CN103030392A - Scandia-stabilized zirconia solid solution and preparation technology thereof - Google Patents
Scandia-stabilized zirconia solid solution and preparation technology thereof Download PDFInfo
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- CN103030392A CN103030392A CN2012105802387A CN201210580238A CN103030392A CN 103030392 A CN103030392 A CN 103030392A CN 2012105802387 A CN2012105802387 A CN 2012105802387A CN 201210580238 A CN201210580238 A CN 201210580238A CN 103030392 A CN103030392 A CN 103030392A
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Abstract
The invention relates to a preparation technology of a scandia-stabilized zirconia solid solution, which comprises the specific steps of 1), preparing zirconium salt, scandium salt and a third component salt into a mixed solution, 2), adding ammonia water for coprecipitation, and adjusting a PH value, 3), water washing and centrifugal dewatering, 4), drying, 5), precalcination, and 7), high-energy ball milling. Compared with other method technologies, the preparation technology of the scandia-stabilized zirconia solid solution is simple, requirements on equipment are not high, the technology stability is excellent, the preparation technology is very suitable for industrial production, powder prepared by the preparation technology is suitable for high-temperature solid oxide fuel cells, and the powder is also suitable for moderate-temperature solid oxide fuel cells as the powder can keep higher conductivity at a moderate temperature section.
Description
Technical field
The present invention relates to field of fine chemical, particularly a kind of zirconia solid solution of scandia stabilized and preparation technology thereof.
Background technology
In recent years SOFC development is rapid especially, because during accidental power failure and other sudden disasters etc. have caused various accidents, by the power supply mode of fuel cell as decentralized power supply, can reduce the range of influence of disaster as far as possible.Simultaneously, because the energy is day by day deficient, fuel cell is as clean energy, and has efficient energy conversion rate, therefore is subject to extensive concern.
Wherein, the electrolyte of the fuel cell gordian technique in the battery technology that acts as a fuel, present research direction mainly concentrates on the higher electric conductivity of acquisition.But, the zirconium white by scandia stabilized (ScSZ) of having found at present has higher ionic conductivity and lower activation energy, and has than traditional 8mol% yttria stabilized zirconia higher specific conductivity under identical use temperature (800-1000 ℃).Therefore, with existing material converting become can suitability for industrialized production product, can advance faster the development of SOFC.
Summary of the invention
For the defective that exists in the prior art, the object of the present invention is to provide a kind of preparation technology of zirconia solid solution of scandia stabilized.
For reaching above purpose, the technical scheme that the present invention takes is:
A kind of preparation technology of zirconia solid solution of scandia stabilized, concrete steps:
1) zirconates, scandium salts and the 3rd component salt are made into mixed aqueous solution;
2) add the ammoniacal liquor co-precipitation, regulate pH value to 7.70-10.50;
3) washing, control is except OH
-Outer other anion-contents are less than 100ppm, centrifuge dehydration;
4) powder after the process dehydration is through 250 ℃ of oven dry of 150 –;
5) powder after the oven dry obtains elementary powder through 600 ℃ of precalcinings of 400 –;
6) elementary powder is calcined in oxidizing atmosphere, and condition is: 5 ℃/min of temperature rise rate 1 –, be warming up to 1000 ℃ of 800 –, and kept 10 – 30 hours;
7) powder after the calcining adopts the vertical ball mill high-energy ball milling, adds dispersion agent, is milled to middle particle diameter D
500.4 – 0.6 μ m, specific surface area=10.5 ± 1.0 m
2/ g;
8) spraying drying, the grain diameter that obtains the zirconia solid solution of scandia stabilized is 100-120 nm.
On the basis of such scheme, described the 3rd component salt is aluminium salt, cerium salt, yttrium salt, ytterbium salt or bismuth salt.
On the basis of such scheme, described zirconates, scandium salts and the 3rd component salt are muriate, nitrate or vitriol.
On the basis of such scheme, described dispersion agent is: modified polyacrylic acid ammonium or poly carboxylic acid ammonium salt.
A kind of zirconia solid solution that utilizes the scandia stabilized of aforesaid method preparation.
A kind of zirconia solid solution that utilizes the scandia stabilized of aforesaid method preparation, Scium trioxide content is 10mol% in the described sosoloid, and the 3rd component oxide content is 0-6mol%, and surplus is zirconium white.
The preparation technology of the zirconia solid solution of scandia stabilized of the present invention uses the automatically co-precipitation system of control of pH, has solved the powder granule lack of homogeneity of traditional coprecipitation technology preparation, the situation that hard aggregation is serious.Simultaneously with respect to other sol-gel methodes, glycine method, hydrothermal method, hydrolysis method etc., technique is simple, not high to equipment requirements, and technology stability is fabulous, be highly suitable for suitability for industrialized production, the present invention adopts coprecipitation technology and the precalcining system of having improved, the composite oxide solid solution that makes has improved the phenomenon of the particle agglomeration that existing coprecipitation technology causes, the dimensional homogeneity of the powder primary particles that obtains good (100-120 nm), have better sintering activity and less specific surface area, keep simultaneously high-caliber specific conductivity.This powder is applicable to high temperature solid oxide fuel cell, and because it also can keep higher specific conductivity at middle-temperature section, so it also is applicable to intermediate temperature solid oxide fuel cell.
