CN114408973A - Nuclear radiation shielding material and preparation method thereof - Google Patents
Nuclear radiation shielding material and preparation method thereof Download PDFInfo
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- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 52
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims abstract description 52
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 49
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 20
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 8
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 8
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- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 claims description 4
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- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
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- QDOAVFZGLCBVQL-UHFFFAOYSA-N bismuth Chemical compound [Bi].[Bi].[Bi] QDOAVFZGLCBVQL-UHFFFAOYSA-N 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing, besides tungsten, two or more other elements, with the exception of oxygen or hydrogen
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
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- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
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- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a nuclear radiation shielding material and a preparation method thereof. The absorption edges of the K layers of tungsten and bismuth are 69.5KeV and 90.5KeV respectively, the absorption edge of the K layer of erbium is 57.5KeV, and erbium has a lower absorption edge of the K layer. The preparation method provided by the invention has the advantages of simple process, low energy consumption, no toxicity, no harm and easy realization, and can provide beneficial reference for the development of environment-friendly and efficient radiation protection materials.
Description
Technical Field
The invention relates to the field of nuclear radiation shielding materials, in particular to a nuclear radiation shielding material and a preparation method thereof.
Background
The application of nuclear energy and nuclear technology is a double-edged sword, and when people enjoy huge welfare, if the people use or protect the sword improperly, the generated high-energy rays (X, gamma rays, neutrons and the like) can cause great harm to the health of the people and the ecological environment. Lead (Pb) is a widely used X/gamma ray protection material, but lead has toxicity and a weak absorption region for rays with energy between 40 and 88KeV, so that the novel, environment-friendly and efficient ray shielding material has important significance for guaranteeing the life health of nuclear personnel and the public.
The traditional radiation protection theory about the attenuation effect of a substance on rays mainly depends on the types and energies of particles, the elemental composition and the density of the material, and other factors. As a shielding material for replacing Pb, the application of tantalum, tungsten, bismuth and rare earth metal elements in X/gamma ray radiation protection is widely concerned. The Chinese invention patent CN107910089A discloses a method for manufacturing a novel flexible lead-free radiation protective garment, which uses nontoxic environment-friendly materials such as tantalum, tungsten, barium and the like as functional fillers, has the performance of shielding X/gamma rays equivalent to that of lead, and can effectively protect nuclear radiation hazards. RST company in the united states developed a lead-free nuclear radiation protective fabric, named Demron, by a new technology of doping tantalum-modified polyvinyl chloride and polyethylene, and has been currently used in a variety of fields.
However, the X-ray has a continuous spectrum and a wide energy range, and the energies of the gamma rays emitted by different nuclides are different, so the shielding effect of the nuclear radiation protection material based on high atomic coefficient elements such as lead and bismuth on low-energy rays is still to be improved.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, the present invention aims to provide a nuclear radiation shielding material and a preparation method thereof, and aims to solve the problem of poor shielding effect of the existing elements such as lead and bismuth on low-energy rays.
The technical scheme of the invention is as follows:
in a first aspect of the invention, there is provided a nuclear radiation shielding material, wherein the nuclear radiation shielding material comprises erbium-doped bismuth tungstate.
Optionally, the nuclear radiation shielding material is erbium-doped bismuth tungstate.
Optionally, the molar ratio of erbium to bismuth tungstate in the erbium-doped bismuth tungstate is (2-15): 100.
Optionally, the microstructure of the erbium-doped bismuth tungstate is a flower ball-shaped structure formed by stacking sheets, the thickness of each sheet is 50-80 nm, the diameter of each flower ball is 0.5-2.0 μm, and the crystalline phase of the erbium-doped bismuth tungstate is an orthorhombic phase.
