CN115215666A - Boron nitride/high-entropy ceramic oxide and composite coating for shielding neutrons and gamma rays and preparation method thereof - Google Patents
Boron nitride/high-entropy ceramic oxide and composite coating for shielding neutrons and gamma rays and preparation method thereof Download PDFInfo
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention discloses a boron nitride/high-entropy ceramic oxide and a composite coating for shielding neutrons and gamma rays and a preparation method thereof, belonging to the field of radiation protection. The invention aims to solve the problem that a single material is difficult to realize the simultaneous shielding of neutrons and gamma rays. A of the present invention 2 B 2 O 7 In the type high-entropy ceramic powder, the element A is composed of five or more than five elements of Gd, er, sm, la, ce, eu and Dy, and the element B is Hf; the surface of the high-entropy ceramic powder is wrapped with boron nitride to form a composite filler, and the composite filler and resin are formedAnd (4) composite coating. The invention is applied to the fields of spacecrafts, radioactive medical treatment, nuclear reactors and the like.
Description
Technical Field
The invention belongs to the field of radiation protection, in particular to a 2 B 2 O 7 The boron nitride/high-entropy ceramic oxide composite coating is used for shielding neutrons and gamma rays. Can be applied to the fields of spacecrafts, radioactive medical treatment, nuclear reactors and the like, and has very wide application prospect.
Background
With the continuous development of nuclear science and technology, nuclear radiation sources and facilities are widely applied to the fields of nuclear energy, industry, medicine, particle accelerators and the like, and great convenience is provided for the work and life of people. However, while the radiation source and facilities benefit mankind, the possible leakage of radiation can cause serious health effects, such as skin burns, cardiovascular diseases, cancer, etc. It is therefore necessary to take certain radiation protection measures in order to safely benefit from nuclear radiation, of which neutrons and gamma rays are the most widely used among the various nuclear rays. Meanwhile, the method is also a hotspot and a difficulty in protection research.
The neutron is an uncharged particle, almost does not interact with electrons outside the atomic nucleus when passing through a substance, mainly interacts with the atomic nucleus, and has strong penetrating power to cause more damage to human bodies than other rays with the same dose. The shielding effect on neutrons is actually fast neutron moderation and slow neutron absorption, and gamma and matter interaction mainly adopts photoelectric effect, compton scattering and electron pair effect. The shielding of high-energy neutrons is realized by selecting medium-heavy metal materials, enabling neutrons to be rapidly reduced to be below inelastic scattering threshold energy through inelastic scattering energy, and then further moderating the neutrons through elastic scattering, wherein the lower the atomic number of the material is, the easier the neutrons are moderated through elastic scattering (such as hydrogen, lithium, boron and the like), and when slow neutrons are absorbed, the absorption material is required to have a larger neutron absorption cross section, and the lower the energy of secondary gamma rays emitted is, the better the neutrons are. In recent years, some rare earth elements such as samarium (Sm), europium (Eu), gadolinium (Gd), and the like become novel neutron absorbers because of having a thermal neutron absorption section higher than that of boron and cadmium, and the high atomic number elements also have a function of attenuating gamma rays; however, the energy of the secondary gamma-ray emitted by gadolinium, samarium, europium, dysprosium and the like through inelastic scattering moderation fast neutrons or radiation capture absorption thermal neutrons is high, and the energy of the secondary gamma-ray emitted by boron through a reaction generated by the absorption of thermal neutrons is lower, so that rare earth elements have stronger secondary radioactivity than boron. Heavy metals such as lead, tungsten, bismuth and hafnium are commonly used gamma-ray shielding materials, but the heavy metals have weak absorption edges, the K layer absorption edge of the rare earth element is just fallen on the area, the rare earth element and the heavy metals are blended and combined to make up the weak absorption area, so the process of shielding neutrons and gamma rays is a process of mutually assisting and mutually matching high atomic number elements and low atomic number elements.
