CN113956846B - Rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, composite coating and preparation method - Google Patents

Rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, composite coating and preparation method Download PDF

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CN113956846B
CN113956846B CN202111142392.1A CN202111142392A CN113956846B CN 113956846 B CN113956846 B CN 113956846B CN 202111142392 A CN202111142392 A CN 202111142392A CN 113956846 B CN113956846 B CN 113956846B
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mxene
rare earth
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earth oxide
aptes
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CN113956846A (en
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吴晓宏
秦伟
李杨
卢松涛
洪杨
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Harbin Institute of Technology
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00Shielding characterised by the composition of the materials
    • G21F1/02Selection of uniform shielding materials
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

A rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, a composite coating and a preparation method thereof belong to the technical field of radiation protection. The invention aims to overcome the defects that the existing radiation-proof material has poor shielding performance on space charged particles and is single in protection. The rare earth oxide nanoparticle doped Mxene material is prepared by adding excessive Mxene suspension with negative charges into APTES-Gd2O3And (3) performing ultrasonic treatment on the dispersion under Ar flow, centrifuging, and performing freeze drying to obtain the product. According to the invention, the two-dimensional layered structure of the Mxene and the high-Z and high-neutron absorption cross sections of the rare earth oxide are utilized, the rare earth oxide is doped into the Mxene layer, high-Z and low-Z layered compounding is realized, and full protection is realized by matching high-Z shielding gamma rays, low-Z shielding neutrons and high-Z. The invention is suitable for the fields of spacecraft, nuclear reactors, nuclear protection, medical treatment and the like, and has very wide application prospect.

Description

Rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, composite coating and preparation method
Technical Field
The invention belongs to the technical field of radiation protection, and particularly relates to a rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection and a preparation method thereof; and a composite coating for radiation protection of spatially charged particles and a preparation method thereof.
Background
Radiation is used in power generation, medicine, research and industry. If sufficient safety precautions are not taken when using radiation, especially ionizing radiation (neutrons, gamma and X-rays), it may damage living cells and their genetic material (DNA). Therefore, radiation safety is very important to human life and the environment. And the spacecraft can meet the severe tests from various space radiation environments during the on-orbit operation, such as electrons, protons, heavy ions, photons and the like, and can cause single event effect, total dose effect, surface charge and discharge effect, internal charging effect, displacement damage effect and the like of spacecraft materials, components and subsystems and the like, so that the performance of the materials or the devices is degraded. Therefore, shielding materials should be used according to the type and energy of radiation to ensure radiation safety.
In the prior art and materials, Mxene is used as a radiation shielding material, and more importantly, the traditional low-Z element is used for shielding neutrons, and the traditional high-Z metal material is used for shielding gamma rays. And basically does not combine high and low Z in application, so that one material can simultaneously have the shielding capability of charged particles such as neutrons, gamma rays and the like.
Disclosure of Invention
The invention aims to overcome the defects that the existing radiation-proof material has poor shielding performance on space charged particles and single protection, and provides a preparation method of a radiation-proof material with good shielding performance on the space charged particles and good thermal stability.
The invention aims to prepare a multi-layer high-low Z complex substance on a microscopic scale by utilizing a layered structure of Mxene, and mix the substance with resin by utilizing a large thermal neutron absorption section of rare earth oxide so as to prepare a coating with excellent radiation resistance. According to the invention, the two-dimensional layered structure of the Mxene and the high-Z and high-neutron absorption cross sections of the rare earth oxide are utilized, the rare earth oxide is doped into the Mxene layer, high-Z and low-Z layered compounding is realized, and the gamma rays are fully protected by matching of high-Z shielding gamma rays, low-Z shielding neutrons and high-Z.
