CN101169983A - Sol-gel method Gd2O3-UO2 microsphere preparation process - Google Patents

Sol-gel method Gd2O3-UO2 microsphere preparation process Download PDF

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CN101169983A
CN101169983A CNA2006101507536A CN200610150753A CN101169983A CN 101169983 A CN101169983 A CN 101169983A CN A2006101507536 A CNA2006101507536 A CN A2006101507536A CN 200610150753 A CN200610150753 A CN 200610150753A CN 101169983 A CN101169983 A CN 101169983A
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microballoon
sol
solution
technology
gel ball
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黎光荣
刘锦洪
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Nuclear Power Institute of China
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Nuclear Power Institute of China
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Abstract

The invention provides a process for preparing Gd2O3-UO2 microball by using the sol gel method, which comprises the steps of pre-processing, dissolving, gel preparation, gelation, drying, calcining, and reduce sintering to prepare a Gd2O3-UO2 microball of burnable poison. The inventive process can prepare the Gd2O3-UO2 microball containing any Gd content, and the diameter of the microball is equal to or less than 300 Mu, the density is larger than or equal to 96 percent T.D, and oxygen-metal atomic ratio of 1.655-1.670. The impurity content of the microball satisfies the requirement and the microball has good uniformity and solid meltability.

Description

Sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon
Technical field
The present invention relates to nuclear material preparation technology, be specifically related to a kind of sol-gal process and prepare Gd 2O 3-UO 2The technology of microballoon.
Background technology
In reactor, Gd commonly used 2O 3-UO 2As burnable poison, to increase the burnup of reactor fuel, prolong the reactor refuling cycle.As mixed oxide fuel, often adopt coprecipitation technology and powder mixing procedure technology of preparing, its accurate component, uniformity and solid solution are the technological difficulties that need control always.As " Characterization of homogeneity in (U, Gd) O that mentions in 212～216 pages of " Journal of Nuclear Materials " 1991 178 volumes 2-pellets " in the literary composition to colloidal sol, prepared (U, Gd) O of chemical coprecipitation technique 2Homogeneity, homogeney feature discuss; " Jouranl ofNuclear Science and Technology " 23[4 in 1986] " the Magnetic susceptibility of U that mentions in the 326th～329 page 1-xGd xO 2Solid solution " in the literary composition to the prepared U of co-precipitation 1-xGd xO 2Magnetic properties discuss.
At present, coprecipitation technology and powder mixing procedure all can prepare Gd 2O 3-UO 2Burnable poison.Coprecipitation technology mixes in liquid phase owing to crystal grain, because the K of Gd, U SpHave than big-difference, thereby low tenor in the accuracy of its restive component and the mother liquor; Though and the powder mixing procedure can solve the accuracy of component, homogeneity and solid solution are restive.
Summary of the invention
The object of the present invention is to provide a kind of employing sol-gal process to prepare Gd 2O 3-UO 2The technology of microballoon can effectively solve the problems such as the restive accurate component of prior art, uniformity and solid solution.