In 2015, rost et al used metal oxides as raw materials to synthesize high-entropy oxides for the first time, and defined a novel multi-element ceramic material formed by mutually solid-dissolving more than or equal to 5 kinds of cations or anions in equal proportion or nearly equal proportion as high-entropy ceramic. Has the characteristics which are not possessed by the traditional ceramics, namely high entropy effect, lattice distortion effect, delayed diffusion effect and cocktail effect. High entropy oxides have great potential for development, but there is currently little and no research on the use of high entropy oxides in the radiation shielding field.
Disclosure of Invention
At present, the design of related research materials for radiation shielding materials is single, and the research on the development and utilization of novel materials is less. The single material is difficult to realize the simultaneous shielding of neutrons and gamma rays, the invention utilizes the low atomic number of boron nitride to realize the moderation of fast neutrons, and utilizes the flexible modulation capability of high-entropy ceramic oxide elements to ensure that the same material not only contains components (Sm and Gd) with high neutron absorption cross sections, but also contains components (Hf, la, sm, gd, er and Ce) for efficiently shielding the gamma rays, and the coated double-layer structure is utilized to realize the gradual attenuation of the fast neutrons in the material.
The preparation process is simple, and the fillers are easy to agglomerate, and the invention realizes the combination of boron nitride and high-entropy ceramics in microscale by a composite form, thereby reducing the agglomeration probability of the same fillers. In addition, the invention also utilizes the random distribution of different elements in the high-entropy ceramic oxide on different lattice sites to realize the atomic-level mixing, fully exerts different functions of the elements in the shielding process, realizes the gradient attenuation of rays among lattices, increases the attenuation probability of the rays in the material and greatly improves the attenuation performance.
The high-entropy oxide can realize mutual matching through various elements in the crystal, thereby shortening the shielding distance of rays between the elements and having great potential in the radiation protection field.
The invention provides a 2 B 2 O 7 The type high-entropy ceramic powder is characterized in that the element A is composed of five or more elements of Gd, er, sm, la, ce, eu and Dy, and the element B is Hf.
The invention also provides A 2 B 2 O 7 The preparation method of the high-entropy ceramic powder comprises the steps of ball-milling oxide powder of an element A and oxide powder of an element B, drying the mixture for at least 5 hours at 60-80 ℃, and sintering the dried mixture for 1-20 hours at 900-1700 ℃ to obtain the A 2 B 2 O 7 Type high entropy ceramic powder.
Further, zirconium beads are used as grinding balls, the diameter of the grinding balls is 2mm, the ball-to-material ratio is (1-5): 1, for example, the ball-to-material ratio can be 1.
The ball milling rotation speed is further limited to 100rpm to 500rpm, and for example, the ball milling rotation speed may be 100rpm, 200rpm, 300rpm, 400rpm, 500rpm, or the like.
Further, the ball milling time is 5h to 25h, for example, the ball milling time can be 5h, 10h, 15h, 20h, 25h, and the like.
Further, the high-temperature sintering temperature may be 900 ℃, 1100 ℃, 1300 ℃, 1500 ℃, 1700 ℃ or the like.
Further limiting, the ball milling time can be from 5 to 25 hours, such as 5 hours, 10 hours, 15 hours, 20 hours, 25 hours, and the like.
The invention also provides a boron nitride/high-entropy ceramic oxide composite filler, wherein the composite filler is the high-entropy ceramic powder or the high-entropy ceramic powder prepared by the method, the surface of the composite filler is coated with boron nitride, and the load of the boron nitride is 5-30% by mass.
In the invention, the preparation method of the boron nitride/high-entropy ceramic oxide composite filler can be carried out by adopting the following methods:
the method 1 takes boron nitride and the high-entropy ceramic powder or the high-entropy ceramic powder prepared by the method as raw materials, and the boron nitride and the high-entropy ceramic powder are prepared by mechanical alloying and compounding in a ball milling mode.
And 3, ball-milling the urea modified boron nitride, and then adding the high-entropy ceramic powder or the high-entropy ceramic powder prepared by the method for ultrasonic freeze drying.
The invention also provides a boron nitride/high-entropy ceramic oxide composite coating for shielding neutrons and gamma rays, which is prepared from a resin matrix and the composite filler or the composite filler prepared by the method, wherein the mixing amount of the composite filler is 10-50% (by mass), such as: the mass fraction of the filler is 5%, 10%, 15%, 20%, 25%, 30% and the like.
