CN100999408A - Method of preparing UO2 ceramic fuel microsphere - Google Patents
Method of preparing UO2 ceramic fuel microsphere Download PDFInfo
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- CN100999408A CN100999408A CNA2006101652525A CN200610165252A CN100999408A CN 100999408 A CN100999408 A CN 100999408A CN A2006101652525 A CNA2006101652525 A CN A2006101652525A CN 200610165252 A CN200610165252 A CN 200610165252A CN 100999408 A CN100999408 A CN 100999408A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
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Abstract
This invention involves a preparation of UO2 fuel ceramic microspheres method, belongs to nuclear material technology. First mix organic monomer with water to prepare premixed liquid, and then make some solid content of the stable slurry through vibration become droplets, decentralized to a certain temperature oily medium, can also add catalysts N, N, N ', N'- tetramethyl ethylenediamine into oily medium. Small drop under the interfacial tension change into ball; the droplet internal polymer monomer carry out polymerization, thereby solidif to ball. Then after washing, drying, roasting and sintering process and ultimately achieve high yields and with the design requirements of UO2 fuel ceramic microspheres. Because in this method slurry contains less organic matter, so skim is easy, and reduce the tendency of crack when microspheres drying and calcination, thus eliminating the need of nitrate dissolving U3O8 powder and plastic cooking processes.
Description
Technical field
The invention belongs to the nuclear matter technical field, particularly a kind of notes type that congeals into prepares high temperature gas cooled reactor element UO
2The method of ceramic fuel microsphere.
Technical background
The fuel of high temperature gas cooled reactor fuel element is by UO
2Ceramic microsphere constitutes, and diameter is 200～600 microns, and density is greater than 10.40g/cm
3General design requirements is 500 microns of diameters.
UO
2The moulding process of ceramic microsphere is based on sol gel process.Be divided into two kinds of outer gelling, interior gellings.For interior gelation, at first under 5 ℃ low temperature, urea and hexamethylenetetramine (HMTA) are dissolved in uranyl nitrate (UO
2(NO
3)
2) be made into colloidal sol in the solution, be dispersed into then and drip and in heated paraffin oil, solidify, obtain the UO of densification more successively through operations such as washing, drying, roasting, reduction and sintering
2Ceramic microsphere.At present in the world external gelatinizing process that adopt more.The external gelatinizing process process is: uranyl nitrate solution is mixed with PVAC polyvinylalcohol solution, tetrahydrofurfuryl alcohol, and vibration is distributed to the gelling that realizes in the ammoniacal liquor from outer to inner then, obtains UO through ageing, washing, drying, roasting, reduction and sintering
2Ceramic microsphere.Germany HOBEG flow process is with ammonia pre-neutralization uranyl nitrate solution, add PVA and be mixed with colloidal sol, disperse to form drop by vibration, surperficial gelling takes place through ammonia earlier in drop, enter further gelling (Naefe P and Zimmer E.Preparation ofUranium Kernels by an External Gelation Process.Nuclear Technology in the ammoniacal liquor then, 1979,42, p163-171).
At China 10MW high temperature gas cooled reactor (HTR-10) fuel element production period, adopt full gelatinizing process to prepare UO
2Ceramic microsphere: urea is carried out complexing by joining in the uranyl nitrate solution, add PVA, tetrahydrofurfuryl alcohol and HMTA preparation glue then, identical (the Fu X M of subsequent technique with the HOBEG flow process, Liang T X, Tang Y P, Xu Z C, Tang C H.Preparation of UO
2Kernel for HTR-10 fuel element, Journal of Nuclear Science and Technology, 2004,41 (9), 943-948).
The common ground of sol gel process comprises: 1, and nitric acid heating for dissolving U
3O
8Powder obtains uranyl nitrate solution.This process produces environmentally harmful NO gas; 2, add a large amount of organism such as PVA preparation glues, increase the difficulty of liquid waste disposal; 3, ageing, washing process are loaded down with trivial details, and it is many to produce waste liquid amount; 4, owing to add a large amount of organism, dry back microballoon needs slow degreasing to avoid the cracking of microballoon.