In a second aspect of the present invention, a method for preparing a nuclear radiation shielding material is provided, wherein the method comprises the steps of:
providing a bismuth source, a tungsten source, an erbium source, an acid solution and water;
dissolving the bismuth source in an acid solution to obtain a bismuth source acid solution;
dissolving the tungsten source in water to obtain a tungsten source water solution;
dissolving the erbium source in water to obtain an erbium source aqueous solution;
mixing the bismuth source acid solution and the tungsten source aqueous solution, and adjusting the pH of the system to 5-7 to obtain a bismuth tungstate precursor solution;
and adding the erbium source aqueous solution into the bismuth tungstate precursor solution, and carrying out hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
Alternatively,
the bismuth source is selected from one or two of bismuth nitrate and bismuth oxide; and/or the presence of a gas in the gas,
the tungsten source is selected from tungstate, and the tungstate is selected from one or two of sodium tungstate and ammonium tungstate; and/or the presence of a gas in the gas,
the erbium source is selected from one or two of erbium nitrate and erbium oxide; and/or the presence of a gas in the gas,
the acid solution is nitric acid water solution or acetic acid water solution.
Alternatively,
the molar ratio of bismuth in the bismuth source to tungsten in the tungsten source is (2-2.2) to (1-1.2); and/or the presence of a gas in the gas,
the molar ratio of erbium in the erbium source to tungsten in the tungsten source is (2-15): 100.
Optionally, adding NaOH aqueous solution to adjust the pH of the system to 5-7;
and/or the temperature of the hydrothermal reaction is 160-200 ℃ and the time is 24-48 h.
Alternatively,
under the condition of stirring, mixing the bismuth source acid solution and the tungsten source aqueous solution, stirring for 30-60 min, adjusting the pH of the system to 7, and continuing stirring for 1-2 h to obtain a bismuth tungstate precursor solution; and/or the presence of a gas in the gas,
and under the condition of stirring, adding the erbium source aqueous solution into the bismuth tungstate precursor solution, stirring for 1-2 h, and carrying out hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
Optionally, the method further comprises the following step after the hydrothermal reaction: and (3) sequentially carrying out centrifugal separation, washing and drying on the solution after the hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
Has the advantages that: the invention provides a nuclear radiation shielding material and a preparation method thereof, wherein the absorption edges of K layers of tungsten and bismuth are 69.5KeV and 90.5KeV respectively, the absorption edge of the K layer of erbium is 57.5KeV, and erbium has a lower absorption edge of the K layer. The preparation method provided by the invention has the advantages of simple process, low energy consumption, no toxicity, no harm and easy realization, and can provide beneficial reference for the development of environment-friendly and efficient radiation protection materials.
Drawings
Fig. 1 is an XRD pattern of erbium-doped bismuth tungstate prepared in example 1 of the present invention.
Fig. 2 (a) and (b) are SEM images of erbium-doped bismuth tungstate prepared in example 1 of the present invention.
FIG. 3 is a graph showing EDS results of erbium-doped bismuth tungstate prepared in example 1 of the present invention.
Fig. 4 is a graph showing the results of the gamma-ray shielding performance test of erbium-doped bismuth tungstate prepared in examples 1 to 4 of the present invention.
Detailed Description
The invention provides a nuclear radiation shielding material and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the prior art, bismuth tungstate (Bi)2WO6) Is a typical Aurivillius oxide with Bi2O2 2+And WO4 2-The perovskite layered structure formed by the layers alternating along the c axis is widely applied to the field of photocatalysis due to the characteristics of safety, no toxicity, easy adjustment of structural morphology, excellent photocatalytic performance, stable physicochemical properties and the like. The inventor finds that the bismuth tungstate has tungsten and bismuth with high atomic coefficients at the same time, has high density and has important application value in the aspect of high-energy ray protection. However, bismuth tungstate has poor shielding performance on low-energy rays, and therefore, the invention provides the nuclear radiation shielding material, wherein the nuclear radiation shielding material comprises erbium-doped bismuth tungstate.
