CN101891253B - Preparation method of monodisperse micron-sized uranium oxide particles - Google Patents
Preparation method of monodisperse micron-sized uranium oxide particles Download PDFInfo
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- CN101891253B CN101891253B CN2010102278193A CN201010227819A CN101891253B CN 101891253 B CN101891253 B CN 101891253B CN 2010102278193 A CN2010102278193 A CN 2010102278193A CN 201010227819 A CN201010227819 A CN 201010227819A CN 101891253 B CN101891253 B CN 101891253B
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- 239000002245 particle Substances 0.000 title claims abstract description 53
- WZECUPJJEIXUKY-UHFFFAOYSA-N [O-2].[O-2].[O-2].[U+6] Chemical compound [O-2].[O-2].[O-2].[U+6] WZECUPJJEIXUKY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910000439 uranium oxide Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title description 16
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000012159 carrier gas Substances 0.000 claims abstract description 25
- 229910002007 uranyl nitrate Inorganic materials 0.000 claims abstract description 16
- 239000000443 aerosol Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000004479 aerosol dispenser Substances 0.000 claims description 11
- 230000004907 flux Effects 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 5
- 239000007921 spray Substances 0.000 abstract description 2
- 230000005611 electricity Effects 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- 229910052770 Uranium Inorganic materials 0.000 description 6
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 229910052778 Plutonium Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000012925 reference material Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IQWPWKFTJFECBS-UHFFFAOYSA-N O=[U](=O)O[U](=O)(=O)O[U](=O)=O Chemical compound O=[U](=O)O[U](=O)(=O)O[U](=O)=O IQWPWKFTJFECBS-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- SHZGCJCMOBCMKK-KGJVWPDLSA-N beta-L-fucose Chemical compound C[C@@H]1O[C@H](O)[C@@H](O)[C@H](O)[C@@H]1O SHZGCJCMOBCMKK-KGJVWPDLSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001149 thermolysis Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- PSPBAKLTRUOTFX-UHFFFAOYSA-N [O-2].[Pu+4].[U+6].[O-2].[O-2].[O-2].[O-2] Chemical compound [O-2].[Pu+4].[U+6].[O-2].[O-2].[O-2].[O-2] PSPBAKLTRUOTFX-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- FLZVXSCVMGKKAK-UHFFFAOYSA-N fluoro hypofluorite uranium Chemical class [U].FOF FLZVXSCVMGKKAK-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- WJWSFWHDKPKKES-UHFFFAOYSA-N plutonium uranium Chemical compound [U].[Pu] WJWSFWHDKPKKES-UHFFFAOYSA-N 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000012358 sourcing Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 description 1
- 229910003452 thorium oxide Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing monodisperse micron-sized uranium oxide particles by a sol spray thermal decomposition method. The method comprises the steps of forming a monodisperse aerosol from a uranyl nitrate solution by using a vibrating-hole aerosol generator; drying and removing static electricity to form uranyl nitrate solid particles; forming monodisperse uranium oxide particles through high-temperature thermal decomposition; cooling and collecting. Preheating a carrier gas at the rear end of the neutralizer to enable the temperature of the carrier gas to reach about 70-80 ℃; the carrier gas flow is 35-45L/min; when high temperature thermal decomposition is carried out, a muffle furnace is adopted for direct heating. The technical scheme provided by the invention is relatively simple and convenient, and ensures the safety in the operation process.
Description
Technical field
The invention belongs to from fluent material and adopt physics and chemical process to prepare the method for particulate, be specifically related to a kind of method that adopts the colloidal sol spray heating decomposition to prepare monodisperse micron-sized uranium oxide particle.
Background technology
Single disperse also to cry monodisperse system or single distribution, typically refer to the dispersion system of the single and Unusually narrow particle size distribution of disperse phase composition.
Important effect is being brought into play in the isotopic analysis of uranium particulate in the nuclear safeguards environmental monitoring.Be precision and the accuracy that guarantees accurately to measure uranium isotope ratio in the single particulate; And analytic process carried out quality monitoring; Experimentation is assessed, just need be simulated as much as possible and come the preparation work standard from the character such as chemical composition, physical aspect and geometrical dimension of uranium particulate in the environmental sample.Environment wipe samples particle diameter is studied needed standard substance diameter of particle and also should and should be possessed monodispersity in this scope as carrying out nuclear safeguards in micron and sub-micrometer range.
At home, though a large amount of scholars are arranged in the research of being engaged in the particulate preparation method, the preparation of uranium oxide particle, also few people relate at present, also do not have relevant bibliographical information.