In recent years, a novel two-dimensional transition metal carbide (Mxene) having a hydrophilic surface and high metal conductivity has been reported. This new 2D Mxene can be produced by etching the "MAX" stage of aluminum, a unique 2D open structure, a large surface area to volume ratio, and high chemical stability, whose highly conductive properties are considered as "inorganic graphene". The microscopic morphology of Mxene is an accordion-shaped multilayer structure, each piece is about 1.33nm, and Mxene is a nano material with good functions and can be assembled with other nano materials. Their unique surface chemistry, i.e., termination at Mxen after etching and delaminationThe hydrophilic groups of the es surface provide a number of opportunities for assembly into Mxene building blocks. Particularly at liquid-liquid, liquid-solid, liquid-gas, solid-solid interfaces, allows for the efficient fabrication of a variety of structures, including Mxene surfactants, Mxene heterostructures, Mxene transparent films. And Ti2CTxThe medium contains low-Z element Ti, which has a shielding effect on neutrons and reduces the generation of secondary gamma particles.
The high atomic number element of the rare earth oxide has the function of attenuating gamma rays; in addition, the rare earth distribution is wide in China, the rare earth ore is various, and the rare earth element quality is high, so that the basic rare earth for the development of the rare earth industry has the following characteristics: no toxicity, light weight, high quality (up to 99.5%), moderate price. The rare earth elements mostly belong to lanthanide elements, when the rare earth elements and other elements form a new compound through valence bond action, due to the special space orbital configuration of the lanthanide elements, 4f, 5d, 6s and 6p orbitals can be used as valence orbitals to perform space orbital hybridization, the space coverage of valence electrons is larger, and the probability of Compton scattering is increased. The absorption edge of the K layer of the rare earth elements is between 60 and 88 Kev. It follows that lanthanides are able to compensate for the "weak absorption edge" of lead. The rare earth oxide is added into the resin, so that the mechanical property of the material is improved, and the effect of protecting rays is obvious, wherein the protection effect of the rare earth element Er on low-energy gamma rays is more obvious than that of lead. And the rare earth oxide also has a thermal neutron absorption cross section higher than that of boron, so that the rare earth oxide becomes a novel neutron absorber. Therefore, the rare earth oxide has a function of protecting rays, and the radiation protection material of the rare earth oxide is applied more and more in practice.
Therefore, the Mxene/rare earth oxide material with high-low Z layered arrangement is prepared by filling the rare earth oxide into the layer gap of the Mxene by utilizing the layered structure of the Mxene, and is used for the radiation shielding field.
In order to solve the technical problem, the rare earth oxide nanoparticle doped Mxene material for the radiation protection of the space charged particles is characterized in that the rare earth oxide nanoparticles are uniformly doped between Mxene layers, and the doping amount of the rare earth oxide nanoparticles is 10-60%.
Further defined, the rare earth oxide is Gd2O3、Eu2O3、Pr2O3、Dy2O3、Er2O3One or any combination of the two in any ratio.
The preparation method of the Mxene comprises the steps of etching Al in MAX by hydrofluoric acid, adjusting the pH value, and drying in a drying oven to obtain the Mxene.
The preparation method of the Mxene can also comprise the steps of mixing MAX and concentrated hydrochloric acid, putting the mixture into an autoclave, putting the autoclave into an oven, heating the mixture for a period of time, cooling the mixture to room temperature, washing the mixture, carrying out freeze drying to obtain the Mxene, transferring the Mxene into a tetramethylammonium hydroxide solution, and stirring the Mxene at the room temperature. And (4) carrying out centrifugal washing and ultrasonic treatment to obtain the Mxene.
The preparation method of the rare earth oxide nanoparticle doped Mxene material for shielding neutron and gamma radiation comprises the following steps: adding aqueous solution of rare earth nitrate into Mxene, stirring, adding ammonia water, heating, stirring, and adding Gd2O3And (3) precipitating and uniformly doping the nanoparticles between the Mxene layers to obtain the rare earth oxide nanoparticle doped Mxene material.
The invention discloses a preparation method of a rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, which can be further carried out by the following steps:
adding excess negatively charged Mxene suspension to APTES-Gd2O3And in the dispersion, performing ultrasonic treatment for 1h under Ar flow, then centrifuging at 3500rpm for 1h, and performing freeze drying to obtain the rare earth oxide nanoparticle doped Mxene material.
APTES-Gd2O3The preparation method and the process parameters of the dispersion are as follows: gd is added2O3Dispersing in 100-200ml of ethanol, performing ultrasonic treatment for 30-120min, adding 1-2ml of cationic surfactant APTES, refluxing for 3-5h, cooling to room temperature, washing with ethanol to remove the unbound APTES, and performing vacuum drying on the product at 40-80 ℃.