The inventor finds that the "absorption edge" effect of the K layer of the element is an important factor for improving the shielding performance of the material through extensive research, and the "absorption edge" of the K layer refers to a phenomenon that the section of the photoelectric effect sharply increases when the energy of incident photons is equal to the binding energy of electrons of the K layer. In bismuth tungstate, the absorption edges of K layers of tungsten and bismuth are 69.5KeV and 90.5KeV respectively, and the shielding capability of the bismuth tungstate on 69.5-88.0 KeV rays and more than or equal to 90.5KeV rays is better than that of lead. However, the X-ray and the gamma-ray are continuous spectrums, the energy ranges of the X-ray and the gamma-ray are wide, the 'absorption edge' of the K layer of the rare earth element is low (for example, the 'absorption edge' of the K layer of the erbium is 57.5KeV), and if the rare earth element such as strontium, the erbium and the like is doped into the bismuth tungstate, and the complementary effect of the 'absorption edge' of the K layer of the erbium is utilized, the shielding performance of the material on low-energy rays can be effectively improved. Therefore, in the embodiment of the invention, erbium is doped into bismuth tungstate, the erbium has a lower K layer absorption edge, and the shielding performance of the bismuth tungstate material on low-energy rays is effectively improved by utilizing the complementary effect of the K layer absorption edge of the erbium.
In one embodiment, the nuclear radiation shielding material is erbium doped bismuth tungstate.
In one embodiment, the molar ratio of erbium to bismuth tungstate in the erbium-doped bismuth tungstate is (2-15): 100. In the embodiment, the molar ratio of erbium to bismuth tungstate in the erbium-doped bismuth tungstate nuclear radiation shielding material is (2-15): 100, that is, the molar doping amount of erbium accounts for 2-15% of the molar number of bismuth tungstate, the doping ratio does not influence the shielding performance of bismuth tungstate on high-energy rays, and the shielding efficiency of erbium-doped bismuth tungstate on low-energy rays is remarkably increased along with the increase of the molar doping amount of erbium in the ratio range. The low-energy rays are low-energy X rays or low-energy gamma rays. The nuclear radiation shielding material provided by the embodiment can effectively shield low-energy X rays or low-energy gamma rays with the energy of 59.5 KeV.
In one embodiment, the microstructure of the erbium-doped bismuth tungstate is a flower-ball-shaped structure formed by stacking sheets, the thickness of each sheet is 50-80 nm, the diameter of each flower-ball is 0.5-2.0 μm, the crystal phase of the erbium-doped bismuth tungstate is an orthorhombic phase, and the bismuth tungstate in the erbium-doped bismuth tungstate in the embodiment is orthorhombic bismuth tungstate (Bi)2WO6) Erbium is doped into the crystal lattice of the bismuth tungstate, and the doping of the erbium does not influence the crystal phase of the bismuth tungstate, but increases the specific surface area of the material and increases the probability of the interaction of the material and high-energy particles.
Bismuth tungstate (Bi)2WO6) Is a typical Aurivillius oxide, has a perovskite layered structure, and is widely applied to the field of photocatalysis due to the characteristics of safety, no toxicity, excellent photocatalytic performance, stable physicochemical properties and the like. The preparation method of the bismuth tungstate photocatalytic material comprises a solid-phase sintering method, a solvothermal method, a sol-gel method and the like, and the methods have different defects: the solid-phase sintering method has higher requirement on the environmental temperature, large energy consumption and low energy utilization rate; organic solvents required by the solvothermal method generally have toxicity, are easy to cause harm to bodies and environment due to improper use, and can bring potential safety hazards to the stability of a reaction system; the sol-gel method consumes a large amount of raw materials in the preparation process, and has poor economic benefit. In the prior art, the preparation method is designed and researched aiming at the bismuth tungstate photocatalysis material. At present, no preparation method which is simple to operate, low in energy consumption, non-toxic and harmless is provided for preparing erbium-doped bismuth tungstate with excellent nuclear radiation shielding performance, and based on the preparation method, the embodiment of the invention also provides nuclear radiationThe preparation method of the radiation shielding material comprises the following steps:
s1, providing a bismuth source, a tungsten source, an erbium source, an acid solution and water;
s2, dissolving the bismuth source in an acid solution to obtain a bismuth source acid solution;
s3, dissolving the tungsten source in water to obtain a tungsten source water solution;
s4, dissolving the erbium source in water to obtain an erbium source water solution;
s5, mixing the bismuth source acid solution and the tungsten source aqueous solution, and adjusting the pH of the system to 5-7 to obtain a bismuth tungstate precursor solution;
s6, adding the erbium source aqueous solution into the bismuth tungstate precursor solution, and carrying out hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
The preparation method provided by the embodiment of the invention has the advantages of simple process, low energy consumption, no toxicity, no harm and easy realization, and can provide beneficial reference for the development of environment-friendly and efficient radiation protection materials. The erbium-doped bismuth tungstate prepared by the embodiment has a good shielding effect on low-energy rays.
