CN101708829B - Method for preparing yttria-stabilized zirconia powder - Google Patents
Method for preparing yttria-stabilized zirconia powder Download PDFInfo
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- CN101708829B CN101708829B CN200910199279XA CN200910199279A CN101708829B CN 101708829 B CN101708829 B CN 101708829B CN 200910199279X A CN200910199279X A CN 200910199279XA CN 200910199279 A CN200910199279 A CN 200910199279A CN 101708829 B CN101708829 B CN 101708829B
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- yttria
- zirconia powder
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Abstract
The invention belongs to the field of material chemistry, and in particular relates to a method for preparing yttria-stabilized zirconia powder. The method particularly adopts an ultrasonic-microwave synthesis method, carries out precursor preparation under an ultrasonic condition so as to ensure that a system can be better dispersed and doped, and adopts a microwave heating mode to dry the precursor so as to avoid agglomeration of the precursor. After the precursor is calcined at high temperature, the yttria-stabilized zirconia powder can be obtained. The powder has good dispersity, and has grain diameter reaching nanometer grade, uniform sizes and uniform distributions. The method has the advantages of simple process, low cost and the like.
Description
Technical field
The invention belongs to the materials chemistry field, be specifically related to a kind of preparation method of yttria-stabilized zirconia powder.
Background technology
Yttria-stabilized zirconia (YSZ) is good oxygen ion conductor, and it is all very stable under oxidizing atmosphere and reducing atmosphere, it is the ionogen of the most frequently used Solid Oxide Fuel Cell (SOFC), also be widely used in oxygen probe, oxygen separation membrane etc., particularly, use very extensive in the function ceramics field.
For obtaining good ceramic post sintering activity, require the particle of powder little, be evenly distributed, do not have reunion, and wish the regular shape of powder granule.In addition,, high performance stupalith be sought out, just the powder raw material that particle diameter is little, activity is high, distribution of particle sizes is concentrated, reunion is little need be used because the densification rate of ceramic powder and the biquadratic of its particle size are inversely proportional to.This class raw material can not only reduce the sintering temperature of pottery, save energy, and can improve the performance of ceramic greatly, as thermostability, mechanical property, mechanical property etc.
At present the preparation method of relevant yttria-stabilized zirconia powder has a variety ofly, and reported have coprecipitation method, sol-gel method, hydrothermal method, co-precipitation-gel method, alcohol-water solution method, azeotropic distn, microwave assisting method, reverse micelle method, a microemulsion method etc.Such as, employing microwave hydrothermal synthesis methods such as Zhao Qing are prepared the yttria-stabilized zirconia powder material (application number: 200410097794.4) of size in nanometer scale.Lin Zhenhan etc. prepare zirconium oxide nano crystal by the hydrothermal decomposition precipitator method, add binding agent and dispersion agent then, obtain spherical particle powder (application number: 200810039796.6) by spraying drying.With the coprecipitation method is the chemical synthesis of representative, because of it has advantages such as equipment is simple, easy to operate, with low cost, is subjected to paying close attention to widely, and still, often there is the hard aggregation problem in the powder of coprecipitation method preparation.Though with ethanol or other organic solvent washings,, avoid the generation of hard aggregation, but practice shows that this can not eliminate hard aggregation fully can remove the coordinated water molecule on surface.The hard aggregation phenomenon has a strong impact on the application performance of powder, causes the ceramic sintering temperature height, adverse consequencess such as sintering character difference.Therefore, explore a kind of method that can solve the hard aggregation problem, have realistic meaning.
Summary of the invention
The objective of the invention is to propose a kind of reducing production costs, effectively solve the novel yttria-stabilized zirconia powder preparation method of traditional agglomeration traits.
The novel yttria-stabilized zirconia powder preparation method that the present invention proposes, utilize the synergy of ultrasonic-microwave, and under the synergy of dispersion agent, realized that yttrium mixes better in crystal of zirconium oxide, reached control product particle diameter, the effect of the degree that reduces to reunite.Not only effectively solve the powder reuniting problem, saved the energy, and can improve the application performance of powder greatly.The present invention is achieved in that with ZrOCl8H
2O and Y
2O
3Be main raw material, adopt ultrasonic-microwave process for synthesizing to be prepared, concrete steps are as follows: a, with deionized water with ZrOCl
2Dissolving fully adds tensio-active agent as dispersion agent; B, use a small amount of concentrated nitric acid, under heating condition, make Y
2O
3Dissolving fully; C, with the ZrOCl for preparing in a, the b step
2Solution and Y
2O
3The solution mixing, the ammoniacal liquor of adding 30% under ultrasound condition, complete to precipitation, at this moment about pH=9; D, the precipitation that suction filtration is intact place microwave reactor dry, grind, and obtain precursor; E, get above-mentioned precursor and place crucible, in retort furnace, calcine, pulverize then, obtain yttria-stabilized zirconia powder.
