WO2022166142A1 - PROCÉDÉ DE PRÉPARATION D'UN MATÉRIAU CALANDRÉ EN PVC D'OXYDE DE TUNGSTÈNE/GADOLINIUM À STRUCTURE CŒUR-ÉCORCE POUR LA PROTECTION CONTRE LES RAYONS X ET γ - Google Patents
PROCÉDÉ DE PRÉPARATION D'UN MATÉRIAU CALANDRÉ EN PVC D'OXYDE DE TUNGSTÈNE/GADOLINIUM À STRUCTURE CŒUR-ÉCORCE POUR LA PROTECTION CONTRE LES RAYONS X ET γ Download PDFInfo
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- WO2022166142A1 WO2022166142A1 PCT/CN2021/111436 CN2021111436W WO2022166142A1 WO 2022166142 A1 WO2022166142 A1 WO 2022166142A1 CN 2021111436 W CN2021111436 W CN 2021111436W WO 2022166142 A1 WO2022166142 A1 WO 2022166142A1
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- core
- shell structure
- gadolinium oxide
- tungsten
- structure tungsten
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 122
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 239000010937 tungsten Substances 0.000 title claims abstract description 112
- 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 111
- 229910001938 gadolinium oxide Inorganic materials 0.000 title claims abstract description 110
- 229940075613 gadolinium oxide Drugs 0.000 title claims abstract description 110
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 109
- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000003490 calendering Methods 0.000 title claims abstract description 40
- 230000005251 gamma ray Effects 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000004744 fabric Substances 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 238000007731 hot pressing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 239000011248 coating agent Substances 0.000 claims description 33
- 238000000576 coating method Methods 0.000 claims description 33
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical class NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 28
- 238000005507 spraying Methods 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 22
- 238000005096 rolling process Methods 0.000 claims description 18
- 230000001681 protective effect Effects 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 14
- 229920001721 polyimide Polymers 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 14
- 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 description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 239000007983 Tris buffer Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000007788 liquid Substances 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
- 238000001914 filtration Methods 0.000 claims description 6
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 6
- 239000000872 buffer Substances 0.000 claims description 4
- 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
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract description 16
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 150000002466 imines Chemical class 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 229920000728 polyester Polymers 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 229920001690 polydopamine Polymers 0.000 description 24
- 229960003638 dopamine Drugs 0.000 description 9
- 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
- 238000001125 extrusion Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 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
- 238000000926 separation method 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
- 230000008859 change Effects 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
- 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000001000 micrograph Methods 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
- 238000002464 physical blending Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009993 protective function Effects 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
- C08J7/0423—Coating with two or more layers, where at least one layer of a composition contains a polymer binder with at least one layer of inorganic material and at least one layer of a composition containing a polymer binder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/04—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C09D127/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2427/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0887—Tungsten
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
Definitions
- the application relates to the field of radiation protection, in particular to a preparation method of a core-shell structure tungsten/gadolinium oxide PVC calendering material 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 a core-shell structure tungsten/gadolinium oxide PVC calendering material for X, ⁇ -ray protection in order to overcome the above-mentioned defects in the prior art.
- the invention provides a preparation method of a core-shell structure tungsten/gadolinium oxide PVC calendering material for X, ⁇ -ray protection, the method comprising 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.
- step (3) The core-shell structure tungsten/gadolinium oxide powder obtained in step (2) is uniformly dispersed into absolute ethanol, and stirred evenly to prepare a core-shell structure tungsten/gadolinium oxide solution.
- step (3) The core-shell structure tungsten/gadolinium oxide solution obtained in step (3) is evenly spread on the polyimide film, and hot-pressed to form a core-shell structure tungsten/gadolinium oxide thin skin layer.
- step (2) the core-shell structure tungsten/gadolinium oxide powder obtained in step (2) and the silane coupling agent are uniformly mixed and treated in an ultrasonic generator for a period of time, and the dimethylacetamide solution is added dropwise to continue stirring until the dispersion is uniform, Add PVC resin and continue to stir evenly, heat up to remove part of dimethylacetamide, adjust the viscosity value, and continue stirring for a period of time to obtain functional PVC adhesive coating.
- step (6) adding the PVC glue coating obtained in step (5) to the barrel of the spraying device, spraying on the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) by spraying process, and drying to obtain a functional PVC coating.
- step (7) rolling the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) and the PVC coating obtained in step (6) through a calender roll, so that the core-shell structure tungsten/gadolinium oxide thin layer and functional PVC
- the layer is flat and evenly covered on the surface of the polyimide film to obtain a lead-free light-weight X and ⁇ -ray protective material formed by rolling.