Sol-gal process of the present invention prepares Gd 2O 3-UO 2The technology of microballoon, it comprises the steps:
1) preliminary treatment: with Gd 2O 3Powder was 300～350 ℃ of lower calcinings 1～2 hour; 800～900 ℃ of lower calcinings 2～4 hours, ammonium diuranate at high temperature changed into U with the ammonium diuranate powder 3O 8
2) dissolving: use dense HNO 3With step 1) in the calcining after Gd 2O 3Dissolving, Gd 2O 3With dense HNO 3The solid-liquid ratio be 1: (1.3～1.5) g/ml has formed Gd (NO 3) 3Solution; Use dense HNO 3With step 1) middle gained U 3O 8Dissolving, U 3O 8With dense HNO 3The solid-liquid ratio be 1: (1.35～1.45) g/ml, filter, filtrate is acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution;
3) join glue: the mass ratio of pressing the quality of metal gadolinium (Gd) and metallic uranium (U) is (2～12): 100, blend step 2) Gd (NO of gained 3) 3Solution and acid deficient uranyl nitrate solution are lower than 5 ℃ of lower stirrings in temperature and cool off; In above-mentioned mixed solution, add urea and hexamethylenetetramine again, the mol ratio of metallic uranium is 1 in urea and the mixed solution: (1.2～1.6), the mol ratio of metallic uranium is 1 in hexamethylenetetramine and the mixed solution: (1.2～1.6) have formed sol solution behind dissolve complete;
4) gelling: temperature is lower than in 8 ℃ the step 3) gained sol solution and is distributed in the organic media and solidifies, formed the aqueous gel ball;
5) washing: with weak aqua ammonia to step 4) in gained aqueous gel ball fully wash airing then;
6) drying and calcining: the gel ball to gained airing in the step 5) carries out drying and calcining, and its temperature slowly heated up 9～10 hours to 50～80 ℃ from room temperature earlier, was incubated 3～4 hours; Be warming up to 180～220 ℃ again, be incubated 2～2.5 hours; Be warming up to 300～350 ℃ again, be incubated 2～2.5 hours; Naturally cool to room temperature then;
7) reduction sintering: to step 6) behind the drying and calcining gel ball of gained at N 2And H 2Reduce calcining under the mixed-gas atmosphere, temperature is warming up to 800～840 ℃ by 5～10 ℃/minute, is incubated 3～4 hours, naturally cools to then room temperature, obtains at last Gd 2O 3-UO 2Microballoon.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, its step 2) describedly uses dense HNO 3Dissolving U 3O 8, it dissolves under room temperature to 80 ℃.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, its step 3) the described stirring under temperature is lower than 5 ℃ cooled off, and is to be lower than in temperature to stir cooling in 5 ℃ of ice-water baths.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, its step 4) described sol solution is distributed to organic media, is sol solution to be distributed to 65～70 ℃ organic media.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, its step 4) organic media described in is paraffin oil or isooctanol.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, its step 5) described in weak aqua ammonia to the washing of aqueous gel ball, used aqueous gel ball and the solid-to-liquid ratio of weak aqua ammonia are 1: (2～6) g/ml, washing times are at least 3 times, wash time is at least 1 hour at every turn.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, it is in step 5) in adopt the mixed solution of weak aqua ammonia and deionized water that the aqueous gel ball is washed, the weak aqua ammonia volume accounts for 40～60% of mixed solution cumulative volume in this mixed solution.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, it is in step 5) described in the mixed solution with weak aqua ammonia and deionized water the aqueous gel ball is washed, the solid-to-liquid ratio of aqueous gel ball and mixed solution is 1: (2～6) g/ml, washing times are at least 3 times, each wash time at least 1 hour.
Aforesaid Prepared by Sol Gel Method Gd 2O 3-UO 2The technology of microballoon, the described N of its step 7) 2And H 2Mixed gas, wherein H 2Volume accounts for the 40-60% of this mixed gas cumulative volume.
Aforesaid sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, it is to step 7) the described Gd that obtains at last 2O 3-UO 2The burnable poison microballoon, with the sieve screening, the microballoon that will meet size changes preferred machine over to, optimizes the satisfactory microballoon of sphericity with preferred machine, the underproof microballoon of size and sphericity returns step 6) calcination process, be qualified Gd through the microballoon after preferred 2O 3-UO 2The burnable poison microballoon.
Effect of the present invention is: the present invention prepares Gd 2O 3-UO 2The burnable poison microballoon has adopted sol-gal process, its proportion speed, and products obtained therefrom purity height, uniformity and solid fusibleness are good, when having solved prior art and having prepared burnable poison, the technological difficulties such as restive accurate component, uniformity and solid solution.The Gd that can prepare any Gd content according to technology of the present invention 2O 3-UO 2The burnable poison microballoon, prepared microspherulite diameter≤300 μ, density 〉=96%T.D, oxygen metallic atom ratio is 1.655～1.670, and impurity content meets the requirements, and uniformity and solid fusibleness are good.
