CN101033078A - Zr-position doped high conductivity proton conductor material for La2Zr2O7 basal body and preparing method thereof - Google Patents
Zr-position doped high conductivity proton conductor material for La2Zr2O7 basal body and preparing method thereof Download PDFInfo
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- CN101033078A CN101033078A CN 200710056688 CN200710056688A CN101033078A CN 101033078 A CN101033078 A CN 101033078A CN 200710056688 CN200710056688 CN 200710056688 CN 200710056688 A CN200710056688 A CN 200710056688A CN 101033078 A CN101033078 A CN 101033078A
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Abstract
This invention discloses a proton conductor material of high electric conductance of La2Zr2O7matrix doped at Zr bit and its preparation method, in which, the molecular structure of the material is: La2Zr2-xMxO7-delta, and M is Yb3+, Er3+, Gd3+ or Sc3+, x is 0.01-1, delta is x/2. The preparation process includes: taking La2O3, ZrO2 and Yb2O3 or Er2O3, Gd2O3 or Sc2O3 as the raw materials to match with them according to the mol ratio of each material in terms of the molecular formula and adds dispersant in light of the mass percentage of the adjuvant then to ball-mill and mix them with the adjuvant with water or alcohol as the medium to be dried to get powder to be milled, dried, screened, synthesized and heat-preserved to get the material, which is ball-milled and pressed to be sintered in 1400-1650deg.C and cooled to the room temperature to get the material.
Description
Technical field
The present invention relates to a kind of La
2Zr
2O
7Adulterated high conductivity proton conductor material in matrix Zr position and preparation method thereof belongs to the advanced ceramics material technology.
Background technology
Studies show that the pyrochlore-type material has good electric property, have required high ionic conductivity of solid electrolyte and the required high mixed conductivity of electrode materials, thereby make its ionogen that may become fuel cell or electrode materials.Zirconic acid lanthanum (La
2Zr
2O
7) be the focus of studying in the pyrrhite, particularly the electric property to it has carried out a large amount of research, its special performance makes it use in a lot of fields and has broad prospects, as: the ionogen of catalytic combustion activity agent, high temperature thermal insulation coating, Solid Oxide Fuel Cell, actinium family element fixing base etc. in the nuke rubbish.The pyrochlore-type material has chemical general formula A
2B
2O
7(wherein A, B be respectively+3 valencys and+4 valency positively charged ions), belong to isometric system, this structure can be considered to the positively charged ion (A by two kinds of different radiis
3+, B
4+) and the fluorite type structure formed of 1/8 anion vacancy.
Pyrrhite is used as heat barrier coat material for a long time.Japanese Patent (JP7130385), United States Patent (USP) (US6258467), United States Patent (USP) (US6284323), world patent (WO02/081768), European patent (EP1514953), document (MaterialsTransactions, 2004,45 (8): 2634-2637) grade has all been carried out many-sided report to this.Japanese Patent (JP6154605) has been reported a kind of La
2Zr
2O
7Preparation methods is used for the support of the catalyst of hydrocarbon combustion, and Pt family metal load is on carrier.
Pyrochlore constitution is a kind of Open architecture, can be by A atom or the B atom in other low price ion (as rare earth or alkaline-earth metal) replacement structure, adjust the relative ionic radius of A and B, increase the randomness that the structure intermediate ion is arranged, improve the vacancy concentration in the structure, finally improve the ionic conduction ability.According to its special structural performance, behind the A atom or B atom in the foreign atom replacement lattice, generation is in two kinds of oxygen rooms of different chemical environment, and the ionic conduction ability that is had can be different, so the ionic conducting property of structure can be adjusted in the controlled doping position.Zr base pyrrhite has some special electrical properties: in the oxygen atmosphere, the ionic conductivity during middle temperature (400～800 ℃) has surpassed the zirconium white of stabilized with yttrium oxide; And some oxide compound is (as La
2Zr
2O
7) under the saturated hydrogen atmosphere of water vapor, show the proton conductive behavior again, after low price ion (as Rare Earth Y or alkaline-earth metal Ca, Sr) replacement rare earth element wherein, specific conductivity increases, and proton conductivity can be compared with perovskite structure proton conductive oxide compound, but the conduction temperature is lower.Pyrrhite improves electrical property, and carries out application and development by doping vario-property, is to study focus at present.