- 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) it is necessary to wash with water and ethanol for 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 powder in step (3) is uniformly dispersed in absolute ethanol, and the mass ratio needs to be controlled to be 1:1 to 1:5.
- step (3) is ultrasonic stirring for 10-20 min.
- the viscosity of the solution in step (3) is 1000-10000 mPa.s.
- step (4) in the hot pressing of step (4), first preheat at 250-270° C. and 0 pressure for 20 minutes, so that the core-shell structure tungsten/gadolinium oxide powder is uniformly heated; the temperature is raised to 285-300° C., Under the mechanical pressure of 25MPa, pressing at constant temperature and pressure for 10-20min, the core-shell structure tungsten/gadolinium oxide powder is melted at high temperature to form a core-shell structure tungsten/gadolinium oxide thin skin layer with a thickness of 50-200 ⁇ m.
- the ultrasonic generator in step (5) needs to be processed for 10-20 minutes.
- the first stirring requires mechanical stirring for 1-2 hours, and the second stirring requires stirring for 20-30 minutes.
- step (5) the temperature increase in step (5) needs to be increased to 50-60°C.
- the viscosity of the PVC adhesive coating in step (5) is 1000-5000 mPa.s.
- the process parameters of spraying described in step (6) are that the amount of liquid applied is 500ml/min ⁇ 800ml/min, the air pressure is 0.3MPa ⁇ 0.7MPa, the diameter of the spray nozzle is 10cm, and the distance between the nozzle and the cloth surface is 15cm, the number of times the spray gun goes back and forth is 30 times/min to 120 times/min; the thickness of the functional PU coating is 0.1 to 0.3 mm.
- the calendering process parameters in step (7) are: the temperature of the upper roll is 80°C to 120°C, the temperature of the middle roll is 70°C to 100°C, the temperature of the lower roll is 60°C to 115°C, the roll distance is 1mm, and the rolling speed is 35°C. ⁇ 50m/min.
- the preparation method of a core-shell structure tungsten/gadolinium oxide PVC calendering material 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, stirring magnetically for a certain period of time, filtering and separating, drying, and then the prepared sample was heated at 800-1000
- the core-shell structure W@Gd 2 O 3 powder was finally obtained by calcining at high temperature under nitrogen for 2-3 h (heating rate of 2-4 °C/min).
- step (3) uniformly dispersing the core-shell structure tungsten/gadolinium oxide powder obtained in step (2) into anhydrous ethanol, controlling the mass ratio to be 1:1-1:5, and ultrasonically stirring for 10-20min, to prepare a solution with a viscosity of 1000 ⁇ 10000mPa.s core-shell tungsten/gadolinium oxide solution.
- the core-shell structure tungsten/gadolinium oxide solution obtained in step (3) is evenly spread on the polyimide film.
- the hot press preheat at 250-270° C. and 0 pressure for 20 minutes to make the core-shell
- the structured tungsten/gadolinium oxide powder is uniformly heated; the temperature is raised to 285 ⁇ 300°C, under the mechanical pressure of 25MPa, pressed at constant temperature and constant pressure for 10 ⁇ 20min, the core-shell structured tungsten/gadolinium oxide powder is melted at high temperature to form a core-shell Structural tungsten/gadolinium oxide thin skin layer with a thickness of 50-200 ⁇ m.
- step (2) The core-shell structure tungsten/gadolinium oxide powder obtained in step (2) and the silane coupling agent are uniformly mixed, and then treated in an ultrasonic generator for 10-20 min, dimethylacetamide solution is added dropwise, and mechanical stirring is performed for 1- 2h, add PVC resin and continue to stir evenly, raise the temperature to 50-60°C to remove part of dimethylacetamide, adjust the viscosity value, and continue stirring for 20-30min to obtain functional PVC adhesive coating with a viscosity of 1000-5000mPa.s.
- step (6) adding the PVC glue coating obtained in step (5) to the barrel of the spraying device, and spraying onto the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) by a spraying process, and the process parameter of spraying is that the amount of liquid applied is 500ml/min ⁇ 800ml/min, the air pressure is 0.3MPa ⁇ 0.7MPa, the diameter of the spray nozzle is 10cm, the distance between the nozzle and the cloth surface is 15cm, and the number of times the spray gun goes back and forth is 30 times/min ⁇ 120 times/min; after drying
- the functional PVC coating is prepared, and the thickness is 0.1-0.3 mm.
- step (7) rolling the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) and the PVC coating obtained in step (6) through a calender roll, so that the core-shell structure tungsten/gadolinium oxide thin layer and functional PVC
- the layer is flat and evenly attached to the surface of the polyimide film.