The yttria-stabilized zirconia powder size of the present invention's preparation has reached nanometer scale, and product is subsphaeroidal particle, and the size homogeneous has good dispersiveness.Precursor of the present invention is to form under the acting in conjunction of ultrasonic wave and template, can produce the oscillating action of linear alternation during ultrasonic wave work, strengthen vibration and shearing between particle, increase the probability that collides between the reactive ion, impel reaction to carry out quickly and evenly.When ultrasonic wave is propagated in reaction system, can make the microbubble in the solution generate, increase, shrink, collapse by the conduct of vibrating, and cause near the liquid the bubble to produce the intensive shock wave, form the thermal extremes high pressure of local location, ultrasonic cavitation makes the frictional belt attenuate, has strengthened the micropore diffusion, and it is long-pending to have increased mass transfer surfaces, improve the speed and the effect of mass transfer, can further improve the ion impact rate.In addition, ultrasonic wave is propagated in system, and its vibrational energy is constantly changed into heat energy and makes self temperature rising by the system absorption, and this also can quicken mass transfer process, helps the diffusing, doping of reactive ion.Even adulterated precursor on the molecular level has been arranged, and is the important prerequisite that yttria-stabilized zirconia powder can form substitutional solid solution well, also is one of key factor of control product dispersiveness.
Precursor adopts the mode of microwave drying, and the water molecules that is heated in the precursor is a polar molecule, and it is under fast-changing high-frequency electromagnetic field action, and its polarity orientation will change along with the variation of external electric field, cause the motion of molecule and mutual friction mutually.This moment, the field energy of microwave field was converted into heat energy in the system, and temperature of charge is raise, and produced thermalization and a series of materializing procedures such as expanded, thereby reached the purpose of micro-wave drying.The advantage that adopts microwave heating is that rate of heating is fast and evenly, regardless of each position shape of object, microwave heating all can make while uniformly penetrating hertzian wave in the object table and produce heat energy.Simultaneously, the microwave drying efficient energy-saving generates heat owing to the material that contains moisture absorbs microwave easily, therefore except that a spot of transmission loss, does not almost have other energy waste.
Beneficial effect
The present invention has following advantage: the yttria-stabilized zirconia uniform particle diameter that prepare (1), and size reaches nanometer scale, has good dispersiveness, solved the hard aggregation problem that prior art occurs in preparation process preferably; (2) preparation method of the present invention, the technology that adopts a ultrasonic microwave to combine is brought into play both advantages, and preparation technology is simple, mild condition; (3) technology of the present invention can effectively reduce production costs to the rate of energy height.
Embodiment
Below, by embodiment, the present invention is described further.
Embodiment 1
Take by weighing 3.22g ZrOCl8H
2O adds deionized water 20mL in beaker, after the dissolving, add 0.2g Triton-100 as dispersion agent fully.Take by weighing 0.0226g Y
2O
3In another beaker, under heating condition, add concentrated nitric acid and dissolve fully to it.Above-mentioned two solution are mixed, the beaker that fills reaction soln is placed ultrasonic disperser, and under the ultrasonic disperser working conditions, add 30% ammoniacal liquor, complete to precipitation.To precipitate suction filtration, washing extremely with till the no chlorion existence of Silver Nitrate check.The precipitation that suction filtration is intact placed microwave reactor dry 6 hours.After drying finishes, porphyrize.Get above-mentioned precursor and place crucible, heating and calcining is 3 hours under 700 ℃ of conditions of retort furnace.Naturally cooling, comminution by gas stream, the gained size is about 2% yttria-stabilized zirconia powder of 25nm.
Embodiment 2
Take by weighing 3.22g ZrOCl8H
2O adds deionized water 20mL in beaker, after the dissolving, add 0.2g soil temperature-60 as dispersion agent fully.Take by weighing 0.0339g Y
2O
3In another beaker, under heating condition, add concentrated nitric acid and dissolve fully to it.After above-mentioned two solution mixing, the beaker that fills reaction soln is placed ultrasonic disperser, and under the ultrasonic disperser working conditions, add 30% ammoniacal liquor, complete to precipitation.To precipitate suction filtration, wash to precipitating suction filtration, washing extremely with till the no chlorion existence of Silver Nitrate check.The precipitation that suction filtration is intact placed microwave dryer dry 3 hours, after drying finishes, and porphyrize.Get above-mentioned precursor and place crucible, under 600 ℃ of conditions of retort furnace, heating calcination 1 hour.Naturally cooling, comminution by gas stream, the gained size is about 3% yttria-stabilized zirconia powder of 30nm.
Embodiment 3
Take by weighing 3.22g ZrOCl8H
2O adds deionized water 20mL in beaker, after the dissolving, add the 0.2g polyoxyethylene glycol as dispersion agent fully.Take by weighing 0.09g Y
2O
3In another beaker, under heating condition, add concentrated nitric acid and dissolve fully to it.Above-mentioned two solution are mixed, the beaker that fills reaction soln is placed ultrasonic disperser, and under the ultrasonic disperser working conditions, add 30% ammoniacal liquor, complete to precipitation.To precipitate suction filtration, wash to precipitating suction filtration, washing extremely with till the no chlorion existence of Silver Nitrate check.The precipitation that suction filtration is intact placed microwave dryer dry 5 hours, after drying finishes, and the porphyrize pack.Take out above-mentioned precursor and place crucible, under 600 ℃ of conditions of retort furnace, heating calcination 6 hours.Naturally cooling, comminution by gas stream, the gained size is about the stable Zirconium powder of 8% yttrium of 30nm.