More bibliographical information the has been arranged electrical property of pyrochlore materials is in the hope of as hydrogen pump and concentration cell.People such as Yamamura (Solid State Ionics, 2003,158 (3-4): 359-365) systematic study Ln
2Zr
2O
7The electrical property of (Ln=La, Nd, Sm, Eu, Gd, Y, Yb) system, near 800 ℃, Eu
2Zr
2O
7Specific conductivity 8.3 * 10 with system maximum
-3S/cm.The adulterated Ln of Y
2Zr
2O
7The specific conductivity of series oxide compound under the saturated hydrogen atmosphere of water vapor: unadulterated La
2Zr
2O
7Specific conductivity in the time of 1000 ℃ is approximately 4.5 * 10
-4S/cm, 10%Y reaches 2.1 * 10 with specific conductivity under the condition after mixing
-3S/cm.With the adulterated La of Y
2Zr
2O
7Be used for hydrogen or water vapor concentration cell as solid electrolyte, shown stable electromotive force; Further with La
2Zr
1.8Y
0.2O
7When being used for the electrochemistry hydrogen pump, anode hydrogen effusion rate and theoretical value meet finely, prove La
2Zr
1.8Y
0.2O
7Proton conductive.People such as Xie Yahong (Chinese Journal of Inorganic Chemistry, 2004,20 (5): 551-554) to chemical method synthetic La
1.9Ca
0.1Zr
2O
7With codope La
1.9Ca
0.1Zr
1.6Ce
0.4O
6.975Carried out the research work of ordinary-pressure synthesis of ammonia, two kinds of systems all demonstrate stable ammonia productive rate, have fully proved the proton-conductive properties of sample.(Solid State Ionics, 1996,86-88 (Part 1): 685-689 such as Shimura, Omata and Labrincha; Solid State Ionics, 1997,104 (3-4): 249-258; Solid State Ionics, 1997,99 (1-2): 33-40) use Ca
2+Doping La
2Zr
2O
7After the system, in wet hydrogen atmosphere, (La
1.95Ca
0.05) Zr
2O
7-δAnd La
2(Zr
1.985Ca
0.025) O
7-δSpecific conductivity in the time of 600 ℃ is respectively 6.8 * 10
-4S/cm and 1.0 * 10
-4S/cm, the proton shifting number that obtains by the hydrogen concentration cell approaches 1.They have also studied a series of alkaline-earth metal (Mg
2+, Ca
2+, Sr
2+, Ba
2+) adulterated La
2Zr
2O
7System shows that from the gasometry of separating out water vapor doped samples all has proton-conductive properties.(Solid State Ionics, 1995,80 (1-2): 99-110) studied Gd such as Kutty
2Zr
2O
7The structural performance of series, and measured the crystals resistance and the grain boundary resistance of system with AC impedence method, system has just shown ionic conducting property preferably under the lesser temps in air atmosphere.Gd
2Zr
2O
7Middle r
3+/ r
4+Equal 1.23, only be a bit larger tham 1.22, be in pyrochlore-type and fluorite type border, a certain amount of doping than heavy ion radius element not only can be stablized pyrochlore constitution, can also increase the unordered degree that ion is arranged, and improves ionic conductivity.Gd in the time of 600 ℃
2Zr
2O
7Total conductivity be 1.1 * 10
-4S/cm uses 20%Sr
2+After the replacement, specific conductivity has improved an order of magnitude.Ga
3+And Sb
3+Average ion radius and Ti
4Much at one.Therefore, (Solid State Ionics, 2000,134 (1-2): such as Takamura 67-73) with Gd
3+And Sb
3+The common Ti that replaces
4+, and with further replacing Gd
3+And Sb
3+Come the ionic conduction ability of improved system.As x=0.4,0.6,0.8 the time, Gd
2(GaSb)
1-xZr
2xO
7Ionic conductivity reaches 2.5 * 10 respectively in the time of 1000 ℃
-6S/cm, 3.6 * 10
-5S/cm, 2.1 * 10
-3S/cm.(Solid State Ionics, 2000,135 (1-4): 675-679) studied Pr such as Holtappels
2Zr
2O
7In the Zr position with Mn or the adulterated system of Ce, at 1000 ℃, 1%H
2/ 3%H
2O/96%N
2In the system, Pr
2Zr
1.9Mn
0.1O
7And Pr
2Zr
1.6Ce
0.4O
7Specific conductivity be respectively 1 * 10
-3S/cm and 3.6 * 10
-3S/cm, in the curve of specific conductivity and temperature, slope is bigger, has obviously shown high ionic conduction behavior.Summing up the work of above-mentioned bibliographical information, mainly is to have studied the different Ln of Ln
2Zr
2O
7Material, La
2Zr
2O
7Independent doping and minority are in the preparation and the performance of the independent dopant material in La position in the Zr position.
