CN101928144A - LaMgAl11O19-8YSZ complex phase ceramic and preparation method thereof - Google Patents

LaMgAl11O19-8YSZ complex phase ceramic and preparation method thereof Download PDF

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Publication number
CN101928144A
CN101928144A CN2010102698556A CN201010269855A CN101928144A CN 101928144 A CN101928144 A CN 101928144A CN 2010102698556 A CN2010102698556 A CN 2010102698556A CN 201010269855 A CN201010269855 A CN 201010269855A CN 101928144 A CN101928144 A CN 101928144A
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8ysz
lamgal
powder
preparation
high temperature
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李吉皎
房明浩
黄赛芳
黄朝晖
刘艳改
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China University of Geosciences
China University of Geosciences Beijing
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China University of Geosciences Beijing
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Abstract

The invention relates to a LaMgAl11O19-8YSZ complex phase ceramic and a preparation method thereof. In the invention, LaMgAl11O19 power and 8YSZ micro powder are used as raw materials, and the method comprises the following steps: designing components, burdening, ball milling, evenly mixing, forming and using a high-temperature solid phase method for sintering to prepare the LaMgA111O19-8YSZ complex phase ceramic materal at the temperature of 1250 DEG C-1850 DEG C. The LaMgAl11O19-8YSZ complex phase ceramic has the characteristics of high strength, large toughness, high temperature resistance and the like. The preparation method has low raw material price, good product property and the like, and is relative simple.

