WO2022166152A1 - PROCÉDÉ DE PRÉPARATION DE POUDRE D'OXYDE DE TUNGSTÈNE/GADOLINIUM À STRUCTURE CŒUR-ÉCORCE POUR LA PROTECTION CONTRE LES RAYONS X ET γ - Google Patents
PROCÉDÉ DE PRÉPARATION DE POUDRE D'OXYDE DE TUNGSTÈNE/GADOLINIUM À STRUCTURE CŒUR-ÉCORCE POUR LA PROTECTION CONTRE LES RAYONS X ET γ Download PDFInfo
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- WO2022166152A1 WO2022166152A1 PCT/CN2021/112700 CN2021112700W WO2022166152A1 WO 2022166152 A1 WO2022166152 A1 WO 2022166152A1 CN 2021112700 W CN2021112700 W CN 2021112700W WO 2022166152 A1 WO2022166152 A1 WO 2022166152A1
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- tungsten
- core
- powder
- gadolinium oxide
- oxide powder
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 36
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000010937 tungsten Substances 0.000 title claims abstract description 25
- 229910001938 gadolinium oxide Inorganic materials 0.000 title claims abstract description 23
- 229940075613 gadolinium oxide Drugs 0.000 title claims abstract description 23
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 22
- 230000005251 gamma ray Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 33
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical class NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 15
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 4
- 239000007853 buffer solution Substances 0.000 claims abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 8
- 239000007983 Tris buffer Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000872 buffer Substances 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract description 16
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000002464 physical blending Methods 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 abstract 1
- 229920001690 polydopamine Polymers 0.000 description 24
- 229960003638 dopamine Drugs 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 241000237536 Mytilus edulis Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- -1 gadolinium ions Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000020638 mussel Nutrition 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000011257 shell material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
Definitions
- the invention relates to the field of preparation of radiation protection materials, in particular to a preparation method of core-shell structure tungsten/gadolinium oxide powder for X, gamma ray protection.
- Radiation protection materials are mainly divided into two types: lead-containing materials and lead-free materials.
- Lead is mainly based on lead.
- the protective effect is excellent, it is toxic, has poor strength and has a large scattering of low-energy X-rays.
- Lead-free materials mainly include composite materials made of rare earth elements and heavy metal compounds such as tin, tungsten, and bismuth, which have excellent protective effects and are lightweight and safe.
- Micro-nano core-shell materials with special structures have attracted extensive attention in recent years.
- Composite particles with different core-shell microstructures have unique physical and chemical properties, which also lead to their broad application prospects in many fields such as optics, electronics, catalysis, biology, and radiation.
- the core-shell structure radiation protection material can cooperate in protection, eliminating the weak protection area and effectively absorbing the secondary radiation generated by the radiation.
- the preparation methods of core-shell structures mainly include template method, precipitation method, hydrothermal synthesis method, spray drying method, layer-by-layer self-assembly technology, etc. Li et al.
- the purpose of the present invention is to provide a preparation method of core-shell structure tungsten/gadolinium oxide powder for X, ⁇ -ray protection in order to overcome the above-mentioned defects of the prior art.
- the invention provides a preparation method of core-shell structure tungsten/gadolinium oxide powder for X, ⁇ -ray protection, the method comprises the following steps:
- step (2) adding the W@PDA obtained in step (1) into the gadolinium nitrate solution, stirring, filtering, and calcining at high temperature to obtain the core-shell structure W@Gd 2 O 3 powder.
- the concentration of the solution should be controlled at 1.5-2.5g/L.
- the main reason is that when the DA concentration is lower than 1.5g/L, only a small amount of PDA particles are deposited on the surface of W.
- the DA concentration is 1.5-2.5g/L, a PDA film is formed on the surface of the W powder.
- the concentration of DA was higher than 2.5 g/L, larger PDA particles were formed by self-polymerization on the surface of W powder due to the high concentration of DA, which was not conducive to the subsequent adsorption of gadolinium ions.
- tris buffer should be added to the system to adjust the pH of the solution to 8-9, because dopamine can self-polymerize into polydopamine under weak alkaline and aerobic conditions.