Injectiong coagulation shaping technology is a kind of new ceramic molding of the beginning of the nineties in last century by U.S.'s Oak Ridge National Laboratory invention, it is a kind of near-net-shape technology, be applicable to part (the OmateteO O of different shape complexity, size and accuracy requirement, Janne M A, Sterehlow R A.Gelcasting-a new ceramic forming process.Am Ceram Soc Bull.1991,70 (10), 1641～1649).Molding blank density is even, defective is less; The coagulation forming cycle is shorter; The base substrate organic content is low, and degreasing is easy, and sintered compact shrinks little, premium propertiess such as shape in the time of can keeping moulding and dimension scale thereof.Yang Jinlong etc. disclose a kind of method that the method that adopts colloidal formation prepares ceramic bead in patent (ZL 02125221.1).This method is that the suspensoid that will add initiator injects the funnel that can regulate diameter, enters the heating liquids oil medium from the funnel liquid bead that drips, and forms ceramic bead, and the diameter of bead is regulated by the diameter of regulating funnel.Literature search is the result show, also do not take injectiong coagulation shaping technology to prepare UO at present
2Ceramic fuel microsphere.
Technology contents:
The purpose of this invention is to provide a kind of notes type that congeals into and prepare UO
2The method of ceramic fuel microsphere is compared with sol gel process, has advantages such as technology radioactive liquid waste amount simple, that produce is few.
A kind of preparation UO that the present invention proposes
2The method of ceramic fuel microsphere adopts to annotate and coagulates the method for forming, and it is characterized in that: described method is carried out successively as follows:
(1) preparation of slurry: organic monomer is mixed with water, be mixed with premixed liquid, described organic monomer is linking agent and coupling agent, accounts for premixed liquid quality 2～30%, and the mass ratio of linking agent and coupling agent is 12～100: 1; Add ceramic powder and dispersion agent, wherein the solid load of ceramic powder in slurry is 40～60%, and dispersant dosage is 0.2～2% of a ceramic powder;
(2) preparation of suspended nitride: above-mentioned slurry is handled by the mode of mechanical stirring or ball milling, obtain the stable suspersion slurry, by the bubble in the degassing processing elimination slurry, stir the adding initiator again, initiator amount accounts for the 0.5～10wt ‰ of slip total mass;
(3) dispersion of slurry: gained slurry in the step 2 is transferred in the pressure-pot, leaves standstill 10～30min froth breaking,, adjust the pressure and the dispersion frequency of slurry according to the size and the density requirements of design microballoon; Open the thermal source that disperses post outer, dispersive slurry bead drops in balling-up in the oil medium;
(4) washing of microballoon, drying, roasting and sintering: the bead of collecting is placed the Rotary drying stove that vacuumizes, wash and drying; Carry out roasting and sintering according to the corresponding system of the character of ceramic powder then, obtain the ceramic microsphere of size.
In above-mentioned preparation method, the ceramic powder in the described step 1 is U
30
8Perhaps UO
2Powder; Described organic monomer is the acrylamide with free radical activity, Methacrylamide, any in N hydroxymethyl acrylamide, the acrylate; Described linking agent is the N-N-methylene-bisacrylamide; Described dispersion agent is ammonium polyacrylate, ammonium citrate, polyacrylic any.
In above-mentioned preparation method, degassing processing comprises and vacuumizes or add defoamer in the described step 2; Described vacuumizing is meant that slurry vacuumizes 10～30min under the operating mode of vibration or stirring, and vacuum tightness is 0.01mpa; Described defoamer comprises one or both of different new ester, lipid acid, and its consumption is 0.05～2% of a ceramic powder quality.
In above-mentioned preparation method, the initiator in the described step 2 is an ammonium persulphate, and the adding method is: with a certain amount of ammonium persulphate dissolving, the stirring arm gob adds ammonium persulfate aqueous solution then earlier.