Description

A kind of LaMgAl 11O 19-8YSZ complex phase ceramic and preparation method thereof
Technical field:
The present invention relates to a kind of LaMgAl 11O 19-8YSZ diphase ceramic material and preparation method thereof belongs to the preparing technical field of diphase ceramic material.
Background technology:
Solid Oxide Fuel Cell (SOFC) is compared with oil engine, have the effciency of energy transfer height, product is pollution-free, security of system is high and has advantages such as modular structure, become the focus of research, it is the new-generation technology that develops rapidly the eighties in 20th century, by generally acknowledging is the green energy resource of 21 century, is representing the development trend of new energy resources system in the future.The core component of SOFC is anode, ionogen and negative electrode, and wherein ionogen plays the O that negative electrode is generated 2-Being delivered to the anodic effect, is the key part of SOFC, and battery performance is had significant effects.8YSZ (8mol%Y 2O 3Stable ZrO 2) pottery have higher ionic conductivity, low electronic migration number, good chemical stability and with the performances such as coupling of other SOFC assembly on thermal expansivity, be to study and use maximum SOFC electrolytes at present.But the mechanical property of 8YSZ material is than 3Y-TZP (3mol%Y 2O 3Stable ZrO 2) material mechanical performance is poor, very easily the different steps in assembling or work is subjected to the effect of external stress and fragmentation takes place, and it is broken that SOFC very easily takes place when assembling or operation mechanical properties decrease, causes the crossover leakage of fuel gas, reduce the performance and the efficient of battery, even cause battery-operated failure.Therefore prepare 8YSZ ionogen, become one of necessary problem that solves of current SOFC development with excellent mechanical performances and electric property.
Stupalith generally can be by adding rigid particles, fiber, whisker or the two-phase of ductile metal particle grade in an imperial examination to reach toughness reinforcing effect.MgO promotes system surface energy and partial potential to descend, and strengthens the sintering motivating force of system, and the lattice distortion that causes activation lattice possesses good wear resistance and low temperature ageing resistance, and shortcoming is that high-temperature aging resisting is bad; Al 2O 3High elastic coefficient increases the phase transformation restraint force, can stop Zr 4+Diffusion and crystal boundary migration reduce grain growth, and the removal of contamination crystal boundary solves the low-temperature performance problem of aging mutually, improve hardness, fracture toughness and the cross-breaking strength of material, but Al 2O 3Make between crystal boundary to interconnect, hinder agglomerating and carry out; SiO 2With Al 2O 3Acting in conjunction, improve the density specific conductivity decline arranged slightly but produce liquid phase activated sintering; Sm 2O 3Sm at a low price 3+Introduce, cause a large amount of oxygen room to form, make grain growing activation energy reduce density and the specific conductivity that improves material, shortcoming is to stablize crystalline phase to mix that specific conductivity has decline slightly when a small amount of.
Adopt the toughness reinforcing mode of above compound particle can't take into account performances such as complex phase ceramic intensity, fracture toughness property and hardness.
The above-mentioned complex phase ceramic of preparation adopts sintering methods such as hot pressing, high pressure at present simultaneously, and complicated process of preparation, agglomerating plant costliness are difficult to obtain complex-shaped complex phase ceramic goods, are difficult to realize industrial production in enormous quantities.
Therefore develop a kind of manufacturing technology of lower cost and under the prerequisite that guarantees 8YSZ ionogen electric property, take into account intensity and flexible LaMgAl 11O 19-8YSZ complex phase ceramic has important use and is worth and the technological innovation meaning.
Summary of the invention:
The objective of the invention is to take into account the problem of intensity, fracture toughness property and hardness, utilize LaMgAl at the 8YSZ base complex phase ceramic of some particulate reinforcement 11O 19En plaque pattern, good insulating and high elastic coefficient, a kind of employing LaMgAl is proposed 11O 19Micro mist is incorporated in the 8YSZ pottery as the second phase particle, prepares LaMgAl by the pressure less high temperature solid state sintering 11O 19The method of-8YSZ complex phase ceramic, thus reach the purpose for preparing the big 8YSZ base complex phase ceramic material of a kind of strength high toughness.
For achieving the above object, the technical scheme of this patent is as follows:
This patent relates to a kind of LaMgAl 11O 19-8YSZ complex phase ceramic is characterized in that it is by LaMgAl 11O 19Powder and 8YSZ powder under 1250 ℃～1850 ℃ the high temperature solid-state method sintering and make, the shared ratio of each component is: LaMgAl 11O 19Powder is 0.01wt.%～45wt.%, and the 8YSZ powder is 55wt.%～99.99wt.%.
The specification of quality of various raw materials is as follows when wherein preparing burden:
LaMgAl 11O 19Require purity greater than 95wt.% with the 8YSZ powder, median size is less than 20 μ m.
LaMgAl of the present invention 11O 19The preparation method of-8YSZ diphase ceramic material is characterized in that it may further comprise the steps:
1) batching: LaMgAl 11O 19Powder is 0.01wt.%～45wt.%, and the 8YSZ powder is 55wt.%～99.99wt.%;
2) batch mixing: adopt wet ball grinding to mix 2～36 hours, then at temperature range inner drying (drying plant can adopt also vacuum available drying, a conventional oven) 6～20h of 70～110 ℃;
3) moulding: at first dry-pressing formed under 10MPa～100MPa, cold isostatic compaction (also can not carry out cold isostatic compaction) under 100MPa～300MPa then;
