiment 4.
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 1~2 The strontium oxide strontia of part quality and the yttrium oxide mixing of 2~3 parts of quality, obtain mixed powder I, then 0.5~2.0 part is added into mixed powder I The ethyl alcohol and 20 of the ammonium polymethacrylate of quality, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality Slurry I is made in the water of~46 parts of quality, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 25~35 parts of quality, the Suzhou soil of 10~20 parts of quality, 10~15 parts of quality The alumina powder mixing of bentonite, 24~28 parts of quality, obtains mixed powder II；0.2~1.7 part of matter is added into mixed powder II again The ethyl alcohol and 25~52 parts of matter of the polycarboxylate of amount, the sodium hydroxyethlcellulose of 0.1~0.7 part of quality, 0.1~0.7 part of quality Slurry II is made in the water of amount, 1~3h of mechanical ball mill；
Neutron shield foamed ceramics prepared by the present embodiment 5, after testing：Bulk density is 0.4~0.49g/cm3；Often Warm compressive resistance is 3.7~4.8MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 3.5~4.6MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 5%.
Embodiment 6
A kind of neutron shield foamed ceramics and preparation method thereof.Preparation method shown in the present embodiment removes step 1 and step 2 Outside, remaining is the same as embodiment 4.
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 1~2 The samarium oxide of part quality and the yttrium oxide mixing of 1~2 part of quality, obtain mixed powder I, then 0.5~2.0 part is added into mixed powder I The ethyl alcohol and 20 of the ammonium polymethacrylate of quality, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality Slurry I is made in the water of~46 parts of quality, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 35~45 parts of quality, the Fujian mud of 20~25 parts of quality, 20~24 parts of quality Alumina powder mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 into mixed powder II again The sodium hydroxyethlcellulose of part quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, Slurry II is made；
Neutron shield foamed ceramics prepared by the present embodiment 6, after testing：Bulk density is 0.42~0.51g/cm3；Often Warm compressive resistance is 3.6~4.5MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 3.2~4.3MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 1%.
Embodiment 7
A kind of neutron shield foamed ceramics and preparation method thereof.The step of preparation method is：
Step 1: by the alumina powder of the zirconium oxide micro mist and 45~50 parts of quality of 45~55 parts of quality, additional 3~5 The strontium oxide strontia mixing of part quality, obtains mixed powder I, then be added into mixed powder I 0.5~2.0 part of quality ammonium polymethacrylate, The sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality ethyl alcohol and 20~46 parts of quality water, mechanical ball 3~5h is ground, slurry I is made；
Step 2: by the gadolinium oxide micro mist of 15~25 parts of quality, the bentonite of 30~35 parts of quality, 28~32 parts of quality Alumina powder mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 into mixed powder II again The sodium hydroxyethlcellulose of part quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, Slurry II is made；
Step 3: pretreated polyurethane sponge is immersed in slurry I, compressed air spraying or centrifugal drying after dipping Slurry is warming up to 600~850 DEG C in 70~110 DEG C of dry 6~12h, then with the rate of 1~2 DEG C/min, keeps the temperature 0.5~1.5h, Obtain foamed ceramics precast body；Then ceramics preparative body is impregnated into slurry II, be evacuated to residual compression be 100~ 10~30min of pressurize when 1500Pa, compressed air sprays or centrifugal drying slurry, and 80~110 DEG C of dryings 6~for 24 hours, obtain neutron screen Cover foamed ceramics green body；
Step 4: by the neutron shield foamed ceramics green body merging high temperature furnace, under air atmosphere, with 2~3 DEG C/speed of min rises to 1650~1750 DEG C, 2~5h is kept the temperature, is made pottery to get to neutron shield foam cooling to room temperature with the furnace Porcelain.
Neutron shield foamed ceramics prepared by the present embodiment 7, after testing：Bulk density is 0.45~0.52g/cm3；Often Warm compressive resistance is 4.3~4.9MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 3.2~4.3MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 10%.
Embodiment 8
A kind of neutron shield foamed ceramics and preparation method thereof.Preparation method shown in the present embodiment removes step 1 and step 2 Outside, remaining is the same as embodiment 7.
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 1~2 The strontium oxide strontia of part quality and the samarium oxide mixing of 2~3 parts of quality, obtain mixed powder I, then 0.5~2.0 part is added into mixed powder I The ethyl alcohol and 20 of the ammonium polymethacrylate of quality, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality Slurry I is made in the water of~46 parts of quality, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 25~35 parts of quality, the Suzhou soil of 10~20 parts of quality, 10~15 parts of quality The alumina powder mixing of Fujian mud, 24~28 parts of quality, obtains mixed powder II；0.2~1.7 part of matter is added into mixed powder II again The ethyl alcohol and 25~52 parts of matter of the polycarboxylate of amount, the sodium hydroxyethlcellulose of 0.1~0.7 part of quality, 0.1~0.7 part of quality Slurry II is made in the water of amount, 1~3h of mechanical ball mill；
Neutron shield foamed ceramics prepared by the present embodiment 7, after testing：Bulk density is 0.49~0.57g/cm3；Often Warm compressive resistance is 4.5~5.2MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 4.2~4.9MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 5%.
Embodiment 9
A kind of neutron shield foamed ceramics and preparation method thereof.Preparation method shown in the present embodiment removes step 1 and step 2 Outside, remaining is the same as embodiment 7.
