CN101397207A - Aluminium titanate base high temperature structural composite material and preparation method thereof - Google Patents

Aluminium titanate base high temperature structural composite material and preparation method thereof Download PDF

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Publication number
CN101397207A
CN101397207A CNA2008101779455A CN200810177945A CN101397207A CN 101397207 A CN101397207 A CN 101397207A CN A2008101779455 A CNA2008101779455 A CN A2008101779455A CN 200810177945 A CN200810177945 A CN 200810177945A CN 101397207 A CN101397207 A CN 101397207A
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China
Prior art keywords
composite material
high temperature
aluminium
structural composite
aluminium titanate
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CNA2008101779455A
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Chinese (zh)
Inventor
王志发
卜景龙
王榕林
贾翠
张利芳
周琳琳
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Hebei University of Science and Technology
Hebei Polytechnic University
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Hebei University of Science and Technology
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Priority to CNA2008101779455A priority Critical patent/CN101397207A/en
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Abstract

The invention relates to an aluminium titanate based high temperature structure composite material and a preparation method thereof, and pertains to the ceramic material field. The raw materials of the composite material and the weight percent thereof are: aluminium titanate powder, 90-98%; zirconium titanate powder, 2-10%. The grain diameter of the used raw material is less than 0.074 mm. The method for preparing the composite material is that: after being measured and proportioned, the raw materials are mixed in dryness for one minute, then 6% (weight percentage) of polyvinyl alcohol solution bonding agent with 0.5% of mass concentration is added, after being stirred for 5 minutes, the aging mixture is let stand for 5 hours so as to obtain the shaping blank; pressing and shaping are carried out on the blank by adopting a hydraulic press or a friction press, the shaping pressure of the blank is 70-100MPa; after shaping, heat retaining at more than or equal to 1500 DEG C for three hours and sintering are carried out on the blank, and the aluminium titanate based composite material with high temperature resistance, excellent thermal shock resistance and higher intensity is obtained. The composite material can be used in the fields such as metallurgy, automobile, aerospace, etc.

