CN102079655A - Preparation method of strontium-doped lanthanum molybdate ceramic - Google Patents
Preparation method of strontium-doped lanthanum molybdate ceramic Download PDFInfo
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- CN102079655A CN102079655A CN2011100450029A CN201110045002A CN102079655A CN 102079655 A CN102079655 A CN 102079655A CN 2011100450029 A CN2011100450029 A CN 2011100450029A CN 201110045002 A CN201110045002 A CN 201110045002A CN 102079655 A CN102079655 A CN 102079655A
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Abstract
The invention discloses a preparation method of strontium-doped lanthanum molybdate ceramic, which is used for solving the technical problem that the traditional preparation method of lanthanum molybdate ceramic has long preparation cycle. The technical scheme of the preparation method comprises the following steps of: synthesizing by adopting a microwave synthesis process to obtain lanthanum molybdate powder, carrying out isostatic pressing on the powder, and then sintering to form ceramic. In the invention, the preparation cycle of the lanthanum molybdate ceramic is reduced to 11-13h from 48h in the background technology; and meanwhile, the preparation temperature is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of lanthanum molybdate pottery, particularly a kind of preparation method of strontium doping lanthanum molybdate pottery.
Background technology
Oxygen ion conductor has obtained at aspects such as Solid Oxide Fuel Cell, oxygen sensor, solid ionic devices using widely.If (as the zirconium white of stabilized with yttrium oxide, YSZ), then its working temperature is wanted enough high and just can be obtained higher working efficiency to adopt traditional oxygen ion conductor.For example, be that electrolytical SOFC must work about 1000 ℃ with YSZ.High working temperature brought such as cost height, sealing difficulty, with a series of problems such as electrode materials coupling difficulty.Lanthanum molybdate is as a kind of good solid electrolyte of oxygen ion conductor.Its oxygen ionic conductivity at 800 ℃ has reached more than the 0.06S/cm.Because preparation technology is simple and the prices of raw and semifnished materials are cheap, make the ionogen of warm SOFC in the conduct of lanthanum molybdate pottery and the candidate material of electrode have bigger competitive edge.
Compared with traditional solid state sintering, microwave digestion technology has obviously reduced energy consumption and preparation cycle, and tentatively the synthetic powder has thinner particle, and surfactivity is bigger, providing enough motivating forces in the sintering process once more, thereby can form finer and close ceramic body to improve its performance.Document " D.Marrero-Lopez; J.Canales-Vazquez; J.C.Ruiz-Morales; A.Rodriguez, J.T.S.Irvine and P.Nunez, Solid State Ionics; 176; 1807 (2005) " discloses a kind of preparation method of lanthanum molybdate pottery, i.e. freeze-drying, and this method is dissolved in molybdenum oxide and lanthanum trioxide respectively in the nitric acid and ammoniacal liquor of dilution by stoichiometric ratio.Under the constant stir speed (S.S.), add ethylenediamine tetraacetic acid (EDTA), the PH of solution is adjusted to 10 with ammoniacal liquor with 0.5: 1 mol ratio.This solution is splashed in the liquid nitrogen freezing, this freezing process will generate little ice crystal, make ice crystal distillation dehydration two days then in a vacuum.Dried powder is calcined under 573K with 15K/ minute speed and was obtained presoma in 10 minutes, grinds sintering more then.Though but it has made the powder than fine particle, it is long still to show preparation cycle, inefficient restricted.
Summary of the invention
Prepare long deficiency of lanthanum molybdate pottery cycle in order to overcome prior preparation method, the invention provides a kind of preparation method of strontium doping lanthanum molybdate pottery.This method adopts microwave synthesis process to synthesize, and obtains the lanthanum molybdate powder, and powder sinters porcelain into through behind the isostatic pressing, can reduce the preparation cycle of lanthanum molybdate pottery.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of strontium doping lanthanum molybdate pottery is characterized in comprising the steps:
(a) with analytical pure La (NO
3)
3, (NH
4)
6Mo
7O
244H
2O, Sr (NO
3)
2, citric acid is according to stoichiometric ratio La
2-xSr
xMo
2O
9Weighing and batching, wherein x=0～0.2;
(b) material that will prepare is put into container, is stirred to the solution that forms homogeneous, and wherein citric acid is about 2: 1 with the mol ratio of total metal ion;
(c) solution of homogeneous is poured in the reaction vessel, at 180～200 ℃, cleared up under 600～800w power 30～50 minutes with microwave;
(d) reacted solution is carried out suction filtration, products therefrom is dried processing then;
(e) powder after the processing carries out isostatic pressing, is sintering the disk after the moulding into porcelain in 10～12 hours 900～950 ℃ of following insulations again.
