CN102976742A - Preparation method of single-phase monolithic ceramic Y4Al2O9 - Google Patents

Preparation method of single-phase monolithic ceramic Y4Al2O9 Download PDF

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CN102976742A
CN102976742A CN2012104470882A CN201210447088A CN102976742A CN 102976742 A CN102976742 A CN 102976742A CN 2012104470882 A CN2012104470882 A CN 2012104470882A CN 201210447088 A CN201210447088 A CN 201210447088A CN 102976742 A CN102976742 A CN 102976742A
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powder
y4al2o9
hot pressing
preparation
ceramic
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卢新坡
周延春
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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Abstract

The invention provides a preparation method of single-phase monolithic ceramic Y4Al2O9 (YAM). The method comprises the steps that: (1) Y2O3 powder and Al2O3 powder are placed in a mixing tank; deionized water is adopted as a medium; and mechanical mixing and drying are carried out; (2) the dried powder is placed into a crucible, and is treated with maintained temperature of 1200-1600 DEG C for 1-4h under an air atmosphere; (3) synthesized Y4Al2O9 ceramic powder is placed into a ball milling tank; alcohol is adopted as a medium; ball milling is carried out for 2-30h; and the material is fetched and bake-dried; and (4) the dried Y4Al2O9 ceramic powder is filled into a graphite mold, and is subjected to cold pressing for 1-5min under a pressure of 10-15MPa; the temperature is increased to 1600-2000 DEG C with a heating rate of 5-40 DEG C/min in a hot pressing furnace with an inert gas protective atmosphere, and hot pressing is carried out for 1-3h under a hot pressing pressure of 20-40MPa; and pure and compact Y4Al2O9 ceramic is finally obtained. The Y4Al2O9 (YAM) ceramic obtained by the invention has excellent performances such as high melting point, high strength, low modulus, good thermal shock resistance, low thermal conductivity, and the like.