Embodiment
Embodiment 1
Sol-gal process of the present invention prepares Gd 2O 3-UO 2The technology of microballoon is specific as follows:
1) preliminary treatment (calcining Gd 2O 3, ammonium diuranate):
With Gd 2O 3Powder is put into Muffle furnace, 350 ℃ of lower calcinings 2 hours, to remove Gd 2O 3In trace water; Ammonium diuranate (ADU) powder is put into Muffle furnace, and 850 ℃ of lower calcinings 2 hours, ADU at high temperature changed into U 3O 8
2) dissolving (preparation Gd (NO 3) 3Solution, acid deficient uranyl nitrate solution):
With step 1) in Gd after the gained calcining 2O 3Powder is used dense HNO 3Dissolving, Gd 2O 3With dense HNO 3The solid-liquid ratio be 1: 1.3g/ml, treat Gd 2O 3Filter after the dissolving fully, filtrate is Gd (NO 3) 3Solution; With step 1) middle gained U 3O 8, use dense HNO 3Dissolving, solution temperature is room temperature, U 3O 8With dense HNO 3The solid-liquid ratio be 1: 1.42g/ml, filter after the dissolving, filtrate is acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution;
3) join glue (preparation sol solution):
Be 3: 97 by the quality of metal gadolinium (Gd) and the mass ratio of metallic uranium (U), take by weighing respectively step 2) Gd (NO of gained 3) 3Solution and acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution, mix, put into temperature and be lower than 5 ℃ of ice-water baths stirring coolings; In this mixed solution, add respectively urea and hexamethylenetetramine again, the mol ratio of metallic uranium (U) is 1: 1.4 in urea and this mixed solution, the mol ratio of metallic uranium (U) is 1: 1.4 in hexamethylenetetramine and this mixed solution, after solid dissolves fully, formed sol solution this moment;
4) gelling (sol solutions is solidified in dispersion, gelling):
The sol solution that temperature is lower than 8 ℃ of following step 3) gained is distributed in 65 ℃ the paraffin oil and solidifies, and forms the aqueous gel ball;
5) washing (washing and aging gelling ball):
Adopt the mixed solution of weak aqua ammonia and deionized water that step 4) gained aqueous gel ball is fully washed, the weak aqua ammonia volume accounts for 50% of this mixed solution cumulative volume in this mixed solution, the solid-to-liquid ratio of aqueous gel ball and this mixed solution is 1: 4g/ml, washing times is 3 times, each wash time 1 hour, the gel ball airing after the washing;
6) drying and calcining:
The gel ball of step 5) gained airing is put into baking oven, slowly heated up 10 hours to 60 ℃, be incubated 4 hours, be warming up to 200 ℃ by 1 ℃/minute again, be incubated 2 hours, be warming up to 350 ℃ again, be incubated 2 hours, naturally cool to room temperature from room temperature;
7) reduction sintering:
Gel ball after the step 6) calcining is put into induction furnace again, at N 2And H 2Reduce calcining under the mixed-gas atmosphere, H 2Volume accounts for 50% of this mixed gas cumulative volume, is warming up to 840 ℃ by 5 ℃/minute, is incubated 3 hours, naturally cools to room temperature, makes Gd at last 2O 3-UO 2Microballoon.
Be Gd through the product after the above-mentioned technology 2O 3-UO 2The burnable poison microballoon sieves thus obtained microsphere with sieve, and the microballoon that will meet size changes preferred machine over to, optimizes the satisfactory microballoon of sphericity with preferred machine, and the underproof microballoon of size and sphericity returns step 6) calcination process, process again.
Microballoon after preferred is qualified Gd 2O 3-UO 2The burnable poison microballoon, prepared microspherulite diameter 70～300 μ, density 〉=96%T.D, oxygen metallic atom ratio is 1.655～1.670, and impurity content meets the requirements, and uniformity and solid fusibleness are good.