Description of drawings:
Fig. 1 the method for the invention process flow sheet.
Embodiment
Embodiment 1
A kind of preparation technology of zirconia solid solution of scandia stabilized, concrete steps:
1) with ZrOCl
28H
2O 22.90Kg, ScCl
36H
2O 4.14Kg and CeCl
37H
2O 0.30Kg is made into mixed aqueous solution;
2) add the ammoniacal liquor co-precipitation, regulate pH value to 7.70;
3) washing, control Cl
-Content is less than 100ppm, centrifuge dehydration;
4) powder after the process dehydration is through 150 ℃ of oven dry;
5) powder after the oven dry obtains elementary powder through 400 ℃ of precalcinings;
6) elementary powder is calcined in oxidizing atmosphere, and condition is: 1 ℃/min of temperature rise rate, be warming up to 800 ℃, and kept 30 hours;
7) powder after the calcining adopts the vertical ball mill high-energy ball milling, adds modified polyacrylic acid ammonium 50g, is milled to middle particle diameter D
500.40-0.60 μ m, specific surface area=10.50 ± 1.00 m
2/ g;
8) spraying drying, the grain diameter that obtains the zirconia solid solution of scandia stabilized is 100-120 nm.
Scium trioxide content is 10mol% in the prepared sosoloid, and cerium oxide content is 1mol%, and surplus is zirconium white.
Embodiment 2
A kind of preparation technology of zirconia solid solution of scandia stabilized, concrete steps:
1) with Zr(NO
3)
45H
2O 29.60Kg, Sc(NO
3)
3H
2O 3.95Kg and Ce(NO
3)
35H
2O 0.99Kg is made into mixing solutions;
2) add the ammoniacal liquor co-precipitation, regulate pH value to 9.00;
3) washing, control NO
3 -Ion content is less than 100ppm, centrifuge dehydration;
4) powder after the process dehydration is through 200 ℃ of oven dry;
5) powder after the oven dry obtains elementary powder through 500 ℃ of precalcinings;
6) elementary powder is calcined in oxidizing atmosphere, and condition is: 3 ℃/min of temperature rise rate, be warming up to 900 ℃, and kept 20 hours;
7) powder after the calcining adopts the vertical ball mill high-energy ball milling, adds modified polyacrylic acid ammonium 50g, is milled to middle particle diameter D
500.40-0.60 μ m, specific surface area=10.50 ± 1.00 m
2/ g;
8) spraying drying, the grain diameter that obtains the zirconia solid solution of scandia stabilized is 100-120 nm.
Scium trioxide content is 10mol% in the prepared sosoloid, and cerium oxide content is 3mol%, and surplus is zirconium white.
Embodiment 3
A kind of preparation technology of zirconia solid solution of scandia stabilized, concrete steps:
1) with Zr (SO
4)
24H
2O 23.39Kg, Sc
2(SO
4)
36H
2O 3.81Kg and Ce (SO
4)
24H
2O 1.90Kg is made into mixing solutions;
2) add the ammoniacal liquor co-precipitation, regulate pH value to 10.50;
3) washing, control SO
4 2-Ion content is less than 100ppm, centrifuge dehydration;
4) powder after the process dehydration is through 250 ℃ of oven dry;
5) powder after the oven dry obtains elementary powder through 600 ℃ of precalcinings;
6) elementary powder is calcined in oxidizing atmosphere, and condition is: 5 ℃/min of temperature rise rate, be warming up to 1000 ℃, and kept 10 hours;
7) powder after the calcining adopts the vertical ball mill high-energy ball milling, adds modified polyacrylic acid ammonium 50g, is milled to middle particle diameter D
500.40-0.60 μ m, specific surface area=10.50 ± 1.00 m
2/ g;
8) spraying drying, the grain diameter that obtains the zirconia solid solution of scandia stabilized is 100-120 nm.
Scium trioxide content is 10mol% in the prepared sosoloid, and cerium oxide content is 6mol%, and surplus is zirconium white.