Embodiment 4
Take by weighing 3.22g ZrOCl8H
2O adds deionized water 20mL in beaker, after the dissolving, add the 0.2g polyoxyethylene glycol as dispersion agent fully.Take by weighing 0.113g Y
2O
3In another beaker, under heating condition, add concentrated nitric acid and dissolve fully to it.Above-mentioned two solution are mixed, the beaker that fills reaction soln is placed ultrasonic disperser, and under the ultrasonic disperser working conditions, add 30% ammoniacal liquor, complete to precipitation.To precipitate suction filtration, wash to precipitating suction filtration, washing extremely with till the no chlorion existence of Silver Nitrate check.The precipitation that suction filtration is intact placed microwave dryer dry 5 hours, after drying finishes, and the porphyrize pack.Take out above-mentioned precursor and place crucible, under 800 ℃ of conditions of retort furnace, heating calcination 6 hours.Naturally cooling, comminution by gas stream, the gained size is about the stable Zirconium powder of 10% yttrium of 50nm.
Claims (3)
1. the preparation method of a yttria-stabilized zirconia powder, it is with ZrOCl8H
2O and Y
2O
3Be main raw material, adopt ultrasonic-microwave process for synthesizing to be prepared, concrete steps are as follows:
A, with deionized water with ZrOCl
2Dissolving fully adds tensio-active agent as dispersion agent, and the dispersion agent of adding is Triton-100, polyoxyethylene glycol or a soil temperature-60;
B, use a small amount of concentrated nitric acid, under heating condition, make Y
2O
3Dissolving fully;
C, with the ZrOCl for preparing in a, the b step
2Solution and Y
2O
3The solution mixing, the ammoniacal liquor of adding 30% under ultrasound condition, extremely precipitation is complete, at this moment pH=9;
D, the precipitation that suction filtration is intact place microwave reactor dry, and be 3-6 hour time of drying, grinds, and obtains precursor;
E, get above-mentioned precursor and place crucible, in retort furnace, calcine, pulverize then, obtain yttria-stabilized zirconia powder.
2. the preparation method of a kind of yttria-stabilized zirconia powder according to claim 1 is characterized in that precursor incinerating temperature is 600-800 ℃, and calcination time is 1-6 hour.
3. the preparation method of a kind of yttria-stabilized zirconia powder according to claim 1, the molar ratio that it is characterized in that Yttrium oxide doping is 2～10%.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857428A (en) * | 2010-05-21 | 2010-10-13 | 华东理工大学 | Preparation method of conductive zinc oxide powder |
| CN101891471B (en) * | 2010-07-12 | 2013-03-13 | 江西泛美亚材料有限公司 | Method for preparing zirconium oxide nanopowder stabilized by yttrium oxide |
| CN102503417B (en) * | 2011-10-11 | 2014-07-16 | 武汉钢铁(集团)公司 | Preparation method for yttria-partially-stabilized zirconia powder |
| CN103623807A (en) * | 2013-12-10 | 2014-03-12 | 江南大学 | Preparation method for novel doped nano-zirconia catalyst |
| CN106946568A (en) * | 2017-04-21 | 2017-07-14 | 浙江金琨锆业有限公司 | A kind of yttrium stable zirconium oxide raw powder's production technology of high dispersive |
| CN108409337A (en) * | 2018-02-02 | 2018-08-17 | 昆明理工大学 | A method of doped metallic oxide YSZ electrolyte ceramics are prepared based on coprecipitation |
| CN108640144B (en) * | 2018-07-17 | 2020-05-08 | 信丰县包钢新利稀土有限责任公司 | Yttrium oxide double-stage nanosphere and preparation method thereof |
| CN110342931A (en) * | 2019-07-11 | 2019-10-18 | 河北铭万精细化工有限公司 | A kind of preparation method of ceramic nano zirconium oxide powder |
| CN111018521B (en) * | 2019-12-06 | 2022-03-25 | 广东工业大学 | Zirconia-zirconium boride composite ceramic and preparation method and application thereof |
| CN112443709A (en) * | 2020-12-07 | 2021-03-05 | 苏州市桔园管业有限公司 | Multi-element composite pipeline |
Citations (1)
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| CN1528706A (en) * | 2003-10-10 | 2004-09-15 | 徐华蕊 | Y2O3 stable tetragonal phase ZrO2 monodisperse nano posder hydrothermal preparation method |
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| CN1528706A (en) * | 2003-10-10 | 2004-09-15 | 徐华蕊 | Y2O3 stable tetragonal phase ZrO2 monodisperse nano posder hydrothermal preparation method |
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