In step S1, in one embodiment, the bismuth source is selected from one or two of bismuth nitrate and bismuth oxide, but is not limited thereto. Wherein, bismuth nitrate [ Bi (NO)3)3·5H2O]Or bismuth oxide (Bi)2O3) Purity of (2)>99 percent. In this embodiment, bismuth nitrate [ Bi (NO)3)3·5H2O]Or bismuth oxide (Bi)2O3) Providing a bismuth source for erbium-doped bismuth tungstate nuclear radiation shielding materials.
In one embodiment, the tungsten source is selected from tungstates selected from one or both of sodium tungstate and ammonium tungstate, but not limited thereto, wherein sodium tungstate (Na)2WO4·2H2O) or ammonium tungstate [ (NH)4)6W7O24·6H2O]Purity of (2)>99 percent. In this embodiment, sodium tungstate (Na)2WO4·2H2O) or ammonium tungstate [ (NH)4)6W7O24·6H2O]Provides a tungsten source for erbium-doped bismuth tungstate nuclear radiation shielding material.
In one embodiment, the erbium source is selected from one or both of erbium nitrate and erbium oxide, but is not limited thereto.
In one embodiment, the acid solution is an aqueous nitric acid solution or an aqueous acetic acid solution, but is not limited thereto.
In one embodiment, the bismuth source is selected from one or two of bismuth nitrate and bismuth oxide, the tungsten source is selected from tungstate, the tungstate is selected from one or two of sodium tungstate and ammonium tungstate, the erbium source is selected from erbium nitrate, and the acid solution is an aqueous nitric acid solution or an aqueous acetic acid solution, but is not limited thereto.
In step S2, dissolving the bismuth source in an acid solution to obtain a bismuth source acid solution; when the bismuth source is selected from bismuth nitrate and the acid solution is selected from aqueous nitric acid, the bismuth nitrate is dissolved in aqueous nitric acid to give an acidic bismuth nitrate solution, with the aim of avoiding hydrolysis of the bismuth nitrate prior to the reaction. When the bismuth source is selected from bismuth oxide and the acid solution is selected from nitric acid aqueous solution, the bismuth oxide is dissolved in the nitric acid aqueous solution and can react to generate bismuth nitrate, and the generated bismuth nitrate is dissolved in the nitric acid aqueous solution to obtain acidic bismuth nitrate solution, so that the generated bismuth nitrate can be prevented from being hydrolyzed.
In one embodiment, the molar ratio of bismuth in the bismuth source to tungsten in the tungsten source is (2-2.2): (1-1.2) in steps S1-S6.
In one embodiment, the molar ratio of erbium in the erbium source to tungsten in the tungsten source is (2-15): 100. In the embodiment, the molar ratio of erbium to bismuth tungstate in the finally obtained erbium-doped bismuth tungstate is (2-15): 100.
In one embodiment, the molar ratio of bismuth in the bismuth source to tungsten in the tungsten source is (2-2.2): 1-1.2, and the molar ratio of erbium in the erbium source to tungsten in the tungsten source is (2-15): 100.
In step S5, in one embodiment, the pH of the system is adjusted to 5-7 by adding NaOH aqueous solution.
In one embodiment, the bismuth source acid solution and the tungsten source aqueous solution are mixed under stirring, stirring is carried out for 30-60 min, the pH value of the system is adjusted to 7, stirring is continued for 1-2 h, and a bismuth tungstate precursor solution is obtained, wherein the reaction can be more thorough under the condition.
In step S6, in one embodiment, the temperature of the hydrothermal reaction is 160 to 200 ℃ and the time is 24 to 48 hours. The erbium-doped bismuth tungstate nuclear radiation shielding material with a microstructure of a flower-ball-shaped structure formed by stacking of sheet layers, the thickness of the sheet layers being 50-80 nm, the diameter of flower balls being 0.5-2.0 mu m and a crystal phase being an orthorhombic phase can be prepared under the hydrothermal reaction condition.