Further defined, the coating thickness is 1cm to 5cm.
Further limited, the resin matrix is selected from epoxy resin, silicon rubber, clay mineral or high density polyethylene.
The invention also provides a preparation method of the boron nitride/high-entropy ceramic oxide composite coating for shielding neutrons and gamma rays, which comprises the following steps:
mechanically stirring the high-entropy ceramic powder and the resin matrix by using a three-roll grinding machine until the mixture is uniform, then coating the mixture on the surface of an object needing radiation protection, and drying the object at the temperature of between 50 and 120 ℃ for 8 to 10 hours.
Further, the coating can be applied by pouring, spraying, knife coating, etc.
Compared with the prior art, the invention has the following beneficial effects:
the invention realizes the common shielding of neutrons and gamma rays by combining high-atomic-number high-entropy oxide with boron nitride for the first time. By utilizing the simultaneous existence of various elements with high atomic number in the same unit cell of the high-entropy oxide, the gradual attenuation of rays is realized through the flexible modulation of the elements, and the collision probability between the elements is greatly increased.
The fast neutron moderation process requires moderation of the neutrons by light elements, while absorption of slow neutrons requires materials of large absorption cross-section. Boron nitride has not only light elements, but also boron (B) element having a large thermal neutron absorption cross section (σ = 760B), and it generates secondary radiation gamma rays having a low energy (E) γ ＝0.478)。
The boron nitride is compounded with the high-entropy oxide to realize the combination under the microscale, compared with direct blending, the composite material boron nitride greatly increases the moderation efficiency of the material to fast neutrons, and the moderated neutrons are directly further absorbed by elements with high absorption cross sections in the high-entropy oxide.
The invention utilizes the boron nitride/high-entropy ceramic oxide composite coating as a shielding material of neutrons and gamma rays, and can effectively control the shielding performance of the composite material by adjusting the element types, the synthesis parameters of the high-entropy oxide, the boron nitride composite process and the related parameters of the mixing process.
The boron nitride/high-entropy ceramic oxide composite coating simultaneously comprises two shielding materials: boron nitride and high-entropy oxide, nitrogen (N) element and boron (B) element atomic nucleus and fast neutron generate elastic scattering to slow the fast neutron, the absorption cross section of boron to low-energy neutron is larger, and boron capture reaction enables the product nucleus to be in an excited state and release gamma rays. The high-entropy oxide simultaneously contains metal elements (Sm, gd and Eu) with large neutron absorption cross sections and heavy metals (Hf, la, sm, gd, er and Ce) with strong gamma ray shielding rate, mutual cooperation of various metal elements is realized in a single cell, energy of gamma rays of secondary radiation is gradually attenuated while the gamma rays are generated, rich and various electron tracks are overlapped, and electron clouds are tightly overlapped, so that the interaction probability with neutrons and gamma rays is increased, and the high-entropy ceramic oxide coating has an excellent shielding effect on the neutrons and the gamma rays.
In addition, the composite coating of the boron nitride/high-entropy ceramic oxide and the epoxy resin increases the contact tightness of the coating and the protective substrate, and realizes coexistence of light weight and shielding performance.
For a better understanding of the nature and technical aspects of the present invention, reference should be made to the following detailed description of the invention, taken in conjunction with the accompanying drawings, which are provided for purposes of illustration and description, and are not intended to limit the invention.