The invention has the beneficial effects as follows: because this method adopts microwave synthesis process to synthesize, obtain the lanthanum molybdate powder, powder is through sintering porcelain into behind the isostatic pressing, and the preparation cycle of lanthanum molybdate pottery was reduced by 11～13 hours by 48 hours of background technology, had reduced preparation temperature simultaneously.
Below in conjunction with the drawings and specific embodiments the present invention is elaborated.
Description of drawings
Fig. 1 is the La of embodiment 1 preparation
2Mo
2O
9Powder surface microstructure photo.
Fig. 2 (figure below) is embodiment 3 prepared La
2Mo
2O
9The powder XRD figure spectrum of powder; Fig. 2 (last figure) is embodiment 3 prepared La
2-xSr
xMo
2O
9The XRD figure spectrum of pottery.
Embodiment
Embodiment 1: with analytical pure La (NO
3)
3, (NH
4)
6Mo
7O
244H
2O, citric acid is according to stoichiometric ratio La
2Mo
2O
9Weighing and batching, wherein citric acid is about 2: 1 with the mol ratio of total metal example, the material for preparing is put into beaker, the solution that is stirred to the formation homogeneous is in pouring reaction vessel into, with microwave at 180 ℃, cleared up under the 800w power 30 minutes, reacted solution is carried out suction filtration, products therefrom is dried processing then; Powder after the processing carries out isostatic pressing, is sintering the disk after the moulding into porcelain in 12 hours 900 ℃ of following insulations again.
As can be seen from Figure 1, the La of present embodiment preparation
2Mo
2O
9Powder surface is cashed out stratiform, and decentralized is good, and specific surface area is easy to sintering greatly.
Embodiment 2: with analytical pure La (NO
3)
3, (NH
4)
6Mo
7O
244H
2O, Sr
2(NO
3)
2, citric acid is according to La
2-xSr
xMo
2O
9Stoichiometric ratio x=0.05 weighing and batching, wherein citric acid is about 2: 1 with the mol ratio of total metal example, the material for preparing is put into beaker, the solution that is stirred to the formation homogeneous is in pouring reaction vessel into, with microwave at 190 ℃, cleared up under the 700w power 40 minutes, reacted solution is carried out suction filtration, products therefrom is dried processing then; Powder after the processing carries out isostatic pressing, is sintering the disk after the moulding into porcelain in 11 hours 930 ℃ of following insulations again.
Embodiment 3: with analytical pure La (NO
3)
3, (NH
4)
6Mo
7O
244H
2O, Sr
2(NO
3)
2, citric acid is according to La
2-xSr
xMo
2O
9Stoichiometric ratio x=0.1 weighing and batching, wherein citric acid is about 2: 1 with the mol ratio of total metal example, the material for preparing is put into beaker, the solution that is stirred to the formation homogeneous is in pouring reaction vessel into, with microwave at 200 ℃, cleared up under the 600w power 50 minutes, reacted solution is carried out suction filtration, products therefrom is dried processing then; Powder after the processing carries out isostatic pressing, is sintering the disk after the moulding into porcelain in 10 hours 950 ℃ of following insulations again.
Fig. 2 is the powder (figure below) that obtains of micro-wave digestion and the La behind the double sintering
2-xSr
xMo
2O
9Ceramic powder (last figure) XRD figure spectrum.The La that finally draws as can be seen
2Mo
2O
9Pure phase.
The contriver is in the disclosed process parameters range of technical scheme, and different parameter collocation are all tested, and have all obtained good effect.
In a word, the present invention substitutes traditional solid-phase sintering method by the micro-wave digestion method, and no matter from preparation cycle still, or the energy consumption aspect all has significant progress, and obtains thinner powder.