In above-mentioned preparation method, described step 3 is with catalyst n, N, and N ', N '-Tetramethyl Ethylene Diamine join in the oiliness dispersion medium, and the adding volume ratio is an oil medium: catalyzer=100: 0～4.
In above-mentioned preparation method, the oil medium in the described step 3 is any of dimethyl silicone oil, paraffin oil, kerosene or edible oil, and oily temperature control is between 50～90 ℃.
The present invention compares with sol gel process, and its major advantage is:
1, do not need nitric acid dissolve U
3O
8Powder, boil operation such as glue, technology is simple, and it is few that process produces waste liquid amount.
2, because the organism amount that contains in the slip is few, and degreasing is easy, the rimose tendency reduces when microballoon drying, roasting.
Specific implementation
Below in conjunction with embodiment technical scheme of the present invention is described further:
The present invention is with the stable slurry of certain solid load (water base), becomes droplet by vibration, is distributed in the oil medium with certain temperature, droplet balling-up under the effect of interfacial tension, gelation reaction takes place in the polymer monomer polymerization of drop inside, solidifies balling-up.Then through technological processs such as washing, drying, roasting and sintering, the UO that finally obtains high rate of finished products and adhere to specification
2Ceramic fuel microsphere.Its method is:
1, the preparation of slurry:
The organic monomer that will have free radical activity mixes with water, be mixed with premixed liquid, described organic monomer is linking agent and coupling agent, account for premixed liquid quality 2～50%, the mass ratio of linking agent and coupling agent is 12～100: 1 adding ceramic powder and dispersion agent, wherein the solid load of ceramic powder in slurry is 40～60%, and dispersant dosage is 0.2～2% of a ceramic powder.
2, the preparation of suspended nitride:
Above-mentioned slurry is handled by the mode of mechanical stirring or ball milling, obtained the stable suspersion slurry of high solid loading, again by the bubble in the degassing processing elimination slurry.Stir and add initiator.Initiator amount accounts for the 0.5～10wt ‰ of slip total mass.
3, the dispersion of slurry:
Above-mentioned gained slurry is transferred in the pressure-pot,, adjusts the pressure and the dispersion frequency of slurry according to the size and the density requirements of design microballoon.Dispersive slurry bead drops in the microballoon that can obtain even size distribution in the oil medium.
4, the washing of microballoon, drying, roasting and sintering
The bead of collecting is placed the Rotary drying stove that can vacuumize, wash and drying.Carry out roasting and sintering according to the corresponding system of the character of ceramic powder then, obtain the ceramic microsphere of size and void content.
The device that the above-mentioned method for preparing gel micro-ball relates to comprises the pressure-pot of placing slurry, the dispersing nozzle that is connected with pressure-pot, the electromagnetic vibrator of static jet and signal thereof take place and control device, the dispersion post of oiliness dispersion medium is housed, disperse the outer thermal source of post, with washing, drying, reduction and the agglomerating plant etc. that disperse post to link to each other.
Porcelain powder of the present invention is UO
2, U
3O
8Powder; Monomer is the acrylamide with free radical activity, Methacrylamide, any in N hydroxymethyl acrylamide, the acrylate; Linking agent is the N-N-methylene-bisacrylamide; Dispersion agent is any of ammonium polyacrylate, ammonium citrate.
Degassing processing of the present invention comprises and vacuumizes or add defoamer; Vacuumize and be meant that slurry vacuumizes 10～30min under the operating mode of vibration or stirring; Defoamer comprises any of different new ester, lipid acid, and consumption is 0.05～2% of a ceramic powder quality.
Initiator of the present invention is an ammonium persulphate, and the adding method is: with a certain amount of ammonium persulphate dissolving, the stirring arm gob adds ammonium persulfate aqueous solution then earlier.
Of the present invention with catalyst n, N, N ', N '-Tetramethyl Ethylene Diamine join in the oil content dispersion media, and the adding volume ratio is an oil medium: catalyzer=100: 0～4.