Drawings
FIG. 1 shows the 5% BN- (La) produced in example 1 of the present invention 0.2 Sm 0.2 Gd 0.2 Er 0.2 Ce 0.2 ) 2 Hf 2 O 7 XRD pattern of high entropy ceramic oxide powder;
FIG. 2 shows 5% of BN- (La) prepared in example 1 of the invention 0.2 Sm 0.2 Gd 0.2 Er 0.2 Ce 0.2 ) 2 Hf 2 O 7 SEM and EDS test results of high entropy ceramic oxide powders;
FIG. 3 shows 5% of BN- (La) prepared in inventive example 1 0.2 Sm 0.2 Gd 0.2 Er 0.2 Ce 0.2 ) 2 Hf 2 O 7 -EP high entropy ceramic oxide coating couple 241 Am、 137 Cs、 60 The result of the mass attenuation coefficient test of the shielding of gamma rays under a Co source;
FIG. 4 shows 5% BN- (La) prepared in example 1 of the present invention 0.2 Sm 0.2 Gd 0.2 Er 0.2 Ce 0.2 ) 2 Hf 2 O 7 In the EP high-entropy ceramic oxide coating couple 25.4MeV and 4MeVNeutron removal cross section test results under a neutron source.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1:
in the embodiment, the preparation method of the boron nitride/high-entropy ceramic oxide composite coating for shielding neutrons and gamma rays comprises two parts, namely a boron nitride/high-entropy ceramic oxide composite material and epoxy resin.
1. Preparation of high-entropy oxide:
taking hafnium oxide, gadolinium oxide, erbium oxide, samarium oxide, lanthanum oxide and cerium oxide powder as ball milling materials, performing mechanical ball milling according to an equal molar ratio of elements, and determining a ball-material ratio of 5 according to the size of a ball milling device; zirconium beads are used as grinding balls with the diameter of 2mm, the ball milling tank is placed into a ball mill and corresponding parameters are set, the ball milling speed is 300rpm, and the ball milling time is 25 hours. And (4) according to the parameter setting, after the ball milling is finished, ball material separation is carried out. After separation, the powder was dried in a vacuum oven for 5 hours at a set temperature of 60 ℃. And sintering the dried mixed oxide in a high-temperature muffle furnace at 1500 ℃ for 10 hours to obtain high-entropy oxide powder.
2. Preparation of boron nitride/high entropy oxide:
taking absolute ethyl alcohol as a medium, carrying out wet mixed grinding on the high-entropy oxide and BN powder in a ball milling tank according to the proportion of 1. And (3) heating and sintering the obtained mixed powder in a tubular furnace with the nitrogen flow rate of 1.0L/min, wherein the heating rate is 3 ℃/min, the sintering temperature is 1600 ℃, and preserving heat for 3h to prepare a sintered sample.
3. Compounding boron nitride/high-entropy oxide composite powder with an epoxy resin matrix:
according to the technical scheme, a certain amount of powder is taken to be mixed with epoxy resin collectively according to the fact that the powder accounts for 20% of the total mass of the composite coating, a three-roll grinder is used for fully grinding and mixing, the grinding time can be controlled to be 6min according to the content of the powder, and after grinding is finished, slurry obtained through mixing is coated on the surface of an object to be protected in a blade coating mode to form the coating. The coating was placed in a vacuum oven and dried at 50 ℃ for 10h.
For the coatings prepared in this example, the following tests were performed:
and (3) testing the radiation protection performance: the coating is used for carrying out shielding tests on gamma-ray sources with different energies, and 241 the linear attenuation coefficient of the coating under the radiation irradiation under an Am source is 3.033 137 Under Cs source, the linear attenuation coefficient of the coating under the radiation irradiation is 0.083 60 Under the Co source, the linear attenuation coefficient of the coating under the radiation is 0.060, and the coating has better shielding performance.
Example 2:
1. preparation of high-entropy oxide:
taking hafnium oxide, cerium oxide, gadolinium oxide, erbium oxide, samarium oxide and europium oxide powder as ball milling materials, performing mechanical ball milling according to an element equimolar ratio, and determining a ball-material ratio of 3 according to the size of a ball milling device; zirconium beads are used as grinding balls with the diameter of 2mm, the ball milling tank is placed into a ball mill and corresponding parameters are set, the ball milling speed is 400rpm, and the ball milling time is 20 hours. And (4) according to the parameter setting, after the ball milling is finished, ball material separation is carried out. After separation, the powder was dried in a vacuum oven for 5 hours, set at 60 ℃. And sintering the dried mixed oxide in a high-temperature muffle furnace at 1400 ℃ for 10 hours to obtain high-entropy oxide powder.