Description

A kind of aluminium titanate base high temperature structural composite material and preparation method thereof
Technical field
The invention belongs to the stupalith field, be specifically related to a kind of aluminium titanate base high temperature structural composite material and preparation method thereof.
Background technology
The present invention is a kind of aluminium titanate base (Al that can be used for fields such as metallurgy, automobile, space flight of exploitation 2TiO 5-ZrTiO 4) high temperature structural composite material.This matrix material is to be principal constituent with the aluminium titanates, is composited with a spot of zirconia titanate, and this matrix material has good high Warm performance, Strong degree and heat-shock resistance.
Aluminium titanates (Al 2TiO 5) stupalith has high fusing point (1860 ℃), in room temperature~1000 ℃ temperature range, aluminium titanates has low thermalexpansioncoefficient (α less than zero, or approach zero), is present only low bulk, dystectic thermal shock resistant ceramic material.
Aluminum titanate ceramic material has two shortcomings: the one, and the thermal dilation difference of each crystallographic axis of aluminium titanates crystal is bigger, causes aluminium titanates to produce tiny crack when cooling, so the physical strength of material of aluminum titanate is lower, strength at normal temperature is lower than 20MPa; The 2nd, high temperature synthetic aluminium titanates is cooled to 900 ℃~1300 ℃ instabilities, resolves into rutile (TiO 2) and corundum (α-Al 2O 3), and lost low expansion character.In the synthetic batching of aluminium titanates, introduce SiO 2, MgO, ZrO 2, Fe 2O 3Deng stablizer, the temperature decomposition is effectively suppressed in the aluminium titanates, and its intensity also makes moderate progress.At present, aluminum titanate ceramic material has been applied to tooth section Stainless Steel Alloy smelting pot, non-ferrous metal aluminum smelting technology crucible, cast aluminium riser pipe, float glass flow liquid flashboard, automobile exhaust purifier carrier etc.Increase (about strength at normal temperature 30MPa) though introduce its intensity of material of aluminum titanate of stablizer, but still belong to, limited the further application of material of aluminum titanate in fields such as ferrous metallurgy, space flight than the low strength stupalith.
Zirconia titanate (ZrTiO 4) be inconsistent fusing compound, peritectic temperature is 1900 ℃.Zirconia titanate has high strength, low-dielectric loss, reaches good temperature stability, is the important electron ceramic material of preparation electrical condenser, piezoelectric transducer and micro-wave dielectric resonator.Yet the good resistance to elevated temperatures of zirconia titanate material does not obtain to pay close attention in the high-temperature structural material field, does not see research and the application report that has zirconia titanate to be used for the high-temperature structural material aspect both at home and abroad as yet.
Material of aluminum titanate and zirconia titanate material is compound, utilize high temperature resistant, the low expansion character of aluminium titanates, and high temperature resistant, the high-strength characteristic of zirconia titanate material, prepare a kind of high temperature resistant, anti-thermal shock is good, the Strong degree is higher aluminium titanate base (Al 2TiO 5-ZrTiO 4) high temperature structural composite material, for industrial circles such as iron and steel and nonferrous metallurgy, space flight provide a kind of new type high temperature structured material.Research does not appear in the newspapers as yet with being applied in both at home and abroad in this respect.
Summary of the invention
Goal of the invention of the present invention is above-mentioned deficiency of the prior art, and a kind of high temperature resistant, anti-thermal shock is good, the Strong degree is higher aluminium titanate base high temperature structural material and preparation method thereof is provided.
A kind of aluminium titanate base high temperature structural composite material is characterized in that this matrix material weight percent raw materials used and raw material is: metatitanic acid aluminium powder 90~98%; Metatitanic acid zirconium powder 2~10%.
Particle diameter<0.074mm that this matrix material is raw materials used.
The weight percent content of the raw materials used purity of this matrix material is: the Al in the metatitanic acid aluminium powder 2TiO 5〉=90%; ZrTiO in the metatitanic acid zirconium powder 4〉=90%.
The preparation method of this matrix material is: with do to mix behind metatitanic acid aluminium powder and the metatitanic acid zirconium powder batching 1 minute, and added mass concentration then is 0.5% polyvinyl alcohol solution bonding 6% (weight percent), stirs to leave standstill ageing mixture 5h behind the 5min and obtain shaping blank; Obtain aluminium titanate base high temperature structural composite material through pressure forming, sintering.
The forming method of this matrix material is: adopt hydraulic press or friction press that blank is pressed, moulding pressure is 70~100MPa.The forming method of this matrix material also comprises: isostatic pressing, hot die-casting molding, injection forming, roll-forming, extrusion under vacuum or gel casting forming.
The sintering method of this matrix material is: employing electric furnace agglomerating temperature 〉=1500 ℃ is incubated 3 hours.The sintering method of this matrix material also comprises: hot pressed sintering, high-temperature vacuum sintering or high temperature nitrogen sintering.
The composition of aluminium titanate base high temperature structural composite material of the present invention and structure Design thinking are:
At Al 2O 3-TiO 2-ZrO 2In the three-part system, ZrO 2-Al 2TiO 5-Al 2O 3The subsystem eutectic temperature is 1610 ℃, ZrO 2-Al 2TiO 5-ZrTiO 4The subsystem eutectic temperature is 1590 ℃, Al 2TiO 5-ZrTiO 4-TiO 2The eutectic temperature of subsystem is 1580 ℃, and the composition position of three eutectic temperature points is in Al substantially 2TiO 5Content is in 50%~70% the scope, therefore prepares Al 2TiO 5-ZrTiO 4Composite diphase material, it forms point should be away from three eutectoid point positions, and at Al 2O 3-TiO 2-ZrO 2The ZrTiO of ternary phase diagrams 4Form point and Al 2TiO 5Form on the line of point.
At Al 2TiO 5Form point to ZrTiO 4Form on the composition line of point, from Al 2TiO 5With ZrTiO 4Mass ratio be 90: 10 to Al 2TiO 5Form in the scope of point, all belong to the high-temperature zone of liquidus line more than 1800 ℃.So in above proportional range, prepare burden, can obtain resistant to elevated temperatures Al 2TiO 5-ZrTiO 4Matrix material.Test preparation aluminium titanate base (Al 2TiO 5-ZrTiO 4) batching of high temperature structural composite material forms and to be defined as nearly Al 2TiO 5The high-temperature area of end.
In sum, the present invention is according to the good characteristic of material of aluminum titanate and zirconia titanate material, at aluminium titanates is to introduce a spot of zirconia titanate in the principal constituent material, and the preparation aluminium titanate base high temperature structural composite material obtains to have the new type high temperature structural ceramic material of high temperature resistant, high strength, anti-thermal shock.This matrix material is expected to be applied to ferrous metallurgy and waters the steel system, and field such as nonferrous metallurgy, glass, automobile exhaust purifier, space flight, military project.To the research and the application of aluminium titanate base high temperature structural composite material, still belong to blank at home at present.
Embodiment
Embodiment 1
Batching is formed: the metatitanic acid aluminium powder 98% of particle diameter<0.74mm, the metatitanic acid zirconium powder 2% of particle diameter<0.074mm.
With do to mix behind metatitanic acid aluminium powder and the metatitanic acid zirconium powder batching 1 minute, and added mass concentration then is 0.5% polyvinyl alcohol solution bonding 6% (weight percent), stirs to obtain shaping blank after leaving standstill ageing mixture 5h behind the 5min.Adopt hydraulic press to carry out the sample moulding shaping blank, sample moulding pressure is 100MPa.Adopt the electric furnace sintered specimen under the atmospheric air condition, sintering temperature is 1500 ℃, and soaking time is 3h.
The volume density of burning back aluminium titanate base high temperature structural composite material sample is 3.32g/cm -3, folding strength is 44.6MPa, thermalexpansioncoefficient is 1.2 * 10 -6/ ℃ (room temperature~1000 ℃), the thermal shock fatigue number of times is 25 times (cooling of 1100 ℃~air at room temperature).
Embodiment 2
Batching is formed: the metatitanic acid aluminium powder 95% of particle diameter<0.74mm, the metatitanic acid zirconium powder 5% of particle diameter<0.074mm.
With do to mix behind metatitanic acid aluminium powder and the metatitanic acid zirconium powder batching 1 minute, and added mass concentration then is 0.5% polyvinyl alcohol solution bonding 6% (weight percent), stirs to obtain shaping blank after leaving standstill ageing mixture 5h behind the 5min.Adopt hydraulic press to carry out the sample moulding shaping blank, sample moulding pressure is 100MPa.Adopt the electric furnace sintered specimen under the atmospheric air condition, sintering temperature is 1500 ℃, and soaking time is 3h.
The volume density of burning back aluminium titanate base high temperature structural composite material sample is 3.37g/cm -3, folding strength is 48.2MPa, thermalexpansioncoefficient is 1.5 * 10 -6/ ℃ (room temperature~1000 ℃), the thermal shock fatigue number of times is 21 times (cooling of 1100 ℃~air at room temperature).
Embodiment 3
Batching is formed: the metatitanic acid aluminium powder 92% of particle diameter<0.74mm, the metatitanic acid zirconium powder 8% of particle diameter<0.074mm.
With do to mix behind metatitanic acid aluminium powder and the metatitanic acid zirconium powder batching 1 minute, and added mass concentration then is 0.5% polyvinyl alcohol solution bonding 6% (weight percent), stirs to obtain shaping blank after leaving standstill ageing mixture 5h behind the 5min.Adopt hydraulic press to carry out the sample moulding shaping blank, sample moulding pressure is 100MPa.Adopt the electric furnace sintered specimen under the atmospheric air condition, sintering temperature is 1500 ℃, and soaking time is 3h.
The volume density of burning back aluminium titanate base high temperature structural composite material sample is 3.41g/cm -3, folding strength is 57.9MPa, thermalexpansioncoefficient is 1.9 * 10 -6/ ℃ (room temperature~1000 ℃), the thermal shock fatigue number of times is 19 times (cooling of 1100 ℃~air at room temperature).