Step 1: by the alumina powder of the zirconium oxide micro mist and 50~55 parts of quality of 35~45 parts of quality, additional 1~2 The strontium oxide strontia of part quality and the yttrium oxide mixing of 1~2 part of quality, obtain mixed powder I, then 0.5~2.0 part is added into mixed powder I The ethyl alcohol and 20 of the ammonium polymethacrylate of quality, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality Slurry I is made in the water of~46 parts of quality, 3~5h of mechanical ball mill；
Step 2: by the gadolinium oxide micro mist of 35~45 parts of quality, the Fujian mud of 20~25 parts of quality, 20~24 parts of quality Alumina powder mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 into mixed powder II again The sodium hydroxyethlcellulose of part quality, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, 1~3h of mechanical ball mill, Slurry II is made；
Neutron shield foamed ceramics prepared by the present embodiment 9, after testing：Bulk density is 0.51~0.6g/cm3；Often Warm compressive resistance is 4.7~5.5MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 4.6~5.2MPa； It uses 300mCi Am-Be neutron sources to carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and is less than 1%.
The present invention uses secondary coating and Vacuum infusion techniques.It will contain shielding by secondary coating and Vacuum infusion techniques Material paste II is coated to foamed ceramics precast body surface, and slurry can be made to be evenly coated in inside matrix surface and hollow hole muscle, But a large amount of shielding material Gd is contained in foamed ceramics matrix surface and inside2O3And then it is obviously improved the neutron shield of sample Energy.At the same time, foamed ceramics hole muscle is repaired because of defect and hollow hole muscle caused by polyurethane sponge volatilization, is improved The mechanical performance and erosion-resisting characteristics of foamed ceramics.
It is primary raw material that gadolinium oxide, clay and alumina powder are selected in slurry II, mainly due in gadolinium oxide Sub- absorption cross-section is much larger than other materials and then has extremely strong moderation of neutrons ability, and gadolinium oxide and aluminium oxide and dioxy SiClx is reacted at high temperature generates Gd2Si2O7And Al5Gd3O12Equal ceramic phases.Due to containing eutectic phase substance in clay, It can promote Gd at a lower temperature2Si2O7And Al5Gd3O12Equal ceramic phases generate and sample densification, improve foamed ceramics Shielding properties and mechanical performance.
Neutron shield foamed ceramics prepared by the present invention, after testing：Bulk density is 0.3~0.6g/cm3；Room temperature pressure resistance Intensity is 2.7~5.5MPa；The compressive resistance that alkali resistant solution washes away sample after 15~20h of erosion is 2.17~5.1MPa；Using 300mCi Am-Be neutron sources carry out irradiation thermal neutron penetrance to shielding foamed ceramics (thickness 2cm) and are less than 10%.
Therefore, the resistance to chemical attack that the bulk density of the neutron shield foamed ceramics that prepared by the present invention is small, intensity is high, excellent Property and neutron shield performance.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to above real Apply any simple modification, equivalent replacement and improvement etc. made by example, still fall within technical solution of the present invention protection domain it It is interior.

Claims (6)

1. a kind of neutron shield foamed ceramics, it is characterised in that：Preparation process is as follows：
Step 1: by the alumina powder of the zirconium oxide micro mist and 45~55 parts of quality of 35~55 parts of quality, additional 3~5 parts of matter The rare earth oxide of amount mixes, and obtains mixed powder I；The polymethyl of 0.5~2.0 part of quality is added into mixed powder I again Sour ammonium, the sodium carboxymethylcellulose of 0.2~1.6 part of quality, 0.1~0.5 part of quality ethyl alcohol and 20~46 parts of quality water, machine Slurry I is made in tool 3~5h of ball milling；
Step 2: by the gadolinium oxide micro mist of 15~45 parts of quality, the aluminium oxide of the clay of 20~35 parts of quality, 20~32 parts of quality Micro mist mixes, and obtains mixed powder II；The polycarboxylate of 0.2~1.7 part of quality of addition, 0.1~0.7 part of quality into mixed powder II again Sodium hydroxyethlcellulose, 0.1~0.7 part of quality ethyl alcohol and 25~52 parts of quality water, slurry is made in 1~3h of mechanical ball mill Body II；
Step 3: pretreated polyurethane sponge is immersed in slurry I, compressed air spraying or centrifugal drying slurry after dipping, 70~110 DEG C of dry 6~12h, then 600~850 DEG C are warming up to the rate of 1~2 DEG C/min, 0.5~1.5h is kept the temperature, is steeped Foam ceramics preparative body；Then ceramics preparative body is impregnated into slurry II, is evacuated to when residual compression is 100~1500Pa and protects 10~30min is pressed, compressed air sprays or centrifugal drying slurry, 80~110 DEG C of dryings 6~for 24 hours, obtain neutron shield foamed ceramics Green body；
Step 4: by the neutron shield foamed ceramics green body merging high temperature furnace, under air atmosphere, with 2~3 DEG C/min Speed rise to 1350~1750 DEG C, keep the temperature 2~5h, cool to room temperature with the furnace to get to neutron shield foamed ceramics.
2. neutron shield foamed ceramics according to claim 1, it is characterised in that：The average grain of the zirconium oxide micro mist Diameter≤1 μm.
3. neutron shield foamed ceramics according to claim 1, it is characterised in that：The average grain of the alumina powder Diameter≤2 μm.
4. neutron shield foamed ceramics according to claim 1, it is characterised in that：The rare earth oxide is oxygen Change one or more mixing in strontium, yttrium oxide or samarium oxide, wherein the μ of strontium oxide strontia, yttrium oxide and samarium oxide average grain diameter≤5 m。
5. neutron shield foamed ceramics according to claim 1, it is characterised in that：The average grain of the gadolinium oxide micro mist Diameter≤5 μm.
6. neutron shield foamed ceramics according to claim 1, it is characterised in that：The clay is Fujian mud, swelling One kind in soil and Suzhou soil, wherein Fujian mud, bentonite and Suzhou soil average grain diameter≤20 μm.
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