Embodiment 2
Sol-gal process of the present invention prepares Gd 2O 3-UO 2The technology of microballoon is specific as follows:
1) preliminary treatment (calcining Gd 2O 3, ammonium diuranate):
With Gd 2O 3Powder is put into Muffle furnace, 300 ℃ of lower calcinings 1 hour, to remove Gd 2O 3In trace water; Ammonium diuranate (ADU) powder is put into Muffle furnace, and 800 ℃ of lower calcinings 4 hours, ADU at high temperature changed into U 3O 8
2) dissolving (preparation Gd (NO 3) 3Solution, acid deficient uranyl nitrate solution):
With step 1) in Gd after the gained calcining 2O 3Powder is used dense HNO 3Dissolving, Gd 2O 3With dense HNO 3The solid-liquid ratio be 1: 1.5g/ml, treat Gd 2O 3Filter after the dissolving fully, filtrate is Gd (NO 3) 3Solution; With step 1) middle gained U 3O 8, use dense HNO 3Dissolving, solution temperature is 50 ℃, U 3O 8With dense HNO 3The solid-liquid ratio be 1: 1.35g/ml, filter after the dissolving, filtrate is acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution;
3) join glue (preparation sol solution):
Be 10: 90 by the quality of metal gadolinium (Gd) and the mass ratio of metallic uranium (U), take by weighing respectively step 2) Gd (NO of gained 3) 3Solution and acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution, mix, be lower than 5 ℃ of lower stirrings in temperature and cool off; In this mixed solution, add respectively urea and hexamethylenetetramine again, the mol ratio of metallic uranium (U) is 1: 1.6 in urea and this mixed solution, the mol ratio of metallic uranium (U) is 1: 1.6 in hexamethylenetetramine and this mixed solution, after solid dissolves fully, formed sol solution this moment;
4) gelling (sol solutions is solidified in dispersion, gelling):
The sol solution that temperature is lower than 8 ℃ of following step 3) gained is distributed in 70 ℃ the isooctyl alcohol and solidifies, and forms the aqueous gel ball;
5) washing (washing and aging gelling ball):
Adopting weak aqua ammonia to step 4) gained aqueous gel ball fully washs, and the solid-to-liquid ratio of aqueous gel ball and weak aqua ammonia is 1: 3g/ml, washing times are 4 times, and wash time is 2 hours at every turn, the gel ball airing after the washing;
6) drying and calcining:
The gel ball of step 5) gained airing is put into baking oven, slowly heated up 9 hours to 80 ℃, be incubated 3 hours, by being warming up to 220 ℃, be incubated 2 hours again, be warming up to 320 ℃ again, be incubated 2.5 hours, naturally cool to room temperature from room temperature;
7) reduction sintering:
Gel ball after the step 6) calcining is put into induction furnace again, at N 2And H 2Reduce calcining under the mixed-gas atmosphere, H 2Volume accounts for 60% of this mixed gas cumulative volume, is warming up to 820 ℃ by 8 ℃/minute, is incubated 4 hours, naturally cools to room temperature, makes Gd at last 2O 3-UO 2Microballoon.
Be Gd through the product after the above-mentioned technology 2O 3-UO 2The burnable poison microballoon sieves thus obtained microsphere with sieve, and the microballoon that will meet size changes preferred machine over to, optimizes the satisfactory microballoon of sphericity with preferred machine, and the underproof microballoon of size and sphericity returns step 6) calcination process.
Microballoon after preferred is qualified Gd 2O 3-UO 2The burnable poison microballoon, prepared microspherulite diameter 70～300 μ, density 〉=96%T.D, oxygen metallic atom ratio is 1.655～1.670, and impurity content meets the requirements, and uniformity and solid fusibleness are good.