Abroad, as far back as 1971, people such as Knudsen.Irving E just invented UF
6Be converted into than small particle UO
2Method (Knudsen.Irving E; Randall.Clinton C.Production of sizedparticles of uranium oxides and uranium oxyfluorides [P] .United States:3978194; 1976-8-31): in fluidized-bed reactor, with UF
6Mix with water vapour, hydrogen, carry out initial reaction, form the oxide fine particle of the uranium of various particle diameters; In cyclonic separator, particle size is separated then; To circulate once more than small particle, will be transported in the next stage fluidized-bed reactor, form comparatively coarse UO than big particulate
2Particulate, its size distribution is in the scope of 50～300 μ m.Subsequently; In 1977; Bezzi.Giovanni utilizes sedimentary method to prepare oxide fine particle and carbonaceous three's blended oxide fine particle (Bezzi.Giovanni, Facchini.Alessandro, the Martignani.Giovanni etal.Production of microspheres of thorium oxide of carbonaceous thorium, uranium, plutonium; Uranium oxide and plutonium oxide and their mixtures containing carbon [P] .United States:4202793; 1980-5-13), but its preparation method is still comparatively loaded down with trivial details, and in its patent, does not also reveal the information of relevant particulate morphology.By 2000; People such as N.Erdmann utilize colloidal sol spraying pyrolysated method (N.Erdmann; M.Betti, O.Stetzer et al.Production of monodisperse uranium oxide particles andtheir characterization by scanning electron microscopy and secondary ion massspectrometry [J] .Spectrochimica Acta Part B, 2000; 55:1565-1575); Success prepared single uranium oxide particle that disperses that particle diameter is 1 μ m, this method is comparatively ripe, but also has certain problem for the big particulate of preparation.2003; People such as Zitouni Ould-Dada utilize colloidal sol spraying pyrolysated method equally; The particulate that has prepared accurate monodispersed uranium oxide, diameter of particle are distributed in 0.13～1.37 mu m range, can't satisfy monodispersed requirement (Zitouni Ould-Dada; George Shaw; Rob Kinnersley.Production of radioactive particles for use in environmentalstudies [J] .Journal of Environmental Radioactivity, 2003,70:177-191).By 2005; People such as Y.J.Park utilize aerosol dispenser to prepare particulate (Y.J.Park; M.H.Lee; H.Y.Pyo etal.The preparation of uranium-adsorbed silica particles as a reference material for thefission track analysis [J] .Nuclear Instruments and Methods in Physics Research A; 2005,545:493-502): after obtaining aerosol, having formed particle diameter through gravity settling, calcination is the SiO of 5,10,15 and 20 μ m
2Particulate has wherein adsorbed abundance and is 5%
235U, with the reference material that is used for analyzing as fission track, though the microparticulate property of this method preparation is better, particle diameter still is bigger than normal than environmental sample.In 2006; People such as Ruth Kips have studied novel method (the Ruth Kips of a cover preparation uranium oxide particle; Ann Leenaers, Gabriele Tamborini et al.Characterization of UraniumParticles Produced by Hydrolysis of UF
6Using SEM and SIMS [J] .Microscopy andMicroanalysis, 2007,13:156-164): they are through utilizing UF
6Used reference material when detecting as environmental sampling through the particulate that generates after the hydrolysis; And the relative air humidity of reaction chamber is controlled the morphology parameter of particulate when regulating hydrolysis, but mostly particulate is spherical or floss, and particle diameter mainly concentrates between 0.5～1.5 μ m, and monodispersity is relatively poor.2010; People such as Y.Ranebo utilize people's such as N.Erdmann in 2000 colloidal sol spraying pyrolysated method (Y.Ranebo, N.Niagolova, N.Erdmann etal.Production and Characterization of Monodisperse Plutonium; Uranium; And MixedUranium-Plutonium Particles for Nuclear Safeguard Applications [J] .Anal.Chem, 2010,82:4055-4062); Ordering parameter, the list of having prepared 1 μ m disperses plutonium oxide particulate and uranium plutonium mixed oxide particulate.
People such as N.Erdmann in 2000 and the disclosed technology of utilizing colloidal sol spraying pyrolysated method to prepare monodisperse micron-sized uranium (plutonium) oxide fine particle of people such as Y.Ranebo in 2010 all are the technology of German transuranium institute (ITU) research and development.But comparatively speaking, ITU provides equipment more complicated in the technical scheme, for example, preheats device in the inner increase of vibration hole aerosol dispenser carrier gas; In carrier gas carrier band process, select to have increased by one tunnel auxiliary gas at particulate; In the particulate thermal decomposition process, ITU adopts three retort furnace series connection, carries out cascade raising temperature.