Oil medium of the present invention can be a kind of of dimethyl silicone oil, paraffin oil, kerosene or edible oil, and oily temperature control is between 50～90 ℃.
Embodiment 1
UO
2Powder, median size are 2 microns.Preparation 100ml premixed liquid, mass ratio is: 82%H
2O: 16% acrylamide: 2%N-N-methylene-bisacrylamide.Add UO
2Powder, the configuration solid load is 50% slurry, adds the dispersion agent ammonium polyacrylate, the dispersion agent quality is UO
20.5% of powder quality.Mechanical stirring 2 hours, froth in vacuum 15min.Add the aqueous solution (mass concentration 2%) 0.8ml of initiator ammonium persulfate, transfer to after the stirring and leave standstill 10min in the pressure-pot.The catalyst n that disperses canned an amount of dimethyl silicone oil (viscosity 50mPaS, density 0.8g/ml) adding silicone oil quality 2% in the post, N, N ', N '-Tetramethyl Ethylene Diamine connects and disperses the outer thermal source of post, and silicone oil is heated to 50 ℃ of constant temperature.Slurry pressurization 0.35MPa, single mouth flow is 1ml/s, dispersion frequency is 120S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, through 500 ℃ of Ar/H2 mixed atmospheres roasting 2 hours and 1600 ℃ of hydrogen atmosphere sintering 2 hours, obtaining density was 10.7g/cm then
3, sphere diameter is 500 ± 20 microns UO
2Ceramic microsphere.
Embodiment 2
Raw material is U
3O
8Powder, median size are 1 micron.Preparation 200ml premixed liquid, mass ratio is: 92%H
2O: 7.2% acrylamide: 0.8%N-N-methylene-bisacrylamide.Add U
3O
8Powder, the configuration solid load is 58% slurry, adds the dispersion agent ammonium polyacrylate, the dispersion agent quality is 1.5% of a powder quality.Ball milling 3 hours adds the defoamer isooctyl alcohol, and consumption is U
3O
80.7% of opaque amount stirs a little.10 of the aqueous solution (mass concentration 5%) of adding initiator ammonium persulfate are transferred to after the stirring and are left standstill 10min in the pressure-pot.Disperse canned an amount of paraffin oil (viscosity 60mPaS, density 0.9g/ml) in the post, connect and disperse the outer thermal source of post, paraffin oil is heated to 80 ℃ of constant temperature.The slurry pressurization, single mouth flow is 1ml/s, dispersion frequency is 100S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, behind the roasting of 500 ℃ of 2 hours air atmospheres and 600 ℃ of hydrogen atmosphere reduction, 1550 ℃ of hydrogen atmosphere sintering, obtain density 10.68g/cm
3, sphere diameter is the UO of 410 ± 13 μ m
2Microballoon.
Embodiment 3
Raw material U
3O
8Powder, median size are 2 microns.Preparation 100ml premixed liquid, mass ratio is: 90%H
2O: 10%N-n-methylolacrylamide: 0.8%N-N-methylene-bisacrylamide.Add material powder, the configuration solid load is 56% slurry, adds the dispersion agent ammonium citrate, and the dispersion agent quality is 2% of a material powder quality.Ball milling 2 hours adds defoamer lipid acid, and consumption is 0.2% of a raw material powder, stirs a little.Add the aqueous solution (mass concentration 10%) 0.1ml of initiator ammonium persulfate, transfer to after the stirring and leave standstill 30min in the pressure-pot.Disperse canned an amount of kerosene (viscosity 5mPaS, density 0.84g/ml) in the post, connect and disperse the outer thermal source of post, kerosene is heated to 60 ℃ of constant temperature.The slurry pressurization, dispersion frequency is 120S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, behind the roasting of 400 ℃, 2 hours air atmospheres and 600 ℃ of hydrogen atmosphere reduction, 1500 ℃ of hydrogen atmosphere sintering, obtain density 10.61g/cm
3, sphere diameter is the UO of 508 ± 12 μ m
2Microballoon.