Further defined, the excess is 5% to 10% by weight.
The composite coating for the radiation protection of spatially charged particles in the present invention is composed of 30-70 wt.% of the doped Mxene material of any of claims 1-4 and the balance of an organic resin matrix; or a doped Mxene material made by the method of claim 5, 6, or 7 in an amount of 30 wt.% to 70 wt.%.
Further, the organic resin matrix is one of cyanate ester, epoxy resin and polyurethane.
The preparation method of the composite coating comprises the following steps: and spraying the coating by a pneumatic spraying process or preparing the coating by a blade coating method, and curing at 30-80 ℃ to obtain the composite coating.
The invention prepares a layered Mxene structure containing low Z elements by MAX through etching, and can dope fillers into the Mxene to form a microscale laminated structure. Rare earth oxide nano particles are doped between layers to form a micro-scale high-low Z matching structure, so that the irradiation of space charged particles can be effectively shielded.
The invention utilizes the multilayer structure characteristics of Mxene, and adds rare earth oxide into Mxene, wherein the rare earth oxide has high atomic number and can effectively shield gamma rays, the thermal neutron absorption cross section of the rare earth oxide is also larger, and the rare earth oxide has good shielding effect on neutrons, and low Z elements contained in Mxene can also well shield neutrons. The laminated structure formed in this way can effectively shield the irradiation of the space charged particles and reduce the secondary particles.
The addition of the nano filler in the invention has a reinforcing effect on the resin matrix.
Compared with the existing radiation-proof material, the Mxene has an accordion structure, is similar to graphene, can be filled with a large amount of rare earth oxides between layers, contains low-Z element Ti, and belongs to a high-Z material, so that the Mxene and the rare earth oxides are compounded to form a high-Z and low-Z matched material, the rare earth elements can protect neutrons and gamma rays, and the low-Z Mxene can effectively protect generated bremsstrahlung, so that the composite material has a better shielding effect on protecting the neutrons and the gamma rays.
Meanwhile, the invention provides that the coating is prepared by compounding the resin and the Mxene doped with the rare earth oxide nanoparticles, which is different from the existing material.
The invention is suitable for the fields of spacecraft, nuclear reactors, nuclear protection, medical treatment and the like, and has very wide application prospect.
Drawings
FIG. 1 is Mxene/Gd obtained by the method of example 12O3SEM photograph of the composite coating;
FIG. 2 is Mxene/Gd obtained by the method of example 12O3EDS photograph of the composite coating.
Detailed Description
Example 1: the preparation method of the rare earth oxide nanoparticle doped Mxene material for the radiation protection of the space charged particles in the embodiment is carried out by the following steps:
mxene material prepared by hydrofluoric acid etching method
4g of Ti3AlC2The powder was dispersed in 40mL of 40 vol% HF solution, and the dispersion was stirred at room temperature for 24 hours to remove the Al layer. The slurry was filtered and washed to remove all HF until pH ≈ 7. Then, the solution was freeze-dried for 24 hours to obtain Ti3C2Tx
Preparation of rare earth oxide nanoparticle doped Mxene
Adding 100mL of 1mol/L gadolinium nitrate aqueous solution into 1g of Mxene, stirring uniformly, adding 20mL of 25% ammonia water, heating and stirring to obtain Gd2O3The nano particles are separated out and uniformly dispersed on the surface between the Mxene layers, and the Mxene/Gd between the Mxene layers is uniformly doped2O3A composite material.
Preparing a composite material:
adding 30% of Mxene doped with rare earth oxide nanoparticles into epoxy resin, putting the mixture into a two-roller grinding machine, grinding for 5min to uniformly mix, and taking down the mixture. The coating is then sprayed using a pneumatic spray process or prepared by a knife coating process, such as knife coating on a glass sheet, to a film thickness of 200 μm. After the blade coating is finished, placing the glass fiber into an oven to be cured for 3 hours at the temperature of 30 ℃; the coating is obtained as shown in figures 1 and 2.