2. Preparation of boron nitride/high entropy oxide:
urea in a molar ratio of 1 3 BO 3 Fully mixing, mixing with high-entropy oxide powder according to the proportion of 1. The mixed sample was calcined at 1000 ℃ in a hydrogen atmosphere for 6 hours. And obtaining the boron nitride/high-entropy oxide compound after the reaction is finished.
3. Compounding boron nitride/high-entropy oxide composite powder with an epoxy resin matrix:
according to the technical scheme, a certain amount of powder is taken to be mixed with epoxy resin collectively according to the fact that the powder accounts for 20% of the total mass of the composite coating, a three-roll grinder is used for fully grinding and mixing, the grinding time can be controlled to be 6min according to the content of the powder, and after grinding is finished, slurry obtained through mixing is coated on the surface of an object to be protected in a blade coating mode to form the coating. The coating was placed in a vacuum oven and dried at 50 ℃ for 10h.
For the coating prepared in this example, the following tests were performed:
and (3) testing the radiation protection performance: the coating is used for carrying out shielding tests on gamma-ray sources with different energies, and 241 the linear attenuation coefficient of the coating under the radiation irradiation under an Am source is 2.859 137 Under Cs source, the linear attenuation coefficient of the coating under the radiation irradiation is 0.081 60 Under a Co source, the linear attenuation coefficient of the coating under the radiation is 0.058, and the coating has better shielding performance.
Example 3:
1. preparation of high-entropy oxide:
taking hafnium oxide, cerium oxide, europium oxide, erbium oxide, samarium oxide and lanthanum oxide powder as ball milling materials, carrying out mechanical ball milling according to the equal molar ratio of elements, and determining the ball-to-material ratio to be 3 according to the size of a ball milling device; zirconium beads are used as grinding balls, the diameter of each grinding ball is 2mm, the ball milling tank is placed into a ball mill, corresponding parameters are set, the rotating speed of the ball mill is 500rpm, and the ball milling time is 10 hours. And (4) according to the parameter setting, after the ball milling is finished, ball material separation is carried out. After separation, the powder was dried in a vacuum oven for 5 hours, set at 60 ℃. And sintering the dried mixed oxide in a high-temperature muffle furnace at 1500 ℃ for 10 hours to obtain high-entropy oxide powder.
2. Preparation of boron nitride/high entropy oxide:
adding 100mg of boron nitride into 2g of urea for grinding, uniformly mixing, drying at 60 ℃ for 10 hours, mechanically grinding by using a planetary ball mill, wherein the rotating speed of the ball mill is 500rmp, the ball milling time is 5 hours, dialyzing for one week by using a dialysis bag after ball milling, freezing the obtained boron nitride aqueous solution by using liquid nitrogen, and drying by using a freezing drying agent. Adding 10% of high-entropy oxide into the dried powder, adding 5ml of distilled water, performing ultrasonic treatment for 2 hours, and freeze-drying the mixed material.
3. Compounding boron nitride/high-entropy oxide composite powder with an epoxy resin matrix:
according to the technical scheme, a certain amount of powder is taken to be mixed with epoxy resin collectively according to the fact that the powder accounts for 20% of the total mass of the composite coating, a three-roll grinder is used for fully grinding and mixing, the grinding time can be controlled to be 6min according to the content of the powder, and after grinding is finished, slurry obtained through mixing is coated on the surface of an object to be protected in a blade coating mode to form the coating. The coating was placed in a vacuum oven and dried at 50 ℃ for 10h.
For the coating prepared in this example, the following tests were performed:
and (3) testing the radiation protection performance: the coating is used for carrying out shielding tests on gamma-ray sources with different energies, and 241 the linear attenuation coefficient of the coating under the radiation irradiation is 3.021 under an Am source, and the linear attenuation coefficient is lower than 137 Under the Cs source, the linear attenuation coefficient of the coating under the radiation irradiation is 0.084 60 Under a Co source, the linear attenuation coefficient of the coating under the radiation irradiation is 0.059, and the coating has better shielding performance.
Claims (10)
1. A 2 B 2 O 7 The high-entropy ceramic powder is characterized in that the element A is composed of five or more elements of Gd, er, sm, la, ce, eu and Dy, and the element B is Hf.