Summary of the invention
The object of the present invention is to provide a kind of La
2Zr
2O
7Adulterated high conductivity proton conductor material in matrix Zr position and preparation method thereof, this proton conductor material specific conductivity height, its preparation method is simple.
The present invention is realized by following technical proposals.A kind of La
2Zr
2O
7The adulterated high conductivity proton conductor material in matrix Zr position is characterized in that the molecular structural formula of this material is: La
2Zr
2-xM
xO
7-δ,
Wherein, M represents Zr position dopant ion, is Yb
3+Or Er
3+Or Gd
3+Or Sc
3+
The X value is 0.01～1;
The oxygen room that produces after the δ representative is mixed, its value is x/2.
The preparation method of above-mentioned high conductivity proton conductor material is characterized in that, comprises following process:
1. with La
2O
3, ZrO
2And Yb
2O
3Or Er
2O
3Or Gd
2O
3Or Sc
2O
3Be raw material, prepare burden by each material mol ratio according to molecular formula, and by adding dispersion agent with 0～4% of the mass percent of preparing burden, described dispersion agent is ammonium polyacrylate or polyoxyethylene glycol, water or ethanol are that medium carries out ball milling with batching and mixed 4～10 hours then, after drying powder.
2. after powder ball milling, 70～80 ℃ of oven dry, 100 orders sieve, prepare burden in 1200～1400 ℃ synthetic, soaking time 2～16 hours, synthetic material.
3. synthetic material is again after ball milling, 70～80 ℃ of oven dry, 40 orders sieve granulation, carries out the compound mould of packing into dry-pressing formed, and pressure is 50～120MPa, waits static pressure again, and pressure is 150～300MPa.
4. at 1400～1650 ℃ of sintering in air atmosphere, 2～10 ℃/minute of temperature rise rates top temperature insulation 2～50 hours, naturally cool to room temperature then.
Preparation method provided by the present invention is simple, and is with low cost, by mixing, improved the electrical property of material greatly.
Innovative point of the present invention is, has adopted the elements of not reported such as Yb to mix, and has prepared the proton conductor material of high conductivity, and its specific conductivity has surpassed the highest Y dopant material that present document is reported, 700 ℃ of proton conductivities reach 1.03 * 10
-3S/cm lays a good foundation for developing hydrogen and water vapor sensor, hydrogen pump, catalyzer and concentration cell electrolyte.
Embodiment
Embodiment 1
Get lanthanum trioxide 54.14 grams, zirconium white 32.76 grams, ytterbium oxide 13.10 grams, preparation La
2Zr
1.6Yb
0.4O
7-δ(δ=0.2).The employing ball milling mixes, and makes medium with dehydrated alcohol, 6 hours ball milling time.Dry back in 1400 ℃ synthetic, be incubated 8 hours.Dry-pressing formed (100MPa)+isostatic pressing (200MPa) moulding sample is adopted in drying, the granulation of sieving behind the ball milling once more, 1580 ℃ of sintering in air, and 3 ℃/minute of temperature rise rates are incubated 6 hours and obtain sintered compact.700 ℃ proton conductivity is 1.03 * 10 in wet hydrogen atmosphere
-3S/cm.
Embodiment 2
Get lanthanum trioxide 54.35 grams, zirconium white 32.89 grams, Erbium trioxide 12.76 grams, preparation La
2Zr
1.6Er
0.4O
7-δ(δ=0.2).The employing ball milling mixes, and makes medium with dehydrated alcohol, 6 hours ball milling time.Dry back is incubated 8 hours in 1400 ℃ of pre-synthesizing.Dry-pressing formed (100MPa)+isostatic pressing (200MPa) moulding sample is adopted in drying, the granulation of sieving behind the ball milling once more, 1600 ℃ of sintering in air, and 4 ℃/minute of temperature rise rates are incubated 2 hours and obtain sintered compact.700 ℃ proton conductivity is 4.0 * 10 in wet hydrogen atmosphere
-4S/cm.