Technical scheme
(1) goal of the invention
To the defective that prior art exists, the present invention aims to provide the fairly simple method for preparing submicron to micron order list dispersion uranium oxide particle of a kind of required equipment.
(2) summary of the invention
A kind of method for preparing monodisperse micron-sized uranium oxide particle comprises the steps:
Step 1 adopts vibration hole aerosol dispenser that uranyl nitrate solution is formed monodisperse aerosol;
Step 2, monodisperse aerosol destatics through neutralizer with carrier gas, and drying forms the uranyl nitrate solia particle;
Step 3, the uranyl nitrate solia particle decomposes through elevated temperature heat, forms single uranium oxide particle that disperses;
Step 4, collect single uranium oxide particle cooling back that disperses.
Key is: in step 2, in the neutralizer rear end carrier gas is preheated, the carrier gas temperature is reached about 70～80 ℃; Carrier gas flux is 35～45L/min.
In step 3, adopt a retort furnace direct heating, temperature is set at 650～750 ℃.
In order to solve the problem that vibration hole aerosol dispenser vibratory orifice plate is corroded, said vibratory orifice plate is that stainless material is processed.
(3) invention effect
Technical scheme provided by the present invention is compared with the disclosed scheme of ITU, is chosen in the neutralizer rear end carrier gas is preheated, and in advance the mode that carrier gas is heated is compared in vibration aerosol dispenser inside, hole with ITU, and is simple and should operate.In carrier gas carrier band process, ITU has selected to have increased by one tunnel auxiliary gas, and adopts bigger carrier gas flux (55L/min) at particulate; The present invention simplifies it, has cancelled auxiliary gas, and uses less relatively carrier gas flux.In addition, in the particulate thermal decomposition process, ITU adopts three retort furnace series connection, and carries out cascade raising temperature (150,300,800 ℃); The present invention is reduced to it and only uses a retort furnace direct heating.Therefore, technical scheme provided by the present invention is relatively simple, convenient, has guaranteed the security in the operating process.
Description of drawings
Fig. 1 is the monodisperse micron-sized uranium oxide particle preparing method's that carries of the present invention a schema;
Fig. 2 is the scanning electron microscope image of the monodisperse micron-sized uranium oxide particle of embodiment 1 preparation;
Fig. 3 is the energy spectrum analysis figure of the monodisperse micron-sized uranium oxide particle of embodiment 1 preparation;
Fig. 4 is the particle size distribution figure of the monodisperse micron-sized uranium oxide particle of embodiment 1 preparation.
Embodiment
Below in conjunction with accompanying drawing technical scheme provided by the present invention is done further to set forth.
Embodiment 1
Present embodiment is an example to prepare the single dispersion of 2 μ m uranium oxide particle.The VOAG-3450 type vibration hole aerosol dispenser that uses U.S. Technical Sourcing Internation to produce is designed to stainless material again with its vibratory orifice plate and processes.The uranous uranic oxide standard reagent
235U/
238The U nominal value is 7.25 * 10
-3
Before preparation, need preparation uranyl nitrate solution solution.Its collocation method is, takes by weighing the uranous uranic oxide powder about 0.098g, puts into polytetrafluoroethylene beaker; Add about the nitric acid 15ml of 1mol/L; Evaporating solvent adds deionized water at last and is settled to 25ml to remaining about 2ml then, and promptly having obtained uranyl nitrate concentration is 5.5 * 10
-3The solution of g/ml adopts 1: 1 (volume ratio) blended Virahol and deionized water as solvent above-mentioned strong solution to be carried out stepwise dilution, obtains 3.2 * 10
-4The uranyl nitrate solution of g/ml.
It is following that single dispersion uranium oxide particle prepares process:
Step 1 is vibrated hole aerosol dispenser vibrational frequency and is set to 55.8kHz, and carrier gas flux is 40L/min, packs in the sampling injector of aerosol dispenser with above-mentioned uranyl nitrate solution, via producer, forms monodisperse aerosol.
Step 2, monodisperse aerosol are removed the aerosol droplets surface electric charge through neutralizer.In the neutralizer rear end carrier gas is preheated subsequently, the heating zone temperature is set to 120 ℃, and carrier gas is warming up to about 79～80 ℃, makes the solvent evaporation in the aerosol droplets, forms the solia particle of uranyl nitrate.