Example 2: this example is different from example 1 in that:
preparing the Mxene doped with the rare earth oxide nanoparticles by adopting another method
By positively charged APTES-Gd2O3Preparing Gd through electrostatic attraction between the Gd and Mxene nano-sheets with negative charges2O3A/Mxene composite material. An excess of Mxene suspension (100mL,0.3mg/mL) was added to APTES-Gd2O3In dispersion (20mL,0.3mg/mL), sonication was performed under Ar flow for 1 h. Then, the mixture was centrifuged at 3500rpm for 1 hour. Freeze drying to obtain Gd2O3a/Mxene composite material.
APTES-Gd2O3The preparation method and the process parameters of the dispersion are as follows: gd is added2O3Dispersing in 200ml ethanol, ultrasonic treating for 30min, adding 2ml cationic surfactant APTES, refluxing for 3h, cooling to room temperature, washing with ethanol to remove unbound APTES, and vacuum drying at 40 deg.C.
The other steps and parameters were the same as in example 1.
Example 3, this example uses europium nitrate instead of gadolinium nitrate, and the other steps and parameters are the same as example 1.
Example 4, this example is different from example 1 in that:
mxene material prepared by hydrochloric acid hydrothermal etching
Fluorine-free Mxenes are prepared by a hydrothermal etching process using concentrated HCl. 200mg of the obtained MAX and 20mL of HCl (12M) were placed in a 50mL autoclave with a polytetrafluoroethylene liner. Thereafter, the autoclave was placed in an oven and baked at 120 ℃ and 140 ℃ for 5 days. After cooling to room temperature, the mixture was washed several times with deionized water and ethanol. Then, fluorine-free Mxenes were obtained after 1 day of freeze-drying. For the demixing of Mxenes, 100mg of Mxenes were transferred to 3mL of 25% tetramethylammonium hydroxide solution and stirred at room temperature for 3 hours. After centrifugation, the precipitate was dispersed in 40mL of water by washing 2 times with deionized water, sonicating at 10 ℃ with water cooling for 1 h. Finally, a suspension of layered mxexes sheets was obtained after centrifugation at 3000rpm for 20 minutes.
The other steps and parameters were the same as in example 1.
The examples were tested for performance by the following method:
and (3) testing the radiation protection performance: shielding tests were performed using the above coatings on an Am-241 radiation source having an energy of 59.5KeV and a linear attenuation coefficient of 3.05 μ/cm under the Am source-1The composite coating shows better radiation protection performance of the space charged particles under the Am source.
TABLE 1
Figure BDA0003284225900000051
As can be seen from fig. 1, the composite coating shows better radiation protection performance of the space charged particles under the Am source.

Claims (11)

1. The Mxene doped rare earth oxide nanoparticle material for the radiation protection of space charged particles is characterized in that the Mxene doped material is formed by uniformly doping rare earth oxide nanoparticles between Mxene layers, and the doping amount of the rare earth oxide nanoparticles is 10-60%;
wherein the Mxene-doped material is prepared by the following steps: adding aqueous solution of rare earth nitrate into Mxene, stirring, adding ammonia water, heating, stirring, and adding Gd2O3And (3) precipitating and uniformly doping the nanoparticles between the Mxene layers to obtain the rare earth oxide nanoparticle doped Mxene material.
2. The Mxene doped rare earth oxide nanoparticle material for the radiation protection of space charged particles is characterized in that the Mxene doped material is formed by uniformly doping rare earth oxide nanoparticles between Mxene layers, and the doping amount of the rare earth oxide nanoparticles is 10-60%;
wherein the Mxene-doped material is prepared by the following steps: adding excessive negatively charged MXene suspension to APTES-Gd2O3In dispersion under Ar flowPerforming ultrasonic treatment for 1h, then centrifuging at 3500rpm for 1h, and performing freeze drying to obtain the rare earth oxide nanoparticle doped Mxene material;
APTES-Gd2O3the preparation method and the process parameters of the dispersion are as follows: gd is added2O3Dispersing in 100-200mL ethanol, performing ultrasonic treatment for 30-120min, adding 1-2mL cationic surfactant APTES, refluxing for 3-5h, cooling to room temperature, washing with ethanol to remove unbound APTES, and vacuum drying at 40-80 deg.C.