Embodiment 3
Get lanthanum trioxide 54.72 grams, zirconium white 33.11 grams, gadolinium sesquioxide 12.18 grams, preparation La
2Zr
1.6Gd
0.4O
7-δ(δ=0.2).The employing ball milling mixes, and makes medium with dehydrated alcohol, 8 hours ball milling time.Dry back is incubated 8 hours in 1400 ℃ of pre-synthesizing.Dry-pressing formed (100MPa)+isostatic pressing (200MPa) moulding sample is adopted in drying, the granulation of sieving behind the ball milling once more, 1580 ℃ of sintering in air, and 3 ℃/minute of temperature rise rates are incubated 6 hours and obtain sintered compact.700 ℃ proton conductivity is 2.8 * 10 in wet hydrogen atmosphere
-4S/cm.
Embodiment 4
Get lanthanum trioxide 60.37 grams, zirconium white 31.96, Scium trioxide 7.67 grams, preparation La
2Zr
1.4Sc
0.6O
7-δThe employing ball milling mixes, and makes medium with dehydrated alcohol, 10 hours ball milling time.Dry back is incubated 4 hours in 1400 ℃ of pre-synthesizing.Dry-pressing formed (100MPa)+isostatic pressing (200MPa) moulding sample is adopted in drying, the granulation of sieving behind the ball milling once more, 1600 ℃ of sintering in air, and 4 ℃/minute of temperature rise rates are incubated 8 hours and obtain sintered compact.700 ℃ proton conductivity is 1.1 * 10 in wet hydrogen atmosphere
-4S/cm.
Embodiment 5
Get lanthanum trioxide 56.87 grams, zirconium white 42.80 grams, Erbium trioxide 0.33 gram, preparation La
2Zr
1.99Er
0.01O
7-δ(δ=0.005).The employing ball milling mixes, and uses water as medium, adds 4 gram ammonium polyacrylates, 4 hours ball milling time.Dry back is incubated 16 hours in 1200 ℃ of pre-synthesizing.Dry-pressing formed (50MPa)+isostatic pressing (150MPa) moulding sample is adopted in drying, the granulation of sieving behind the ball milling once more, 1400 ℃ of sintering in air, and 2 ℃/minute of temperature rise rates are incubated 10 hours and obtain sintered compact.This material has higher proton conductivity in 700 ℃ of wet hydrogen atmosphere.
Embodiment 6
Get lanthanum trioxide 62.90 grams, zirconium white 27.79 grams, Scium trioxide 13.31 grams, preparation La
2ZrScO
7-δ(δ=0.5).The employing ball milling mixes, and uses water as medium, adds 4 gram polyoxyethylene glycol (molecular weight 400), 8 hours ball milling time.Dry back is incubated 2 hours in 1400 ℃ of pre-synthesizing.Dry-pressing formed (120MPa)+isostatic pressing (300MPa) moulding sample is adopted in drying, the granulation of sieving behind the ball milling once more, 1650 ℃ of sintering in air, and 10 ℃/minute of temperature rise rates are incubated 50 hours and obtain sintered compact.This material has higher proton conductivity in 700 ℃ of wet hydrogen atmosphere.
Claims (2)
1. La
2Zr
2O
7The adulterated high conductivity proton conductor material in matrix Zr position is characterized in that the molecular structural formula of this material is: La
2Zr
2-xM
xO
7-δ,
Wherein, M represents Zr position dopant ion, is Yb
3+Or Er
3+Or Gd
3+Or Sc
3+
The X value is 0.01～1;
The oxygen room that produces after the δ representative is mixed, its value is x/2.
2. one kind prepares the described La of claim 1
2Zr
2O
7The method of the adulterated high conductivity proton conductor material in matrix Zr position is characterized in that, comprises following process:
1) with La
2O
3, ZrO
2And Yb
2O
3Or Er
2O
3Or Gd
2O
3Or Sc
2O
3Be raw material, prepare burden by each material mol ratio according to molecular formula, and by adding dispersion agent with 0～4% of the mass percent of preparing burden, described dispersion agent is ammonium polyacrylate or polyoxyethylene glycol, water or ethanol are that medium carries out ball milling with batching and mixed 4～10 hours then, after drying powder;
2) after powder ball milling, 70～80 ℃ of oven dry, 100 orders sieve, in 1200～1400 ℃ synthetic, soaking time 2～16 hours, synthetic material;
3) synthetic material is again after ball milling, 70～80 ℃ of oven dry, 40 orders sieve granulation, carries out the compound mould of packing into dry-pressing formed, and pressure is 50～120MPa, waits static pressure again, and pressure is 150～300MPa;
4) at 1400～1650 ℃ of sintering in air atmosphere, 2～10 ℃/minute of temperature rise rates top temperature insulation 2～50 hours, naturally cool to room temperature then.