Claims (6)
1, a kind of preparation UO
2The method of ceramic fuel microsphere adopts to annotate and coagulates the method for forming, and it is characterized in that: described method is carried out successively as follows:
(1) preparation of slurry: organic monomer is mixed with water, be mixed with premixed liquid, described organic monomer is linking agent and coupling agent, accounts for premixed liquid quality 2～50%, and the mass ratio of linking agent and coupling agent is 12～100: 1; Add ceramic powder and dispersion agent, wherein the solid load of ceramic powder in slurry is 40～60%, and dispersant dosage is 0.2～2% of a ceramic powder;
(2) preparation of suspended nitride: above-mentioned slurry is handled by the mode of mechanical stirring or ball milling, obtain the stable suspersion slurry, by the bubble in the degassing processing elimination slurry, stir the adding initiator again, initiator amount accounts for the 0.5～10wt ‰ of slip total mass;
(3) dispersion of slurry: gained slurry in the step 2 is transferred in the pressure-pot,, adjusts the pressure and the dispersion frequency of slurry according to the size and the density requirements of design microballoon; Open the thermal source that disperses post outer, dispersive slurry bead drops in balling-up in the oil medium;
(4) washing of microballoon, drying, roasting and sintering: the bead of preparation is placed the Rotary drying stove that vacuumizes, wash and drying; Carry out roasting and sintering according to the corresponding system of the character of ceramic powder then, obtain the ceramic microsphere of size and void content.
2, method according to claim 1 is characterized in that: the ceramic powder in the described step 1 is U
3O
8Perhaps UO
2Powder; Described organic monomer is the acrylamide with free radical activity, Methacrylamide, any in N hydroxymethyl acrylamide, the acrylate; Described coupling agent is the N-N-methylene-bisacrylamide; Described dispersion agent is any of ammonium polyacrylate, ammonium citrate.
3, method according to claim 1 is characterized in that: degassing processing comprises and vacuumizes or add defoamer in the described step 2; Described vacuumizing is meant that slurry vacuumizes under the operating mode of vibration or stirring; Described defoamer comprises one or both of different new ester, lipid acid, and its consumption is 0.05～2% of a ceramic powder quality.
4, method according to claim 1 is characterized in that: the initiator in the described step 2 is an ammonium persulphate, and the adding method is: with a certain amount of ammonium persulphate dissolving, the stirring arm gob adds ammonium persulfate aqueous solution then earlier.
5, method according to claim 1 is characterized in that: described step 3 is with catalyst n, N, and N ', N '-Tetramethyl Ethylene Diamine join in the oiliness dispersion medium, and the adding volume ratio is an oil medium: catalyzer=100: 0～4.
6, method according to claim 1 is characterized in that: the oil medium in the described step 3 is any of methyl-silicone oil, paraffin oil, kerosene or edible oil, and oily temperature control is between 50～90 ℃.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102280152A (en) * | 2011-05-12 | 2011-12-14 | 清华大学 | Method for producing uranium dioxide ceramic fuel microspheres |
| CN102800374A (en) * | 2012-08-31 | 2012-11-28 | 清华大学 | Continuous operation feeding device and method |
| CN103492069A (en) * | 2011-08-17 | 2014-01-01 | 阿海珐有限公司 | Method for producing a catalyst containing uranium oxide as active component |
| CN103936076A (en) * | 2014-01-16 | 2014-07-23 | 中国科学院高能物理研究所 | Uranium oxide micro-sphere and preparation method thereof |