- the calendering process parameters are: the temperature of the upper roll is 80°C ⁇ 120°C, the temperature of the middle roll is 70°C ⁇ 100°C, the temperature of the lower roll is 60°C ⁇ 115°C, and the roll distance is 1mm. , the rolling speed is 35-50 m/min, and the lead-free light-weight X and ⁇ -ray protective materials are obtained by rolling.
- 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 .
- Fig. 1 is the scanning electron microscope image of a kind of X, ⁇ -ray protective function powder prepared in Example 1.
- the present embodiment provides a preparation method of a core-shell structure tungsten/gadolinium oxide PVC calendering material 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).
- step (3) The core-shell tungsten/gadolinium oxide powder obtained in step (2) is uniformly dispersed in absolute ethanol, the mass ratio is controlled to be 1:2, and ultrasonically stirred for 10 minutes to prepare a core-shell with a solution viscosity of 5000 mPa.s Structural tungsten/gadolinium oxide solution.
- step (3) Apply the core-shell tungsten/gadolinium oxide solution obtained in step (3) evenly on the polyimide film.
- the hot press preheat at 250° C. and 0 pressure for 20 minutes to make the core-shell structure tungsten /Gadolinium oxide powder is uniformly heated; raise the temperature to 285°C, press at a constant temperature and pressure for 10min under the mechanical pressure of 25MPa, the core-shell structure tungsten/gadolinium oxide powder is melted at high temperature to form a core-shell structure tungsten/gadolinium oxide thin skin layer with a thickness of 50 ⁇ m.
- step (6) adding the PVC glue coating obtained in step (5) to the barrel of the spraying device, and spraying onto the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) by a spraying process, and the process parameter of spraying is that the amount of liquid applied is 500ml/min, the air pressure is 0.3MPa, the diameter of the nozzle of the spray head is 10cm, the distance between the nozzle and the cloth surface is 15cm, and the number of round trips of the spray gun is 30 times/min; after drying, a functional PVC coating with a thickness of 0.1mm is obtained.
- step (7) rolling the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) and the PVC coating obtained in step (6) through a calender roll, so that the core-shell structure tungsten/gadolinium oxide thin layer and functional PVC
- the layer is flat and evenly attached to the surface of the polyimide film.
- the calendering process parameters are: the temperature of the upper roll is 80°C, the temperature of the middle roll is 70°C, the temperature of the lower roll is 60°C, the roll distance is 1mm, and the calendering speed is 35m/min.
- a lead-free light-weight X and ⁇ -ray protective material is obtained by rolling.
- 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 a core-shell structure tungsten/gadolinium oxide PVC calendering material 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 carried out, 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).
- step (3) The core-shell tungsten/gadolinium oxide powder obtained in step (2) is uniformly dispersed into absolute ethanol, the mass ratio is controlled to be 1:3, and ultrasonically stirred for 15 minutes to prepare a core-shell with a solution viscosity of 7000 mPa.s Structural tungsten/gadolinium oxide solution.
- step (3) Apply the core-shell tungsten/gadolinium oxide solution obtained in step (3) evenly on the polyimide film.
- the hot press preheat for 20 minutes at 260° C. and 0 pressure to make the core-shell structure tungsten /Gadolinium oxide powder is heated evenly; the temperature is raised to 290°C, under the mechanical pressure of 25MPa, press at constant temperature and pressure for 15min, the core-shell structure tungsten/gadolinium oxide powder is melted at high temperature to form a core-shell structure tungsten/gadolinium oxide thin skin layer with a thickness of 100 ⁇ m.
- step (2) The core-shell structured tungsten/gadolinium oxide powder obtained in step (2) and the silane coupling agent are uniformly mixed, and then treated in an ultrasonic generator for 15 minutes, dimethylacetamide solution is added dropwise, mechanically stirred for 1.5 hours, and added
- the PVC resin continued to be stirred evenly, the temperature was raised to 55° C. to remove part of the dimethylacetamide, the viscosity value was adjusted, and the stirring was continued for 25 minutes to obtain a functional PVC adhesive coating with a viscosity of 3000 mPa.s.
- step (6) adding the PVC glue coating obtained in step (5) to the barrel of the spraying device, and spraying onto the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) by a spraying process, and the process parameter of spraying is that the amount of liquid applied is 700ml/min, the air pressure is 0.5MPa, the diameter of the nozzle of the spray head is 10cm, the distance between the nozzle and the cloth surface is 15cm, and the number of times the spray gun goes back and forth is 80 times/min; after drying, a functional PVC coating with a thickness of 0.2mm is obtained.