Claims (6)
1. the preparation technology of the zirconia solid solution of a scandia stabilized is characterized in that concrete steps:
1) zirconates, scandium salts and the 3rd component salt are made into mixed aqueous solution;
2) add the ammoniacal liquor co-precipitation, regulate pH value to 7.70-10.50;
3) washing, control is except OH
-Outer other anion-contents are less than 100ppm, centrifuge dehydration;
4) powder after the process dehydration is through 250 ℃ of oven dry of 150 –;
5) powder after the oven dry obtains elementary powder through 600 ℃ of precalcinings of 400 –;
6) elementary powder is calcined in oxidizing atmosphere, and condition is: 5 ℃/min of temperature rise rate 1 –, be warming up to 1000 ℃ of 800 –, and kept 10 – 30 hours;
7) powder after the calcining adopts the vertical ball mill high-energy ball milling, adds dispersion agent, is milled to middle particle diameter D
500.4 – 0.6 μ m, specific surface area=10.5 ± 1.0 m
2/ g;
8) spraying drying, the grain diameter that obtains the zirconia solid solution of scandia stabilized is 100-120 nm.
2. the preparation technology of the zirconia solid solution of scandia stabilized according to claim 1 is characterized in that described the 3rd component salt is aluminium salt, cerium salt, yttrium salt, ytterbium salt or bismuth salt.
3. the preparation technology of the zirconia solid solution of scandia stabilized according to claim 1 is characterized in that described zirconates, scandium salts and the 3rd component salt are muriate, nitrate or vitriol.
4. the preparation technology of the zirconia solid solution of scandia stabilized according to claim 1 is characterized in that described dispersion agent is: modified polyacrylic acid ammonium or poly carboxylic acid ammonium salt.
5. the zirconia solid solution of the scandia stabilized of the preparation technology of the zirconia solid solution of a scandia stabilized according to claim 1 preparation.
6. the zirconia solid solution of a kind of scandia stabilized according to claim 5, its feature Scium trioxide content in described sosoloid is 10mol%, and the 3rd component oxide content is 0-6mol%, and surplus is zirconium white.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445203A (en) * | 2017-09-06 | 2017-12-08 | 潮州三环（集团）股份有限公司 | A kind of zirconium oxide of scandia stabilized and preparation method thereof |
| CN111138189A (en) * | 2020-01-20 | 2020-05-12 | 中国恩菲工程技术有限公司 | Method and device for preparing scandium-zirconium powder |
| CN111138188A (en) * | 2020-01-20 | 2020-05-12 | 中国恩菲工程技术有限公司 | Preparation facilities of scandia stabilized zirconia powder |
| CN111205090A (en) * | 2020-01-15 | 2020-05-29 | 中国恩菲工程技术有限公司 | Scandium oxide stabilized zirconia powder and preparation method thereof |
| CN111233467A (en) * | 2020-01-15 | 2020-06-05 | 中国恩菲工程技术有限公司 | Oxide-doped scandium-zirconium powder and preparation method thereof |
| CN112724836A (en) * | 2020-12-24 | 2021-04-30 | 德米特（苏州）电子环保材料有限公司 | Cerium-zirconium-doped polishing solution and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699279A (en) * | 2005-05-25 | 2005-11-23 | 宜兴新兴锆业有限公司 | Improved yttrium partially stabilized zirconia production process |
-
2012
- 2012-12-28 CN CN201210580238.7A patent/CN103030392B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699279A (en) * | 2005-05-25 | 2005-11-23 | 宜兴新兴锆业有限公司 | Improved yttrium partially stabilized zirconia production process |
Non-Patent Citations (1)
| Title |
|---|
| M. PASTOR ET AL.: "Microstructural and impedance study of nanocrystalline lanthana-doped scandia-stabilized zirconia", 《J NANOPART RES》, vol. 14, 25 July 2012 (2012-07-25), pages 1 - 11 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445203A (en) * | 2017-09-06 | 2017-12-08 | 潮州三环（集团）股份有限公司 | A kind of zirconium oxide of scandia stabilized and preparation method thereof |
| CN107445203B (en) * | 2017-09-06 | 2019-06-21 | 潮州三环（集团）股份有限公司 | A kind of zirconium oxide of scandia stabilized and preparation method thereof |
| CN111205090A (en) * | 2020-01-15 | 2020-05-29 | 中国恩菲工程技术有限公司 | Scandium oxide stabilized zirconia powder and preparation method thereof |
| CN111233467A (en) * | 2020-01-15 | 2020-06-05 | 中国恩菲工程技术有限公司 | Oxide-doped scandium-zirconium powder and preparation method thereof |
| CN111138189A (en) * | 2020-01-20 | 2020-05-12 | 中国恩菲工程技术有限公司 | Method and device for preparing scandium-zirconium powder |
| CN111138188A (en) * | 2020-01-20 | 2020-05-12 | 中国恩菲工程技术有限公司 | Preparation facilities of scandia stabilized zirconia powder |
| CN112724836A (en) * | 2020-12-24 | 2021-04-30 | 德米特（苏州）电子环保材料有限公司 | Cerium-zirconium-doped polishing solution and preparation method and application thereof |
| CN112724836B (en) * | 2020-12-24 | 2022-03-29 | 德米特（苏州）电子环保材料有限公司 | Cerium-zirconium-doped polishing solution and preparation method and application thereof |
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| CN103030392B (en) | 2015-12-23 |
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