4) sintering: adopt the high temperature solid-state method sintering, place High Temperature Furnaces Heating Apparatus to heat on sample, employed High Temperature Furnaces Heating Apparatus can adopt electrically heated kiln, combustion gas heating kiln, fuel Heating kiln, microwave oven, induction heater and the coal-fired heating kiln of air atmosphere, its sintering range is 1250 ℃～1850 ℃, soaking time is 0.5h～20h, naturally cools to room temperature at last and promptly obtains LaMgAl involved in the present invention 11O 19-8YSZ diphase ceramic material.
LaMgAl of the present invention 11O 19-8YSZ complex phase ceramic has characteristics such as high strength and toughness, high temperature resistant, and it is cheap that its preparation method has a cost of material, and can realize the preparation of complicated shape ceramic, is easy to advantages such as suitability for industrialized production.
Embodiment:
Embodiment 1
LaMgAl 11O 19The powder add-on is 5wt.%, requires LaMgAl 11O 19Powder purity is 99.9wt.%, and median size is 1 μ m, and the 8YSZ powder is that add-on is 95wt.%, and requiring 8YSZ powder purity is 99.9wt.%, and median size is 5 μ m.
At first various raw materials being packed in the ball grinder according to above-mentioned ratio, is medium with the dehydrated alcohol, carries out wet ball grinding 24h, and raw material is milled down to screen over-size less than the aperture sieve of 15 μ m less than 2.0wt.%.
Above-mentioned compound is carried out drying in rotatory evaporator, in baking oven, continued dry 4 hours and crossed 100 mesh sieves then in 100 ℃.
With the compression moulding under 30MPa of dried raw material powder, under 200MPa, carry out the closely knit processing of isostatic cool pressing then.
Sample after the moulding is placed the high temperature kiln roasting, calcining system is: at first with the heat-up rate to 1250 of 8 ℃/min ℃, be incubated two hours, then with the heat-up rate to 1550 of 5 ℃/min ℃, be incubated and naturally cool to room temperature after three hours, promptly obtain corresponding LaMgAl 11O 19-8YSZ diphase ceramic material.
The main performance index of resulting product is as follows: volume density is 5.72g/cm 3Fracture toughness property is 3.29MPam 1/2Folding strength is 206.17MPa.
Embodiment 2
LaMgAl 11O 19The powder add-on is 10wt.%, requires LaMgAl 11O 19Powder purity is 99.9wt.%, and median size is 1 μ m, and the 8YSZ powder is that add-on is 90wt.%, and requiring 8YSZ powder purity is 99.9wt.%, and median size is 5 μ m.
At first various raw materials being packed in the ball grinder according to above-mentioned ratio, is medium with the dehydrated alcohol, carries out wet ball grinding 24h, and raw material is milled down to screen over-size less than the aperture sieve of 15 μ m less than 2.0wt.%.
Above-mentioned compound is carried out drying in rotatory evaporator, in baking oven, continued dry 4 hours and crossed 100 mesh sieves then in 100 ℃.
With the compression moulding under 30MPa of dried raw material powder, under 200MPa, carry out the closely knit processing of isostatic cool pressing then.
Sample after the moulding is placed the high temperature kiln roasting, calcining system is: at first with the heat-up rate to 1250 of 8 ℃/min ℃, be incubated two hours, then with the heat-up rate to 1550 of 5 ℃/min ℃, be incubated and naturally cool to room temperature after three hours, promptly obtain corresponding LaMgAl 11O 19-8YSZ diphase ceramic material.
The main performance index of resulting product is as follows: volume density is 5.59g/cm 3Fracture toughness property is 3.27MPam 1/2Folding strength is 203.65MPa.
Embodiment 3
LaMgAl 11O 19The powder add-on is 20wt.%, requires LaMgAl 11O 19Powder purity is 99.9wt.%, and median size is 1 μ m, and the 8YSZ powder is that add-on is 80wt.%, and requiring 8YSZ powder purity is 99.9wt.%, and median size is 5 μ m.
At first various raw materials being packed in the ball grinder according to above-mentioned ratio, is medium with the dehydrated alcohol, carries out wet ball grinding 24h, and raw material is milled down to screen over-size less than the aperture sieve of 15 μ m less than 2.0wt.%.
Above-mentioned compound is carried out drying in rotatory evaporator, in baking oven, continued dry 4 hours and crossed 100 mesh sieves then in 100 ℃.
With the compression moulding under 30MPa of dried raw material powder, under 200MPa, carry out the closely knit processing of isostatic cool pressing then.
Sample after the moulding is placed the high temperature kiln roasting, calcining system is: at first with the heat-up rate to 1250 of 8 ℃/min ℃, be incubated two hours, then with the heat-up rate to 1550 of 5 ℃/min ℃, be incubated and naturally cool to room temperature after three hours, promptly obtain corresponding LaMgAl 11O 19-8YSZ diphase ceramic material.
The main performance index of resulting product is as follows: volume density is 5.35g/cm 3Fracture toughness property is 3.99MPam 1/2Folding strength is 297.38MPa.
Embodiment 4
LaMgAl 11O 19The powder add-on is 25wt.%, requires LaMgAl 11O 19Powder purity is 99.9wt.%, and median size is 1 μ m, and the 8YSZ powder is that add-on is 75wt.%, and requiring 8YSZ powder purity is 99.9wt.%, and median size is 5 μ m.
At first various raw materials being packed in the ball grinder according to above-mentioned ratio, is medium with the dehydrated alcohol, carries out wet ball grinding 24h, and raw material is milled down to screen over-size less than the aperture sieve of 0.150mm less than 2.0wt.%.
Above-mentioned compound is carried out drying in rotatory evaporator, in baking oven, continued dry 4 hours and crossed 100 mesh sieves then in 100 ℃.
With the compression moulding under 30MPa of dried raw material powder, under 200MPa, carry out the closely knit processing of isostatic cool pressing then.
Sample after the moulding is placed the high temperature kiln roasting, calcining system is: at first with the heat-up rate to 1250 of 8 ℃/min ℃, be incubated two hours, then with the heat-up rate to 1550 of 5 ℃/min ℃, be incubated and naturally cool to room temperature after three hours, promptly obtain corresponding LaMgAl 11O 19-8YSZ diphase ceramic material.
The main performance index of resulting product is as follows: volume density is 5.24g/cm 3Fracture toughness property is 3.22MPam 1/2Folding strength is 235.59MPa.