- Polydopamine has extraordinary surface activity and adhesion on the surface of different substances, which can provide a platform for the secondary functionalization of materials.
- step (1) needs to be stirred under an electric stirrer for 18-24h.
- step (1) water and ethanol need to be washed 2-3 times respectively.
- step (1) the specific conditions for drying described in step (1) are not specifically limited, as long as the purpose of drying the sample can be achieved.
- the concentration of the solution should be controlled at 0.3-0.5M/L. Because when the Gd + concentration is 0.02 M/L, the surface of W is coated with a small amount and sparse nano-dot-like Gd 2 O 3 particles. When the Gd + concentration increases to 0.1M/L, the Gd 2 O 3 nanoparticles on the W surface become larger and larger, which is due to the increase of Gd + concentration. The Gd 2 O 3 nanoparticles combine with each other to form larger Gd 2 O 3 particles. When the Gd + concentration increased to 0.2 M/L, the Gd 2 O 3 nanoparticles on the W surface became larger and denser.
- the Gd 2 O 3 nanoparticles on the W surface were combined with each other to form the core-shell structured W@Gd 2 O 3 .
- the Gd2O3 nanoparticles on the W surface did not change much compared to when the Gd + concentration was 0.3M/L, which was due to the chelation of Gd + by polydopamine on the W surface .
- the synergistic effect has reached saturation at Gd + concentration of 0.3M/L, and excessive concentration will cause waste.
- step (2) is not specifically limited, and only needs to be magnetically stirred for a certain period of time.
- the high-temperature calcination in step (2) needs to be calcined in a muffle furnace at 800-1000° C. for 2-3 hours, and the heating temperature is 2-4° C./min.
- the calcination in step (2) of the present invention is carried out in a protective gas, and the protective gas includes nitrogen or an inert gas, and the inert gas can be argon, helium, etc.
- the protective gas includes nitrogen or an inert gas
- the inert gas can be argon, helium, etc.
- the invention does not make any special limitation on this.
- the preparation method of the core-shell structure tungsten/gadolinium oxide powder for X, ⁇ -ray protection of the present invention comprises the following steps:
- step (2) adding the W@PDA obtained in step (1) into the gadolinium nitrate solution with a concentration of 0.3-0.5M/L, magnetic stirring for a certain period of time, filtration and separation, drying, and then the prepared sample was heated at 800-1000 It was calcined at high temperature under nitrogen for 2-3h (the heating rate was 2-4°C/min), and finally the core-shell structure W@Gd 2 O 3 powder was obtained.
- the core-shell structure W@Gd 2 O 3 powder prepared by the above preferred technical solution has a core-shell structure that can play a synergistic protective role in radiation protection and eliminates weak protection. At the same time, the secondary radiation generated by the radiation is effectively absorbed.
- the present invention at least has the following beneficial effects:
- the present invention firstly utilizes that dopamine can self-polymerize into polydopamine under weak alkaline and aerobic conditions, and polydopamine has extraordinary adhesion on the surfaces of different substances, and can successfully coat tungsten to obtain W@PDA.
- the surface of PDA contains a large number of polar groups such as phenolic hydroxyl groups and amine groups, which provide abundant active sites for complexing various metal ions, which can effectively chelate Gd + in gadolinium nitrate solution.
- PDA forms a nitrogen-doped carbon layer attached to the surface of tungsten, and the W@PDA chelated with Gd + transforms into W@Gd 2 O 3 .
- Example 1 is a scanning electron microscope image of the core-shell structure tungsten/gadolinium oxide powder prepared in Example 1.
- the present embodiment provides a preparation method of core-shell structure tungsten/gadolinium oxide powder for X, ⁇ -ray protection, and the method includes the following steps:
- step (2) The W@PDA obtained in step (1) was added to a solution of gadolinium nitrate with a concentration of 0.3M/L, and after magnetic stirring for 2h, filtration and separation were performed, and dried at 80°C for 5h, and then the prepared sample was heated at 800°C.