Step 3, the uranyl nitrate solia particle decomposes through 1 retort furnace elevated temperature heat, and the Heating temperature of retort furnace is 690～710 ℃, and the final list that forms disperses uranium oxide particle.
Step 4 is set at 15 ℃ with temperature of cooling water, and the high temperature uranium oxide particle after the thermolysis is collected on the nucleopore membranes after cooling, about about 30 minutes of collection time, and promptly having obtained particle diameter is single uranium oxide particle that disperses of 2 μ m.
Like Fig. 2,, confirm the form of preparation particulate through the particulate on the SEM direct viewing nucleopore membranes.In ability spectrogram (Fig. 3), do not find the spectrum peak of N, UO is described
2(NO
3)
2Thermolysis is more complete, and prepared particulate is an oxide form; C peak in all spectrograms causes by contained C in nucleopore membranes (polyester) material, the spectrum peak of Au, Pd be since before detecting on nucleopore membranes and particulate due to the deposited gold, the Al peak is that the sample platform of scanning electronic microscope matrix produces.The particle diameter of each particulate that provides according to electronic microscope photos software through the complicate statistics arrangement, obtains the result of size distribution, and is as shown in Figure 4, explains that this uranium oxide particle satisfies monodispersity.
Embodiment 2
Operation steps is with embodiment 1, and difference is: in the step 1, vibrate hole aerosol dispenser vibrational frequency and be set to 57.2kHz, carrier gas flux is 45L/min; In the step 2, the heating zone temperature is set to 115 ℃, makes carrier gas be warming up to about 75～77 ℃; In the step 3, the uranyl nitrate solia particle decomposes through the retort furnace elevated temperature heat, and the Heating temperature of retort furnace is 740～750 ℃.
Embodiment 3
Operation steps is with embodiment 1, and difference is: in the step 1, carrier gas flux is 35L/min; In the step 2, the heating zone temperature is set to 110 ℃, makes carrier gas be warming up to about 70～72 ℃; In the step 3, the uranyl nitrate solia particle decomposes through the retort furnace elevated temperature heat, and the Heating temperature of retort furnace is 650～670 ℃.
Obviously those skilled in the art can carry out various modifications and modification and not break away from the spirit and scope of the present invention the present invention.Like this, if of the present invention these revise and modification belongs in the scope of its equivalent technologies of claim of the present invention, then the present invention also is intended to comprise these modifications and modification.
Claims (2)
1. a method for preparing monodisperse micron-sized uranium oxide particle comprises the steps:
Step 1 adopts vibration hole aerosol dispenser that uranyl nitrate solution is formed monodisperse aerosol;
Step 2, monodisperse aerosol destatics through neutralizer with carrier gas, and drying forms the uranyl nitrate solia particle;
Step 3, the uranyl nitrate solia particle decomposes through elevated temperature heat, forms single uranium oxide particle that disperses;
Step 4, collect single uranium oxide particle cooling back that disperses;
It is characterized in that: in step 2, carrier gas is preheated, the carrier gas temperature is reached about 70～80 ℃ in the neutralizer rear end; Carrier gas flux is 35～45L/min;
In step 3, adopt a retort furnace direct heating, temperature is set at 650～750 ℃.
2. the method for preparing monodisperse micron-sized uranium oxide particle according to claim 1 is characterized in that: the vibratory orifice plate of said vibration hole aerosol dispenser is that stainless material is processed.
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| CN104302813B (en) * | 2011-12-21 | 2017-07-21 | 斯坦福设备有限公司 | Aerosol generator |
| CN103936076B (en) * | 2014-01-16 | 2015-11-25 | 中国科学院高能物理研究所 | Uranium oxide micron ball and preparation method thereof |
| FR3037331B1 (en) * | 2015-06-12 | 2019-09-13 | Orano Cycle | INSTALLATION, THERMAL DENITRATING METHOD, USE OF SUCH A INSTALLATION AND PRODUCT OBTAINED BY SUCH A METHOD |
| CN107715809B (en) * | 2017-11-28 | 2024-04-26 | 中国工程物理研究院核物理与化学研究所 | Plutonium aerosol particle generation device |
| CN113753956B (en) * | 2021-09-02 | 2022-11-01 | 中国原子能科学研究院 | Micron-sized monodisperse uranium-thorium mixed particle and preparation method and preparation system thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1924594A1 (en) * | 1969-05-14 | 1970-11-26 | Nukem Gmbh | Device for precipitating uranium from aqueous solution |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1924594A1 (en) * | 1969-05-14 | 1970-11-26 | Nukem Gmbh | Device for precipitating uranium from aqueous solution |
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