Embodiment 3
Sol-gal process of the present invention prepares Gd 2O 3-UO 2The technology of microballoon is specific as follows:
1) preliminary treatment (calcining Gd 2O 3, ammonium diuranate):
With Gd 2O 3Powder is put into Muffle furnace, 320 ℃ of lower calcinings 1.5 hours, to remove Gd 2O 3In trace water; Ammonium diuranate (ADU) powder is put into Muffle furnace, and 900 ℃ of lower calcinings 3 hours, ADU at high temperature changed into U 3O 8
2) dissolving (preparation Gd (NO 3) 3Solution, acid deficient uranyl nitrate solution):
With step 1) in Gd after the gained calcining 2O 3Powder is used dense HNO 3Dissolving, Gd 2O 3With dense HNO 3The solid-liquid ratio be 1: 1.4g/ml has formed Gd (NO 3) 3Solution; With step 1) middle gained U 3O 8, use dense HNO 3Dissolving, solution temperature is 80 ℃, U 3O 8With dense HNO 3The solid-liquid ratio be 1: 1.45g/ml, filter after the dissolving, filtrate is acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution;
3) join glue (preparation sol solution):
Be 7: 93 by the quality of metal gadolinium (Gd) and the mass ratio of metallic uranium (U), take by weighing respectively step 2) Gd (NO of gained 3) 3Solution and acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution, mix, put into ice-water bath and stir cooling; In this mixed solution, add respectively urea and hexamethylenetetramine again, the mol ratio of metallic uranium (U) is 1: 1.2 in urea and this mixed solution, the mol ratio of metallic uranium (U) is 1: 1.3 in hexamethylenetetramine and this mixed solution, after solid dissolves fully, formed sol solution this moment;
4) gelling (sol solutions is solidified in dispersion, gelling):
The sol solution that temperature is lower than 8 ℃ of following step 3) gained is distributed in 68 ℃ the paraffin oil and solidifies, and forms the aqueous gel ball;
5) washing (washing and aging gelling ball):
Adopt the mixed solution of weak aqua ammonia and deionized water that step 4) gained aqueous gel ball is fully washed, the weak aqua ammonia volume accounts for 40% of this mixed solution cumulative volume in this mixed solution, the solid-to-liquid ratio of aqueous gel ball and this mixed solution is 1: 2g/ml, washing times is 5 times, each wash time 3 hours, the gel ball airing after the washing;
6) drying and calcining:
The gel ball of step 5) gained airing is put into baking oven, slowly heated up 9.5 hours to 50 ℃, be incubated 4 hours, be warming up to 180 ℃ by 2 ℃/minute again, be incubated 2.5 hours, be warming up to 300 ℃ again, be incubated 2.5 hours, naturally cool to room temperature from room temperature;
7) reduction sintering:
Gel ball after the step 6) calcining is put into induction furnace again, at N 2And H 2Reduce calcining under the mixed-gas atmosphere, H 2Volume accounts for 40% of this mixed gas cumulative volume, is warming up to 800 ℃ by 10 ℃/minute, is incubated 3.5 hours, naturally cools to room temperature, makes Gd at last 2O 3-UO 2Microballoon.
Be Gd through the product after the above-mentioned technology 2O 3-UO 2The burnable poison microballoon sieves thus obtained microsphere with sieve, and the microballoon that will meet size changes preferred machine over to, optimizes the satisfactory microballoon of sphericity with preferred machine, and the underproof microballoon of size and sphericity returns step 6) calcination process, process again.
Microballoon after preferred is qualified Gd 2O 3-UO 2The burnable poison microballoon, prepared microspherulite diameter 70～300 μ, density 〉=96%T.D, oxygen metallic atom ratio is 1.655～1.670, and impurity content meets the requirements, and uniformity and solid fusibleness are good.