Claims (1)
1. the preparation method of a strontium doping lanthanum molybdate pottery is characterized in that comprising the steps:
(a) with analytical pure La (NO
3)
3, (NH
4)
6Mo
7O
244H
2O, Sr (NO
3)
2, citric acid is according to stoichiometric ratio La
2-xSr
xMo
2O
9Weighing and batching, wherein x=0～0.2;
(b) material that will prepare is put into container, is stirred to the solution that forms homogeneous, and wherein citric acid is about 2: 1 with the mol ratio of total metal ion;
(c) solution of homogeneous is poured in the reaction vessel, at 180～200 ℃, cleared up under 600～800w power 30～50 minutes with microwave;
(d) reacted solution is carried out suction filtration, products therefrom is dried processing then;
(e) powder after the processing carries out isostatic pressing, is sintering the disk after the moulding into porcelain in 10～12 hours 900～950 ℃ of following insulations again.
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|---|---|---|---|
| CN2011100450029A CN102079655A (en) | 2011-02-24 | 2011-02-24 | Preparation method of strontium-doped lanthanum molybdate ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100450029A CN102079655A (en) | 2011-02-24 | 2011-02-24 | Preparation method of strontium-doped lanthanum molybdate ceramic |
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|---|---|
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Family
ID=44085881
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124594B (en) * | 2016-06-12 | 2018-07-03 | 西安电子科技大学 | A kind of preparation method based on lanthanum molybdate nano material air-sensitive testing element |
| CN109713347A (en) * | 2018-12-10 | 2019-05-03 | 合肥学院 | A kind of metallic element doping La2Mo2O9Method for preparing solid electrolyte |
| CN109987622A (en) * | 2019-04-10 | 2019-07-09 | 宁波大学 | A kind of cobalt doped lanthanum molybdate micro Nano material and preparation method thereof |
-
2011
- 2011-02-24 CN CN2011100450029A patent/CN102079655A/en active Pending
Non-Patent Citations (6)
| Title |
|---|
| 《Journal of the European Ceramic Society》 20041231 R. Subasri et al. Synthesis and characterization of (La1-xMx)2Mo2O9-delta; M = Ca2+, Sr2+ or Ba2+ 第129-137页 1 第24卷, * |
| 《Solid State Ionics》 20101231 D.M. Zhang et al. Electrical properties and microstructure of nanocrystalline La2-xAxMo2O9-delta (A=Ca, Sr, Ba, K) films 第1510-1515页 1 第181卷, * |
| D.M. ZHANG ET AL.: "Electrical properties and microstructure of nanocrystalline La2-xAxMo2O9-δ (A=Ca, Sr, Ba, K) films", 《SOLID STATE IONICS》 * |
| JEONG HO RYU ET AL.: "Microwave-assisted synthesis of BaMoO4 nanocrystallites by a citrate complex method and their anisotropic aggregation", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| R. SUBASRI ET AL.: "Synthesis and characterization of (La1-xMx)2Mo2O9-δ; M = Ca2+, Sr2+ or Ba2+", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
| 石晓波等: "铈-钼复合氧化物超微粒子的合成", 《江西师范大学学报(自然科学版)》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124594B (en) * | 2016-06-12 | 2018-07-03 | 西安电子科技大学 | A kind of preparation method based on lanthanum molybdate nano material air-sensitive testing element |
| CN109713347A (en) * | 2018-12-10 | 2019-05-03 | 合肥学院 | A kind of metallic element doping La2Mo2O9Method for preparing solid electrolyte |
| CN109713347B (en) * | 2018-12-10 | 2021-01-19 | 合肥学院 | La doped with metal element2Mo2O9Method for preparing solid electrolyte |
| CN109987622A (en) * | 2019-04-10 | 2019-07-09 | 宁波大学 | A kind of cobalt doped lanthanum molybdate micro Nano material and preparation method thereof |
| CN109987622B (en) * | 2019-04-10 | 2021-07-30 | 宁波大学 | Cobalt-doped lanthanum molybdate micro-nano material and preparation method thereof |
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Application publication date: 20110601 |