Claims (6)

1, a kind of aluminium titanate base high temperature structural composite material is characterized in that this matrix material weight percent raw materials used and raw material is: metatitanic acid aluminium powder 90~98%; Metatitanic acid zirconium powder 2~10%.
2, aluminium titanate base high temperature structural composite material according to claim 1 is characterized in that raw materials used particle diameter<0.074mm.
3, aluminium titanate base high temperature structural composite material according to claim 1 is characterized in that the weight percent content of raw materials used purity is: the A1 in the metatitanic acid aluminium powder 2TiO 5Amount 〉=90%; ZrTiO in the metatitanic acid zirconium powder 4〉=90%.
4, a kind of preparation method of aluminium titanate base high temperature structural composite material according to claim 1, it is characterized in that: mixed 1 minute doing behind metatitanic acid aluminium powder and the metatitanic acid zirconium powder batching, add mass concentration then and be 0.5% polyvinyl alcohol solution bonding 6% (weight percent), leave standstill ageing mixture 5h acquisition shaping blank after stirring 5min, obtain aluminium titanate base high temperature structural composite material through pressure forming, sintering.
5, as the preparation method of aluminium titanate base high temperature structural composite material as described in the claim 4, it is characterized in that: adopt hydraulic press or friction press that blank is pressed, moulding pressure is 70~100MPa.The forming method of this matrix material also comprises: isostatic pressing, hot die-casting molding, injection forming, roll-forming, extrusion under vacuum or gel casting forming.
6, as the preparation method of aluminium titanate base high temperature structural composite material as described in the claim 4, it is characterized in that: adopt electric furnace agglomerating temperature 〉=1500 ℃, be incubated 3 hours.The sintering method of this matrix material also comprises: hot pressed sintering, high-temperature vacuum sintering or high temperature nitrogen sintering.
CNA2008101779455A 2008-11-19 2008-11-19 Aluminium titanate base high temperature structural composite material and preparation method thereof Pending CN101397207A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114477999A (en) * 2022-03-28 2022-05-13 泰州市宏华冶金机械有限公司 Preparation method of thermal shock resistant Al2TiO5-Ti3AlC2 ceramic
CN114538918A (en) * 2022-03-28 2022-05-27 泰州市宏华冶金机械有限公司 Preparation method of composite material ceramic cushion block for metallurgical industry

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114477999A (en) * 2022-03-28 2022-05-13 泰州市宏华冶金机械有限公司 Preparation method of thermal shock resistant Al2TiO5-Ti3AlC2 ceramic
CN114538918A (en) * 2022-03-28 2022-05-27 泰州市宏华冶金机械有限公司 Preparation method of composite material ceramic cushion block for metallurgical industry
CN114477999B (en) * 2022-03-28 2022-09-20 泰州市宏华冶金机械有限公司 Preparation method of thermal shock resistant Al2TiO5-Ti3AlC2 ceramic
CN114538918B (en) * 2022-03-28 2022-11-01 泰州市宏华冶金机械有限公司 Preparation method of composite material ceramic cushion block for metallurgical industry

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Open date: 20090401