Claims (10)

1. a sol-gal process prepares Gd 2O 3-UO 2The technology of microballoon, it comprises the steps:
1) preliminary treatment: with Gd 2O 3Powder was 300～350 ℃ of lower calcinings 1～2 hour; 800～900 ℃ of lower calcinings 2～4 hours, ammonium diuranate at high temperature changed into U with the ammonium diuranate powder 3O 8
2) dissolving: use dense HNO 3With step 1) in the calcining after Gd 2O 3Dissolving, Gd 2O 3With dense HNO 3The solid-liquid ratio be 1: (1.3～1.5) g/ml has formed Gd (NO 3) 3Solution; Use dense HNO 3With step 1) middle gained U 3O 8Dissolving, U 3O 8With dense HNO 3The solid-liquid ratio be 1: (1.35～1.45) g/ml, filter, filtrate is acid deficient uranyl nitrtate (UO 2(NO 3) 2) solution;
3) join glue: the mass ratio of pressing the quality of metal gadolinium (Gd) and metallic uranium (U) is (2～12): 100, blend step 2) Gd (NO of gained 3) 3Solution and acid deficient uranyl nitrate solution are lower than 5 ℃ of lower stirrings in temperature and cool off; In above-mentioned mixed solution, add urea and hexamethylenetetramine again, the mol ratio of metallic uranium is 1 in urea and the mixed solution: (1.2～1.6), the mol ratio of metallic uranium is 1 in hexamethylenetetramine and the mixed solution: (1.2～1.6) have formed sol solution behind dissolve complete;
4) gelling: temperature is lower than in 8 ℃ the step 3) gained sol solution and is distributed in the organic media and solidifies, formed the aqueous gel ball;
5) washing: with weak aqua ammonia to step 4) in gained aqueous gel ball fully wash airing then;
6) drying and calcining: the gel ball to gained airing in the step 5) carries out drying and calcining, and its temperature slowly heated up 9～10 hours to 50～80 ℃ from room temperature earlier, was incubated 3～4 hours; Be warming up to 180～220 ℃ again, be incubated 2～2.5 hours; Be warming up to 300～350 ℃ again, be incubated 2～2.5 hours; Naturally cool to room temperature then;
7) reduction sintering: to step 6) behind the drying and calcining gel ball of gained at N 2And H 2Reduce calcining under the mixed-gas atmosphere, temperature is warming up to 800～840 ℃ by 5～10 ℃/minute, is incubated 3～4 hours, naturally cools to then room temperature, obtains at last Gd 2O 3-UO 2Microballoon.
2. sol-gal process according to claim 1 prepares Gd 2O 3-UO 2The technology of microballoon is characterized in that: step 2) describedly use dense HNO 3Dissolving U 3O 8, it dissolves under room temperature to 80 ℃.
3. sol-gal process according to claim 1 prepares Gd 2O 3-UO 2The technology of microballoon is characterized in that: step 3) the described stirring under temperature is lower than 5 ℃ cooled off, and is to be lower than in temperature to stir cooling in 5 ℃ of ice-water baths.
4. sol-gal process according to claim 1 prepares Gd 2O 3-UO 2The technology of microballoon is characterized in that: step 4) described sol solution is distributed to organic media, is sol solution to be distributed to 65～70 ℃ organic media.
5. sol-gal process according to claim 4 prepares Gd 2O 3-UO 2The technology of microballoon is characterized in that: step 4) described in organic media be paraffin oil or isooctanol.
6. sol-gal process according to claim 1 prepares Gd 2O 3-UO 2The technology of microballoon is characterized in that: step 5) described in weak aqua ammonia to aqueous gel ball washing, used aqueous gel ball and the solid-to-liquid ratio of weak aqua ammonia are 1: (2～6) g/ml, washing times are at least 3 times, wash time is at least 1 hour at every turn.
7. sol-gal process according to claim 1 prepares Gd 2O 3-UO 2The technology of microballoon is characterized in that: in step 5) in adopt the mixed solution of weak aqua ammonia and deionized water that the aqueous gel ball is washed, the weak aqua ammonia volume accounts for 40～60% of mixed solution cumulative volume in this mixed solution.
8. sol-gal process according to claim 7 prepares Gd 2O 3-UO 2The technology of microballoon, it is characterized in that: in step 5) described in the mixed solution with weak aqua ammonia and deionized water the aqueous gel ball is washed, the solid-to-liquid ratio of aqueous gel ball and mixed solution is 1: (2～6) g/ml, washing times are at least 3 times, each wash time at least 1 hour.
9. Prepared by Sol Gel Method Gd according to claim 1 2O 3-UO 2The technology of microballoon is characterized in that: the described N of step 7) 2And H 2Mixed gas, wherein H 2Volume accounts for the 40-60% of this mixed gas cumulative volume.