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|---|---|---|---|
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|---|---|---|---|
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| CN100480186C CN100480186C (en) | 2009-04-22 |
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|---|---|---|---|---|
| CN101543732B (en) * | 2009-02-25 | 2011-03-16 | 中国科学技术大学 | Metallic oxide proton conduction material and preparation method thereof |
| CN102153892A (en) * | 2010-12-03 | 2011-08-17 | 西南科技大学 | (La, gd)2Zr2O7-(Zr, gd) O2-δcomplex phase thermal barrier coating material and its preparation method |
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| CN103172371A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Method for preparing La2O3 and Yb2O3 stabilized ZrO2 thermal barrier coating material |
| CN103396119A (en) * | 2013-08-25 | 2013-11-20 | 中国人民解放军国防科学技术大学 | Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder |
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- 2007-02-01 CN CNB2007100566885A patent/CN100480186C/en not_active Expired - Fee Related
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| CN101543732B (en) * | 2009-02-25 | 2011-03-16 | 中国科学技术大学 | Metallic oxide proton conduction material and preparation method thereof |
| CN102153892A (en) * | 2010-12-03 | 2011-08-17 | 西南科技大学 | (La, gd)2Zr2O7-(Zr, gd) O2-δcomplex phase thermal barrier coating material and its preparation method |
| CN102153892B (en) * | 2010-12-03 | 2013-04-17 | 西南科技大学 | (La, gd)2Zr2O7-(Zr, gd) O2-δcomplex phase thermal barrier coating material and its preparation method |
| CN103172371A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Method for preparing La2O3 and Yb2O3 stabilized ZrO2 thermal barrier coating material |
| CN102659403A (en) * | 2012-05-31 | 2012-09-12 | 北京科技大学 | Ceramic material for high-temperature-resistant thermal barrier coating and preparation method thereof |
| CN102719778B (en) * | 2012-06-27 | 2014-04-02 | 中国地质大学（武汉） | Nanostructured cerium-doped lanthanum zirconate spherical powder for thermal spraying and preparation method thereof |
| CN102719778A (en) * | 2012-06-27 | 2012-10-10 | 中国地质大学（武汉） | Nanostructured cerium-doped lanthanum zirconate spherical powder for thermal spraying and preparation method thereof |
| CN103396119B (en) * | 2013-08-25 | 2014-11-12 | 中国人民解放军国防科学技术大学 | Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder |
| CN103396119A (en) * | 2013-08-25 | 2013-11-20 | 中国人民解放军国防科学技术大学 | Preparation method of single-phase pyrochlore-type La2Zr2O7 nano-powder |
| CN105694113A (en) * | 2016-03-16 | 2016-06-22 | 无锡锡洲封头制造有限公司 | Composite for oval end socket |
| CN108017388A (en) * | 2017-12-11 | 2018-05-11 | 内蒙古科技大学 | A kind of air plasma spraying zirconic acid lanthanum base ceramic prilling powder and preparation method thereof |
| CN110652873A (en) * | 2019-09-26 | 2020-01-07 | 电子科技大学 | Tubular hydrogen isotope extraction pump based on barium-zirconium ceramic |
| CN111548159A (en) * | 2020-05-16 | 2020-08-18 | 中国科学院新疆理化技术研究所 | Zirconate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112661511A (en) * | 2021-01-13 | 2021-04-16 | 中国人民解放军国防科技大学 | Doped and modified rare earth zirconate powder and preparation method and application thereof |
| CN112960979A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Zirconate system high-temperature negative temperature coefficient thermistor material and preparation method thereof |
| CN115341174A (en) * | 2022-07-29 | 2022-11-15 | 中国航发北京航空材料研究院 | Lanthanum-zirconium-praseodymium-oxygen thermal barrier coating material and preparation method thereof |
| CN115341174B (en) * | 2022-07-29 | 2024-01-12 | 中国航发北京航空材料研究院 | Lanthanum zirconium praseodymium oxygen thermal barrier coating material and preparation method thereof |
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