In one embodiment, under the condition of stirring, adding the erbium source aqueous solution into the bismuth tungstate precursor solution, stirring for 1-2 hours, and performing hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material. In one embodiment, the hydrothermal reaction further comprises the following steps: and (3) sequentially carrying out centrifugal separation, washing and drying on the solution after the hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
The invention is further illustrated by the following specific examples.
Example 1
(1) Weighing 48.51g (0.1mol) of Bi (NO)3)3·5H2O dissolved in 250mL of 1mol/L HNO3In the solution, stirring by magnetic force until the solution is completely dissolved, and marking as solution A; 16.5g (0.05mol) Na were weighed out2WO4·2H2Dissolving O in 50mL of deionized water, and stirring by magnetic force until the O is completely dissolved, and marking as a solution B; 0.443g (0.001mol) of Er (NO) is weighed3)3·5H2O was dissolved in 25mL of deionized water and magnetically stirred until completely dissolved, which was designated as solution C.
(2) Slowly dropwise adding the solution A into the solution B under the condition of magnetic stirring, continuously stirring for 30min at the dropwise adding speed of 10mL/min until the solutions are fully mixed, and dropwise adding 2mol/L sodium hydroxide solution to adjust the pH value of a solution system to 7 to prepare a bismuth tungstate precursor solution.
(3) And (3) under the condition of magnetic stirring, dropwise adding the solution C into the bismuth tungstate precursor solution, and continuously stirring for 30min until the solution is fully mixed to obtain a mixed solution.
(4) And (2) placing the mixed solution in a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a constant-temperature drying box at 180 ℃ for reaction for 24 hours, then carrying out centrifugal separation on a reaction product, washing the reaction product with ethanol and distilled water for 3 times respectively, and carrying out vacuum drying on the obtained solid at 80 ℃ for 10 hours to obtain the erbium-doped bismuth tungstate.
Example 2
(1) Weighing 48.51g (0.1mol) of Bi (NO)3)3·5H2O dissolved in 250mL of 1mol/L HNO3In the solution, stirring by magnetic force until the solution is completely dissolved, and marking as solution A; 16.5g (0.05mol) of Na were weighed2WO4·2H2Dissolving O in 50mL of deionized water, and stirring by magnetic force until the O is completely dissolved, and marking as a solution B; 1.108g (0.0025mol) Er (NO) are weighed out3)3·5H2O was dissolved in 25mL of deionized water and magnetically stirred until completely dissolved, which was designated as solution C.
(2) Slowly dropwise adding the solution A into the solution B under the condition of magnetic stirring, continuously stirring for 30min at the dropwise adding speed of 10mL/min until the solutions are fully mixed, and dropwise adding 2mol/L sodium hydroxide solution to adjust the pH value of a solution system to 7 to prepare a bismuth tungstate precursor solution.
(3) And (3) under the condition of magnetic stirring, dropwise adding the solution C into the bismuth tungstate precursor solution, and continuously stirring for 30min until the solution is fully mixed to obtain a mixed solution.
(4) And (2) placing the mixed solution in a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a constant-temperature drying box at 180 ℃ for reaction for 24 hours, then carrying out centrifugal separation on a reaction product, washing the reaction product with ethanol and distilled water for 3 times respectively, and carrying out vacuum drying on the obtained solid at 80 ℃ for 10 hours to obtain the erbium-doped bismuth tungstate.
Example 3
(1) Weighing 48.51g (0.1mol) of Bi (NO)3)3·5H2O dissolved in 250mL of 1mol/L HNO3In the solution, stirring by magnetic force until the solution is completely dissolved, and marking as solution A; 16.5g (0.05mol) Na were weighed out2WO4·2H2Dissolving O in 50mL of deionized water, and stirring by magnetic force until the O is completely dissolved, and marking as a solution B; 2.217g (0.005mol) Er (NO) was weighed3)3·5H2O dissolved in 25mL deionizationIn water, magnetically stir until completely dissolved, and mark as solution C.
(2) Slowly dropwise adding the solution A into the solution B under the condition of magnetic stirring, continuously stirring for 30min at the dropwise adding speed of 10mL/min until the solutions are fully mixed, and dropwise adding 2mol/L sodium hydroxide solution to adjust the pH value of a solution system to 7 to prepare a bismuth tungstate precursor solution.