2. A as claimed in claim 1 2 B 2 O 7 The preparation method of the type high-entropy ceramic powder is characterized in that the preparation method comprises the steps of ball milling oxide powder of an element A and oxide powder of an element B, drying the ball milled oxide powder of the element A and the oxide powder of the element B in vacuum at 60-80 ℃ for at least 5h, and sintering the ball milled oxide powder of the element B at 900-1700 ℃ for 1-20 h to obtain the element A 2 B 2 O 7 Type high entropy ceramic powder.
3. The preparation method of the high-performance ball mill is characterized in that the ball-to-material ratio is (1-5) to 1, the ball milling rotating speed is 100rpm to 500rpm, and the ball milling time can be 5h to 25h.
4. A boron nitride/high-entropy ceramic oxide composite filler is characterized in that the composite filler is the high-entropy ceramic powder in claim 1 or the high-entropy ceramic powder prepared by the method in claim 2 or 3, the surface of the high-entropy ceramic powder is coated with boron nitride, and the loading amount of the boron nitride is 5 mass percent to 30 mass percent.
5. The preparation method of the composite filler according to claim 4, wherein the preparation method is characterized in that the composite filler is prepared by taking boron nitride and the high-entropy ceramic powder according to claim 1 or the high-entropy ceramic powder prepared by the method according to claim 2 or 3 as raw materials and mechanically alloying the raw materials in a ball milling manner.
6. The method for preparing the composite filler according to claim 4, wherein the method for preparing is to mix H with the filler 3 BO 3 Carrying out wet ball milling on the high-entropy ceramic powder or the high-entropy ceramic powder prepared by the method of claim 1 or claim 2 or claim 3, and reducing the mixture under hydrogen to generate boron nitride.
7. The method for preparing the composite filler according to claim 4, wherein the method comprises the steps of ball milling the urea modified boron nitride, adding the high-entropy ceramic powder according to claim 1 or the high-entropy ceramic powder prepared by the method according to claim 2 or 3, and performing ultrasonic freeze drying.
8. A boron nitride/high-entropy ceramic oxide composite coating for shielding neutrons and gamma rays is characterized in that the composite coating is prepared from a resin matrix and the composite filler of claim 4 or the composite filler prepared by the method of any one of claims 5 to 7, and the content of the composite filler is 10 to 50 percent (mass).
9. The composite coating of claim 8, wherein the coating thickness is 1cm to 5cm; the resin matrix is made of epoxy resin, silicon rubber, clay mineral or high-density polyethylene.
10. The method for preparing the composite coating according to claim 8, wherein the method comprises the following steps:
mechanically stirring the high-entropy ceramic powder and the resin matrix by using a three-roll grinding machine until the mixture is uniform, then coating the mixture on the surface of an object needing radiation protection, and drying the object at the temperature of between 50 and 120 ℃ for 8 to 10 hours.
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| CN111533557A (en) * | 2020-03-27 | 2020-08-14 | 东华大学 | Pyrochlore type high-entropy oxide solidified body and preparation method thereof |
| CN111908922A (en) * | 2020-08-06 | 2020-11-10 | 西北工业大学 | Low-temperature synthesized rare earth hafnate high-entropy ceramic powder and preparation method thereof |
| CN113969078A (en) * | 2021-09-27 | 2022-01-25 | 哈尔滨工业大学 | Boron-based material modified rare earth oxide space n-gamma mixed field radiation shielding composite coating and preparation method thereof |
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| CN111533557A (en) * | 2020-03-27 | 2020-08-14 | 东华大学 | Pyrochlore type high-entropy oxide solidified body and preparation method thereof |
| CN111908922A (en) * | 2020-08-06 | 2020-11-10 | 西北工业大学 | Low-temperature synthesized rare earth hafnate high-entropy ceramic powder and preparation method thereof |
| CN113969078A (en) * | 2021-09-27 | 2022-01-25 | 哈尔滨工业大学 | Boron-based material modified rare earth oxide space n-gamma mixed field radiation shielding composite coating and preparation method thereof |
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Application publication date: 20221021 |