3. A doped Mxene material according to claim 1 or 2, wherein the rare earth oxide is Gd2O3、Eu2O3、Pr2O3、Dy2O3、Er2O3Or a combination of both.
4. A doped Mxene material according to claim 1 or 2, wherein the Mxene is prepared by etching away Al in MAX with hydrofluoric acid, adjusting pH, and drying in an oven.
5. A doped Mxene material according to claim 1 or 2, wherein the Mxene is prepared by mixing MAX with concentrated hydrochloric acid, placing the mixture in an autoclave, placing the autoclave in an oven, heating for a period of time, cooling to room temperature, washing, freeze-drying to obtain Mxene, transferring the Mxene into a tetramethylammonium hydroxide solution, stirring at room temperature, centrifuging, washing, and performing ultrasonic treatment to obtain Mxene.
6. A method of preparing a doped Mxene material of claim 1, comprising the steps of:
adding aqueous solution of rare earth nitrate into Mxene, stirring, adding ammonia water, heating, stirring, and adding Gd2O3And (3) precipitating and uniformly doping the nanoparticles between the Mxene layers to obtain the rare earth oxide nanoparticle doped Mxene material.
7. A method of preparing a doped Mxene material according to claim 2, comprising the steps of:
adding excess negatively charged MXene suspension to APTES-Gd2O3In the dispersion, performing ultrasonic treatment for 1h under Ar flow, then centrifuging for 1h at 3500rpm, and performing freeze drying to obtain a rare earth oxide nanoparticle doped Mxene material;
APTES-Gd2O3the preparation method and the process parameters of the dispersion are as follows: gd is added2O3Dispersing in 100-200mL ethanol, performing ultrasonic treatment for 30-120min, adding 1-2mL cationic surfactant APTES, refluxing for 3-5h, cooling to room temperature, washing with ethanol to remove unbound APTES, and vacuum drying at 40-80 deg.C.
8. A method of preparing a doped Mxene material according to claim 7, characterized in that an excess of 5% -10% by weight of negatively charged MXene suspension is added to APTES-Gd2O3In dispersion.
9. A composite coating for radiation protection of spatially charged particles, characterized in that the composite coating consists of 30-70 wt.% of a doped Mxene material according to any one of claims 1-5 and the balance an organic resin matrix; or a doped Mxene material made by the method of claim 6, 7 or 8 in an amount of 30 wt.% to 70 wt.%.
10. The composite coating of claim 9, wherein the organic resin matrix is one of cyanate, epoxy, and polyurethane.
11. The method of preparing the composite coating of claim 9, wherein the composite coating is prepared by: and spraying the coating by a pneumatic spraying process or preparing the coating by a blade coating method, and curing at 30-80 ℃ to obtain the composite coating.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3516948A (en) * 1967-03-24 1970-06-23 Commissariat Energie Atomique Neutron-absorbing graphitic product and method of preparation
CN105304154A (en) * 2014-07-03 2016-02-03 中国科学院宁波材料技术与工程研究所 Application of two-dimensional transitional metal carbide nanosheet as radionuclide adsorbent
CN106563479A (en) * 2016-10-19 2017-04-19 河南理工大学 Two-dimensional carbide-supported rare earth fluoride nanometer powder, preparation method and applications thereof
CN113260242A (en) * 2021-04-27 2021-08-13 北京理工大学 Composite wave-absorbing material with magnetic particles doped with rare earth elements loaded on layered MXene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3516948A (en) * 1967-03-24 1970-06-23 Commissariat Energie Atomique Neutron-absorbing graphitic product and method of preparation
CN105304154A (en) * 2014-07-03 2016-02-03 中国科学院宁波材料技术与工程研究所 Application of two-dimensional transitional metal carbide nanosheet as radionuclide adsorbent
CN106563479A (en) * 2016-10-19 2017-04-19 河南理工大学 Two-dimensional carbide-supported rare earth fluoride nanometer powder, preparation method and applications thereof
CN113260242A (en) * 2021-04-27 2021-08-13 北京理工大学 Composite wave-absorbing material with magnetic particles doped with rare earth elements loaded on layered MXene

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