(3) And (3) under the condition of magnetic stirring, dropwise adding the solution C into the bismuth tungstate precursor solution, and continuously stirring for 30min until the solution is fully mixed to obtain a mixed solution.
(4) And (2) placing the mixed solution in a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a constant-temperature drying box at 180 ℃ for reaction for 24 hours, then carrying out centrifugal separation on a reaction product, washing the reaction product with ethanol and distilled water for 3 times respectively, and carrying out vacuum drying on the obtained solid at 80 ℃ for 10 hours to obtain the erbium-doped bismuth tungstate.
Example 4
(1) Weighing 48.51g (0.1mol) of Bi (NO)3)3·5H2O dissolved in 250mL of 1mol/L HNO3In the solution, stirring by magnetic force until the solution is completely dissolved, and marking as solution A; 16.5g (0.05mol) Na were weighed out2WO4·2H2Dissolving O in 50mL of deionized water, and stirring by magnetic force until the O is completely dissolved, and marking as a solution B; 3.325g (0.0075mol) Er (NO) are weighed3)3·5H2O was dissolved in 25mL of deionized water and magnetically stirred until completely dissolved, which was designated as solution C.
(2) Slowly dropwise adding the solution A into the solution B under the condition of magnetic stirring, continuously stirring for 30min at the dropwise adding speed of 10mL/min until the solutions are fully mixed, and dropwise adding 2mol/L sodium hydroxide solution to adjust the pH value of a solution system to 7 to prepare a bismuth tungstate precursor solution.
(3) And (3) under the condition of magnetic stirring, dropwise adding the solution C into the bismuth tungstate precursor solution, and continuously stirring for 30min until the solution is fully mixed to obtain a mixed solution.
(4) And (2) placing the mixed solution in a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a constant-temperature drying box at 180 ℃ for reaction for 24 hours, then carrying out centrifugal separation on a reaction product, washing the reaction product with ethanol and distilled water for 3 times respectively, and carrying out vacuum drying on the obtained solid at 80 ℃ for 10 hours to obtain the erbium-doped bismuth tungstate.
And (3) testing:
(1) XRD, SEM and EDS tests were performed on erbium-doped bismuth tungstate prepared in example 1
From XRD, SEM and EDS tests, as can be derived from figures 1, 2, 3:
1) by comparing PDF standard cards, the erbium-doped bismuth tungstate prepared in example 1 has an orthorhombic structure (JCPDS: 79-2381 Bi)2WO6Matched), no diffraction peak of erbium element or erbium compound in figure 1, erbium doping does not make Bi2WO6The position of the diffraction peak is changed, which shows that Er ions can possibly enter a bismuth tungstate crystal lattice;
2) under a neutral condition, as shown in (a) and (b) in fig. 2, erbium-doped bismuth tungstate generated through a hydrothermal reaction is of a flake-stacked flower-sphere structure, the thickness of each flake layer is 50-80 nm, and the diameter of each flower-sphere particle is about 0.5-2.0 μm.
3) From the EDS results, fig. 3 can derive: er-doped bismuth tungstate samples can be tested to contain Er element, and further proves that Er ions really enter bismuth tungstate crystal lattices.
(2) And (3) testing the gamma ray shielding performance:
59.5KeV (KeV) (of) pairs of erbium-doped bismuth tungstate prepared in examples 1 to 4 were measured by a high-purity germanium gamma spectrometer241Am) shielding properties of gamma rays.
As a result, as shown in fig. 4, the shielding efficiency of the material against 59.5KeV gamma rays increases significantly as the erbium doping content increases.
In conclusion, the invention provides a nuclear radiation shielding material and a preparation method thereof, the absorption edges of K layers of tungsten and bismuth are 69.5KeV and 90.5KeV respectively, and the absorption edge of K layer of erbium is 57.5 KeV. The preparation method provided by the invention has the advantages of simple process, low energy consumption, no toxicity, no harm and easy realization, and can provide beneficial reference for the development of environment-friendly and efficient radiation protection materials.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A nuclear radiation shielding material, wherein the nuclear radiation shielding material comprises erbium-doped bismuth tungstate.