- the layer is flat and evenly attached to the surface of the polyimide film.
- the calendering process parameters are: the temperature of the upper roll is 100 °C, the temperature of the middle roll is 80 °C, the temperature of the lower roll is 80 °C, the roll distance is 1 mm, and the rolling speed is 40 m/min.
- the present embodiment provides a preparation method of a core-shell structure tungsten/gadolinium oxide PVC calendering material 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).
- step (3) The core-shell tungsten/gadolinium oxide powder obtained in step (2) is uniformly dispersed into absolute ethanol, the mass ratio is controlled to be 1:4, and ultrasonically stirred for 20 minutes to prepare a core-shell with a solution viscosity of 10000 mPa.s Structural tungsten/gadolinium oxide solution.
- the core-shell structure tungsten/gadolinium oxide solution obtained in step (3) is evenly spread on the polyimide film.
- the hot press preheat for 20 minutes at 270°C and 0 pressure to make the core-shell structure tungsten /Gadolinium oxide powder is heated evenly; the temperature is raised to 300°C, under the mechanical pressure of 25MPa, press at constant temperature and pressure for 20min, the core-shell structure tungsten/gadolinium oxide powder is melted at high temperature to form a core-shell structure tungsten/gadolinium oxide thin skin layer with a thickness of 200 ⁇ m.
- step (2) The core-shell structured tungsten/gadolinium oxide powder obtained in step (2) and the silane coupling agent are uniformly mixed, and then treated in an ultrasonic generator for 20 minutes, dimethylacetamide solution is added dropwise, mechanically stirred for 2 hours, and PVC is added The resin continued to be stirred evenly, the temperature was raised to 60° C. to remove part of the dimethylacetamide, the viscosity value was adjusted, and the stirring was continued for 30 minutes to obtain a functional PVC adhesive coating with a viscosity of 5000 mPa.s.
- step (6) adding the PVC glue coating obtained in step (5) to the barrel of the spraying device, and spraying onto the core-shell structure tungsten/gadolinium oxide thin skin layer obtained in step (4) by a spraying process, and the process parameter of spraying is that the amount of liquid applied is 800ml/min, the air pressure is 0.7MPa, the diameter of the nozzle of the spray head is 10cm, the distance between the nozzle and the cloth surface is 15cm, and the number of round trips of the spray gun is 120 times/min; after drying, a functional PVC coating with a thickness of 0.3mm is obtained.
- the layer is flat and evenly attached to the surface of the polyimide film.
- the calendering process parameters are: the temperature of the upper roll is 120 °C, the temperature of the middle roll is 100 °C, the temperature of the lower roll is 115 °C, the roll distance is 1 mm, and the rolling speed is 50 m/min.
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Abstract
Procédé de préparation d'un matériau calandré en PVC d'oxyde de tungstène/gadolinium à structure cœur-écorce pour la protection contre les rayons X et γ, le procédé comprenant : tout d'abord, la préparation d'une poudre d'oxyde de tungstène/gadolinium à structure cœur-écorce ; et la préparation d'un matériau calandré en PVC d'oxyde de tungstène/gadolinium à structure cœur-écorce à partir de la poudre. Un film mince de polyester-imine est uniformément déposé avec la poudre d'oxyde de tungstène/gadolinium à structure cœur-écorce ; la poudre d'oxyde de tungstène/gadolinium à structure cœur-écorce est fondue dans une couche de peau mince d'oxyde de tungstène/gadolinium à structure cœur-écorce lors d'un pressage à chaud à haute température ; la poudre d'oxyde de tungstène/gadolinium à structure cœur-écorce est ajoutée dans une résine de PVC et celle-ci est mélangée uniformément ; le mélange est ensuite pulvérisé sur la surface de la couche de peau mince d'oxyde de tungstène/gadolinium à structure cœur-écorce ; et après séchage, le tissu est soumis à un moulage de calandrage au moyen d'un rouleau d'une machine de calandrage pour préparer un matériau de protection contre les rayons X et γ, sans plomb et léger. Le matériau de protection contre les rayons X et γ peut avoir un effet de protection synergique pour la protection contre les rayonnements, et une zone de protection faible peut être éliminée tandis que le rayonnement secondaire généré par le rayonnement est efficacement absorbé. Le matériau fonctionnel a les caractéristiques d'être exempt de plomb et léger en poids, et présente de bonnes perspectives d'application dans la protection contre les rayons X et γ.
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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 |
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CN113321877B (zh) * | 2021-06-15 | 2023-04-07 | 天津天颐科苑科技有限公司 | 一种可循环利用的柔性防辐射片材及其制备方法 |
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