10. prepare Gd according to any one described sol-gal process of claim 1～9 2O 3-UO 2The technology of microballoon is characterized in that: to step 7) the described Gd that obtains at last 2O 3-UO 2The burnable poison microballoon, with the sieve screening, the microballoon that will meet size changes preferred machine over to, optimizes the satisfactory microballoon of sphericity with preferred machine, the underproof microballoon of size and sphericity returns step 6) calcination process, be qualified Gd through the microballoon after preferred 2O 3-UO 2The burnable poison microballoon.
CNA2006101507536A 2006-10-25 2006-10-25 Sol-gel method Gd2O3-UO2 microsphere preparation process Pending CN101169983A (en)

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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
CN104821187A (en) * 2015-03-11 2015-08-05 中国核动力研究设计院 Al2O3 doped UO2-10wt%Gd2O3 burnable poison and preparation method thereof
CN105377763A (en) * 2013-04-29 2016-03-02 原子能与替代能源委员会 Novel material made of uranium, gadolinium and oxygen and use thereof as a consumable neutron poison
CN106145198A (en) * 2016-06-29 2016-11-23 中国科学技术大学 Prepare the method and device of uranium oxide microsphere
CN107833645A (en) * 2017-10-26 2018-03-23 中国科学院上海应用物理研究所 A kind of preparation method of thorium based mixed oxide ceramic microsphere
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
CN109443874A (en) * 2018-11-22 2019-03-08 核工业北京化工冶金研究院 Uranium and impurity element standard substance preparation method in a kind of triuranium octoxide
CN109824355A (en) * 2019-02-22 2019-05-31 西南科技大学 A kind of processing method of Spent Radioactive organic solvent tributyl phosphate pyrolysis ashes
CN111039326A (en) * 2020-01-13 2020-04-21 清华大学 Method for preparing uranium dioxide microspheres at normal temperature

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CN105377763B (en) * 2013-04-29 2017-06-27 原子能与替代能源委员会 The new material formed by uranium, gadolinium and oxygen and its purposes as consumable neutron poison
CN105377763A (en) * 2013-04-29 2016-03-02 原子能与替代能源委员会 Novel material made of uranium, gadolinium and oxygen and use thereof as a consumable neutron poison
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CN103366846A (en) * 2013-07-19 2013-10-23 清华大学 Uranium dioxide core aging tank, and system and method for aging, cleaning and drying
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CN103474114B (en) * 2013-08-23 2016-03-23 中国核动力研究设计院 A kind of preparation method of nuclear power uranium titanium oxide hybrid ceramic fuel pellet
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
CN104821187A (en) * 2015-03-11 2015-08-05 中国核动力研究设计院 Al2O3 doped UO2-10wt%Gd2O3 burnable poison and preparation method thereof
CN106145198A (en) * 2016-06-29 2016-11-23 中国科学技术大学 Prepare the method and device of uranium oxide microsphere
CN107833645A (en) * 2017-10-26 2018-03-23 中国科学院上海应用物理研究所 A kind of preparation method of thorium based mixed oxide ceramic microsphere
CN107833645B (en) * 2017-10-26 2020-02-07 中国科学院上海应用物理研究所 Preparation method of thorium-based mixed oxide ceramic microspheres
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
CN109443874A (en) * 2018-11-22 2019-03-08 核工业北京化工冶金研究院 Uranium and impurity element standard substance preparation method in a kind of triuranium octoxide
CN109824355A (en) * 2019-02-22 2019-05-31 西南科技大学 A kind of processing method of Spent Radioactive organic solvent tributyl phosphate pyrolysis ashes
CN109824355B (en) * 2019-02-22 2021-09-03 西南科技大学 Treatment method of radioactive waste organic solvent tributyl phosphate pyrolysis furnace ash
CN111039326A (en) * 2020-01-13 2020-04-21 清华大学 Method for preparing uranium dioxide microspheres at normal temperature
CN111039326B (en) * 2020-01-13 2020-12-01 清华大学 Method for preparing uranium dioxide microspheres at normal temperature

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