2. The nuclear radiation shielding material of claim 1, wherein the nuclear radiation shielding material is erbium doped bismuth tungstate.
3. The nuclear radiation shielding material of claim 1 or 2, wherein the molar ratio of erbium to bismuth tungstate in the erbium-doped bismuth tungstate is (2-15): 100.
4. The nuclear radiation shielding material of claim 1 or 2, wherein the microstructure of the erbium-doped bismuth tungstate is a flower-ball-shaped structure formed by stacking of sheets, the thickness of each sheet is 50-80 nm, the diameter of each flower ball is 0.5-2.0 μm, and the crystalline phase of the erbium-doped bismuth tungstate is an orthorhombic phase.
5. A method for preparing a nuclear radiation shielding material is characterized by comprising the following steps:
providing a bismuth source, a tungsten source, an erbium source, an acid solution and water;
dissolving the bismuth source in an acid solution to obtain a bismuth source acid solution;
dissolving the tungsten source in water to obtain a tungsten source water solution;
dissolving the erbium source in water to obtain an erbium source aqueous solution;
mixing the bismuth source acid solution and the tungsten source aqueous solution, and adjusting the pH of the system to 5-7 to obtain a bismuth tungstate precursor solution;
and adding the erbium source aqueous solution into the bismuth tungstate precursor solution, and carrying out hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
6. The method of preparing a nuclear radiation shielding material of claim 5,
the bismuth source is selected from one or two of bismuth nitrate and bismuth oxide; and/or the presence of a gas in the gas,
the tungsten source is selected from tungstate, and the tungstate is selected from one or two of sodium tungstate and ammonium tungstate; and/or the presence of a gas in the gas,
the erbium source is selected from one or two of erbium nitrate and erbium oxide; and/or the presence of a gas in the gas,
the acid solution is nitric acid water solution or acetic acid water solution.
7. The method of preparing a nuclear radiation shielding material of claim 5,
the molar ratio of bismuth in the bismuth source to tungsten in the tungsten source is (2-2.2) to (1-1.2); and/or the presence of a gas in the gas,
the molar ratio of erbium in the erbium source to tungsten in the tungsten source is (2-15): 100.
8. The preparation method of the nuclear radiation shielding material according to claim 5, wherein the pH of the system is adjusted to 5-7 by adding NaOH aqueous solution;
and/or the temperature of the hydrothermal reaction is 160-200 ℃ and the time is 24-48 h.
9. The method of preparing a nuclear radiation shielding material of claim 5,
under the condition of stirring, mixing the bismuth source acid solution and the tungsten source aqueous solution, stirring for 30-60 min, adjusting the pH of the system to 7, and continuing stirring for 1-2 h to obtain a bismuth tungstate precursor solution; and/or the presence of a gas in the gas,
and under the condition of stirring, adding the erbium source aqueous solution into the bismuth tungstate precursor solution, stirring for 1-2 h, and carrying out hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
10. The method for preparing the nuclear radiation shielding material according to claim 9, further comprising the following steps after the hydrothermal reaction: and (3) sequentially carrying out centrifugal separation, washing and drying on the solution after the hydrothermal reaction to obtain the erbium-doped bismuth tungstate nuclear radiation shielding material.
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| CN103623813A (en) * | 2013-09-12 | 2014-03-12 | 陕西科技大学 | Visible-light response Er/Bi2WO6 microspheres and preparation method and application thereof |
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| CN110105743A (en) * | 2019-04-12 | 2019-08-09 | 深圳大学 | A kind of unleaded X, gamma ray shielding material and preparation method thereof |
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| CN103623813A (en) * | 2013-09-12 | 2014-03-12 | 陕西科技大学 | Visible-light response Er/Bi2WO6 microspheres and preparation method and application thereof |
| CN107983336A (en) * | 2017-12-11 | 2018-05-04 | 湖北大学 | A kind of praseodymium doped bismuth tungstate light urges agent and preparation method thereof |
| CN110105743A (en) * | 2019-04-12 | 2019-08-09 | 深圳大学 | A kind of unleaded X, gamma ray shielding material and preparation method thereof |
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