| CN102232231B (en) * | 2008-12-01 | 2014-11-26 | 德国纽克姆技术公司 | Method and arrangement for producing fuel cores |
| CN104446479A (en) * | 2014-11-06 | 2015-03-25 | 中国核动力研究设计院 | Method of preparing ceramic grade uranium dioxide ball |
| CN105642907A (en) * | 2016-01-29 | 2016-06-08 | 中国核动力研究设计院 | UO2-W metal ceramic ball preparation method |
| CN107910084A (en) * | 2017-11-21 | 2018-04-13 | 中国科学技术大学 | A kind of uranium carbide nuclear fuel micro and preparation method thereof |
| CN110835263A (en) * | 2019-10-31 | 2020-02-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing zirconia ceramic microspheres |
| CN110903084A (en) * | 2019-11-12 | 2020-03-24 | 西安交通大学 | High-entropy oxide submicron powder and preparation method thereof |
| CN111032205A (en) * | 2017-08-23 | 2020-04-17 | 原子能和替代能源委员会 | Method for preparing a powder containing uranium oxide UO2, optionally plutonium oxide PuO2, and optionally americium oxide AmO2 and/or other minor actinide oxides |
| CN111167387A (en) * | 2020-01-13 | 2020-05-19 | 清华大学 | Device for preparing large-size monodisperse uranium dioxide microspheres |
| CN115947361A (en) * | 2022-11-21 | 2023-04-11 | 江苏联瑞新材料股份有限公司 | Low-radioactivity alumina powder and preparation method thereof |
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|---|---|---|---|---|
| CN102232231B (en) * | 2008-12-01 | 2014-11-26 | 德国纽克姆技术公司 | Method and arrangement for producing fuel cores |
| CN102280152A (en) * | 2011-05-12 | 2011-12-14 | 清华大学 | Method for producing uranium dioxide ceramic fuel microspheres |
| CN103492069A (en) * | 2011-08-17 | 2014-01-01 | 阿海珐有限公司 | Method for producing a catalyst containing uranium oxide as active component |
| CN102800374A (en) * | 2012-08-31 | 2012-11-28 | 清华大学 | Continuous operation feeding device and method |
| CN102800374B (en) * | 2012-08-31 | 2014-11-26 | 清华大学 | Continuous operation feeding device and method |
| CN103936076A (en) * | 2014-01-16 | 2014-07-23 | 中国科学院高能物理研究所 | Uranium oxide micro-sphere and preparation method thereof |
| 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 |
| CN104446479A (en) * | 2014-11-06 | 2015-03-25 | 中国核动力研究设计院 | Method of preparing ceramic grade uranium dioxide ball |
| CN105642907A (en) * | 2016-01-29 | 2016-06-08 | 中国核动力研究设计院 | UO2-W metal ceramic ball preparation method |
| CN111032205A (en) * | 2017-08-23 | 2020-04-17 | 原子能和替代能源委员会 | Method for preparing a powder containing uranium oxide UO2, optionally plutonium oxide PuO2, and optionally americium oxide AmO2 and/or other minor actinide oxides |
| CN111032205B (en) * | 2017-08-23 | 2022-07-05 | 原子能和替代能源委员会 | Method for preparing a powder containing uranium oxide, optionally plutonium oxide, and optionally americium oxide and/or other minor actinide oxides |
| CN107910084A (en) * | 2017-11-21 | 2018-04-13 | 中国科学技术大学 | A kind of uranium carbide nuclear fuel micro and preparation method thereof |
| CN107910084B (en) * | 2017-11-21 | 2020-01-03 | 中国科学技术大学 | Uranium carbide nuclear fuel microsphere and preparation method thereof |
| CN110835263A (en) * | 2019-10-31 | 2020-02-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing zirconia ceramic microspheres |
| CN110903084A (en) * | 2019-11-12 | 2020-03-24 | 西安交通大学 | High-entropy oxide submicron powder and preparation method thereof |
| CN110903084B (en) * | 2019-11-12 | 2021-02-02 | 西安交通大学 | High-entropy oxide submicron powder and preparation method thereof |
| CN111167387A (en) * | 2020-01-13 | 2020-05-19 | 清华大学 | Device for preparing large-size monodisperse uranium dioxide microspheres |
| CN115947361A (en) * | 2022-11-21 | 2023-04-11 | 江苏联瑞新材料股份有限公司 | Low-radioactivity alumina powder and preparation method thereof |
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