- the core-shell structure W@Gd 2 O 3 powder was finally obtained by calcining at high temperature under nitrogen for 2 h (heating rate of 2 °C/min).
- the W@Gd 2 O 3 powder prepared in this example was scanned by SEM, and the obtained photo is shown in Figure 1. It can be seen from the figure that a PDA film is formed on the surface of the W powder.
- the present embodiment provides a preparation method of core-shell structure tungsten/gadolinium oxide powder for X, ⁇ -ray protection, and the method includes the following steps:
- step (2) The W@PDA obtained in step (1) was added to a gadolinium nitrate solution with a concentration of 0.35M/L, and after magnetic stirring for 3h, filtration and separation were performed, and dried at 60°C for 8h, and then the prepared sample was heated at 900 °C.
- the core-shell structure W@Gd 2 O 3 powder was finally obtained by calcining at high temperature under nitrogen for 2.5 h (heating rate of 3 °C/min).
- the present embodiment provides a preparation method of core-shell structure tungsten/gadolinium oxide powder for X, ⁇ -ray protection, and the method includes the following steps:
- step (2) The W@PDA obtained in step (1) was added to a gadolinium nitrate solution with a concentration of 0.4M/L, magnetically stirred for 2.5h, filtered and separated, dried at 70°C for 6h, and then the prepared sample was placed in The core-shell structure W@Gd 2 O 3 powder was finally obtained by calcining at 1000 °C under nitrogen for 3 h (the heating rate was 4 °C/min).
Abstract
Procédé de préparation de poudre d'oxyde de tungstène/gadolinium à structure cœur-écorce pour la protection contre les rayons X et γ, comprenant : (1) la préparation d'une solution de sel de dopamine, l'ajout d'une solution tampon pour ajuster une valeur de pH, l'ajout de la poudre de tungstène, l'agitation, le filtrage, le lavage et le séchage pour obtenir du W@PDA ; et (2) l'ajout du W@PDA obtenu à l'étape (1) à une solution de nitrate de gadolinium, l'agitation, le filtrage et la réalisation d'une calcination à haute température pour obtenir une poudre de W@Gd2O3 à structure à cœur-écorce. Par comparaison avec un seul mode de mélange physique de métal, une structure cœur-écorce d'oxyde de tungstène/gadolinium dans la nanopoudre préparée peut jouer un rôle protecteur synergique dans la protection contre les rayonnements, peut absorber efficacement un rayonnement secondaire généré par un rayonnement tout en éliminant une zone de protection faible, présente des caractéristiques sans fil et légères, et est utilisé pour la protection contre les rayons X et γ.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110179938.4 | 2021-02-08 | ||
| CN202110179938.4A CN112846173A (zh) | 2021-02-08 | 2021-02-08 | 一种X，γ射线防护用核壳结构钨/氧化钆粉末的制备方法 |
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| Publication Number | Publication Date |
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| WO2022166152A1 true WO2022166152A1 (fr) | 2022-08-11 |
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| PCT/CN2021/112700 WO2022166152A1 (fr) | 2021-02-08 | 2021-08-16 | PROCÉDÉ DE PRÉPARATION DE POUDRE D'OXYDE DE TUNGSTÈNE/GADOLINIUM À STRUCTURE CŒUR-ÉCORCE POUR LA PROTECTION CONTRE LES RAYONS X ET γ |
Country Status (2)
| Country | Link |
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| CN (1) | CN112846173A (fr) |
| WO (1) | WO2022166152A1 (fr) |
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| CN112831078B (zh) * | 2021-02-08 | 2022-08-16 | 南通大学 | 一种X，γ射线防护用核壳结构钨/氧化钆PVC压延材料的制备方法 |
| CN112831855B (zh) * | 2021-02-08 | 2022-05-31 | 南通大学 | 一种X，γ射线防护用核壳结构钨/氧化钆功能纤维的制备方法 |
| CN112846173A (zh) * | 2021-02-08 | 2021-05-28 | 南通大学 | 一种X，γ射线防护用核壳结构钨/氧化钆粉末的制备方法 |
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