Claims (4)

1. this patent relates to a kind of LaMgAl 11O 19-8YSZ diphase ceramic material is characterized in that it is by LaMgAl 11O 19Powder and 8YSZ powder under 1250 ℃～1850 ℃ the high temperature solid-state method sintering and make, the shared ratio of each component is: LaMgAl 11O 19Powder is 0.01wt.%～45wt.%, and the 8YSZ powder is 55wt.%～99.99wt.%.
2. LaMgAl according to claim 1 11O 19-8YSZ diphase ceramic material is characterized in that: the specification of quality of each raw material is as follows during batching:
LaMgAl 11O 19Require purity greater than 95wt.% with the 8YSZ powder, median size is less than 20 μ m;
3. LaMgAl according to claim 1 11O 19The preparation method of-8YSZ diphase ceramic material is characterized in that the processing step that it comprises is: 1) batching: LaMgAl 11O 19Powder is 0.01wt.%～45wt.%, and the 8YSZ powder is 55wt.%～99.99wt.%; 2) adopt universal method batch mixing and moulding; 3) high temperature solid-state method sintering: the ceramic body after the moulding is placed on the refractory support, place High Temperature Furnaces Heating Apparatus to heat, the sintering temperature of its ceramic body is 1250 ℃～1850 ℃, insulation 0.5h～20h when the highest sintering temperature; 5) take out ceramic behind the naturally cooling, promptly obtain LaMgAl 11O 19-8YSZ complex phase ceramic.
4. LaMgAl according to claim 3 11O 19The preparation method of-8YSZ diphase ceramic material is characterized in that employed High Temperature Furnaces Heating Apparatus can adopt electrically heated kiln, combustion gas heating kiln, fuel Heating kiln, microwave oven, induction heater and coal-fired heating kiln etc.
CN2010102698556A 2010-09-01 2010-09-01 LaMgAl11O19-8YSZ complex phase ceramic and preparation method thereof Pending CN101928144A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603293A (en) * 2011-12-27 2012-07-25 中国地质大学（北京） Preparation method for high-temperature erosion and abrasion resistant LnMgAl11O19-ZrO2 composite ceramic material
CN102826837A (en) * 2012-09-12 2012-12-19 中国地质大学（北京） LaMgAl11O19-ZrO2-Al2O3 complex-phase wear-resistant ceramic material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《Journal of Alloys and Compounds》 20090417 Jiangfeng Zhanga et al. Thermal-shock resistance of LnMgAl11O19 (Ln = La, Nd, Sm, Gd) with magnetoplumbite structure 第376-381页 1-4 第482卷, *
JIANGFENG ZHANGA ET AL.: "Thermal-shock resistance of LnMgAl11O19 (Ln = La, Nd, Sm, Gd) with magnetoplumbite structure", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603293A (en) * 2011-12-27 2012-07-25 中国地质大学（北京） Preparation method for high-temperature erosion and abrasion resistant LnMgAl11O19-ZrO2 composite ceramic material
CN102826837A (en) * 2012-09-12 2012-12-19 中国地质大学（北京） LaMgAl11O19-ZrO2-Al2O3 complex-phase wear-resistant ceramic material

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Application publication date: 20101229