Description

Single-phase block ceramic Y 4Al 2O 9The preparation method
Technical field
The present invention relates to the preparation method of ternary oxide pottery, be specifically related to a kind of block Y that utilizes pressure sintering to prepare compact single-phase 4Al 2O 9Method.
Background technology
The fast development of Aeronautics and Astronautics technology is faced with new challenges material and structure to the develop rapidly that the performance of material has proposed more and more higher requirement, especially hypersonic aircraft and advanced propulsion system-scramjet engine.Extreme heat, power and corrosive environment that they require material can bear hypersonic flight to face, therefore, anti-heat-insulation integrative material is the critical material of the anti-heat insulating member of hypersonic near space vehicle and heat seal assembly, and the research and development of high temperature resistant low thermal conductivity material have more and more important effect.
The advantages such as Y-Al-O system pottery has high-melting-point, lower thermal conductivity and good heat, chemical stability is good, high temperature resistance vapor corrosion more and more receive people's concern in recent years.Y-Al-O system pottery mainly comprises three kinds of phase: Y 3Al 5O 12(YAG) phase, Y 4Al 2O 9(YAM) phase and YAlO 3(YAP) phase, so far, YAG is the Y-Al-O ceramic systems of most study mutually.The people such as Zhan have studied respectively the thermal conductivity of three phases in the Y-Al-O system by the method for utilizing first principle to calculate, find that YAG, YAM and YAP have lower thermal conductivity, and the minimum (YAG:1.59Wm of the thermal conductivity of YAM wherein -1K -1, YAP:1.61Wm -1K -1, YAM:1.10Wm -1K -1), the people such as while Zhan have found to compare with YAG theoretically, and the YAM pottery has lower Young's modulus (YAG:290MPa, YAM:190MPa), illustrates that the YAM pottery should have more excellent thermal shock resistance.These excellent properties are so that YAM(Y 4Al 2O 9) in the hypersonic near space vehicle in future, have potential application as anti-heat-insulation integrative structural part, high temperature elastic sealing elements, anti-oxidant and water vapour coating.
But all the time, the YAM pottery is considered to the middle metastable phase of synthetic YAG pottery, and single-phase block YAM pottery is difficult to prepare, so the experimentally also seldom research of its calorifics and mechanical property.
Summary of the invention
The object of the present invention is to provide a kind of single-phase block Y for preparing 4Al 2O 9(YAM) method of pottery, thus Y can be studied 4Al 2O 9(YAM) performances such as the calorifics of pottery and mechanics.
Realize the technical scheme of the object of the invention: a kind of single-phase block ceramic Y 4Al 2O 9The preparation method, it comprises the steps:
(1) with Y 2O 3Powder and Al 2O 3Powder is raw material, is Y in molar ratio 2O 3: Al 2O 3=2:(0.8～1.2) weighing; Two kinds of powder are packed in the mixing tank, and take deionized water as medium, then mechanically mixing 2～30 hours takes out oven dry;
(2) powder that mixes and dry in the step (1) is packed in the alumina crucible, under air atmosphere, be warmed up to 1200～1600 ° of C and be incubated 1～4 hour with 2～20 ° of C/min, thereby synthesize single-phase Y 4Al 2O 9Ceramics powder;
(3) with the Y that is synthesized in the step (2) 4Al 2O 9Ceramics powder is put into ball grinder, take alcohol as the medium ball milling 2～30 hours, then takes out oven dry;
(4) with the Y of drying in the step (3) 4Al 2O 9Ceramics powder is packed in the graphite jig, colds pressing 1～5 minute with the pressure of 10～15MPa, and the temperature rise rate with 5～40 ° of C/min in the hot pressing furnace that is connected with protection of inert gas atmosphere rises to 1600～2000 ° of C hot pressing 1～3 hour, and hot pressing pressure is 20～40MPa; Finally obtain the Y of pure densification 4Al 2O 9Pottery.
Aforesaid a kind of single-phase block ceramic Y 4Al 2O 9The preparation method, Y in its step (1) 2O 3Powder and Al 2O 3The Powder Particle Size scope is 300～500 orders.
Aforesaid a kind of single-phase block ceramic Y 4Al 2O 9The preparation method, the described rare gas element of its step (4) is argon gas, helium or neon.
Aforesaid a kind of single-phase block ceramic Y 4Al 2O 9The preparation method, its described graphite jig inwall scribbles boron nitride.
Effect of the present invention is: the Y of gained of the present invention 4Al 2O 9(YAM) pottery has the excellent properties such as high-melting-point, high strength, low modulus, good thermal shock resistance and lower thermal conductivity, thus it the application in fields such as Aeronautics and Astronautics industry has huge potentiality as the high temperature insulation structured material.The block Y that the present invention is prepared 4Al 2O 9(YAM) ceramic diameter can reach 100mm, and can utilize the conventional mechanical processing means to be processed into difform sample, substantially satisfies the practical application of some heat insulation structural spares.
Description of drawings
Fig. 1 is the Y that the present invention prepares 4Al 2O 9(YAM) X-ray diffractogram of pottery;
Fig. 2 is the Y that the present invention prepares 4Al 2O 9(YAM) surface topography of pottery after thermal etching;
Fig. 3 is the Y that the present invention prepares 4Al 2O 9(YAM) the high-temperature elastic modulus result of pottery illustrates that prepared pottery has excellent mechanical behavior under high temperature.
Embodiment
Below in conjunction with specific embodiment to single-phase block ceramic Y of the present invention 4Al 2O 9The preparation method be further described.
Embodiment 1
A kind of single-phase block lower thermal conductivity pottery Y of the present invention 4Al 2O 9The preparation method, it comprises the steps:
(1) with size range is 300～500 purpose Y 2O 3Powder 50.0 gram and Al 2O 3Powder 11.5 gram is packed in the mixing tank, and take deionized water as medium, then mechanically mixing 2 hours is taken out and dry 3h under 80 degree;
(2) powder that mixes and dry in the step (1) is packed in the alumina crucible, under air atmosphere, be warmed up to 1200 ° of C and be incubated 4 hours with 5 ° of C/min, furnace cooling subsequently, thus synthesize single-phase Y 4Al 2O 9Ceramics powder;
(3) with the Y that is synthesized in the step (2) 4Al 2O 9Ceramics powder is put into ball grinder, take alcohol as the medium ball milling 30 hours, then takes out the lower oven dry of 50 degree 3h;
(4) with the Y of drying in the step (3) 4Al 2O 9The ceramics powder diameter of packing into is that the inwall of 50mm scribbles in the graphite jig of boron nitride (BN), colded pressing 3 minutes with the pressure of 10MPa, under the argon shield of flowing, the temperature rise rate with 5 ° of C/min in hot pressing furnace rises to 1600 ° of C hot pressing 3 hours, and hot pressing pressure is 40MPa; Finally obtain the Y of pure densification 4Al 2O 9Pottery.
The block materials that obtains is single-phase Y through X-ray diffraction analysis 4Al 2O 9(YAM) pottery is substantially without other impurity, as shown in Figure 1.The density of measuring is 96.05%, and three-point bending strength is 238.8 ± 8.2MPa, and Vickers' hardness is 10.8 ± 0.3GPa, fracture toughness property 3.2 ± 0.2MPam1/2, and Young's modulus is 201GPa.
Embodiment 2
A kind of single-phase block lower thermal conductivity pottery Y of the present invention 4Al 2O 9The preparation method, it comprises the steps:
(1) with size range is 300～500 purpose Y 2O 3Powder 65.0 gram and Al 2O 3Powder 15.6 restrains in the mixing tank of packing into, take deionized water as medium, mixes 30 hours, then takes out and oven dry under 80 degree.
(2) powder that mixes and dry in the step (1) is packed in the alumina crucible, under air atmosphere, be warmed up to 1600 ° of C and be incubated 1 hour with 20 ° of C/min, furnace cooling subsequently, thus synthesize single-phase Y 4Al 2O 9Ceramics powder;
(3) with the Y that is synthesized in the step (2) 4Al 2O 9Ceramics powder is put into ball grinder, take alcohol as the medium ball milling 2 hours, then takes out oven dry under 50 degree;
(4) with the Y of drying in the step (3) 4Al 2O 9The ceramics powder diameter of packing into is that the inwall of 50mm scribbles in the graphite jig of BN, colds pressing 1 minute with the pressure of 15MPa, and under the argon shield of flowing, the temperature rise rate with 20 ° of C/min in hot pressing furnace rises to 2000 ° of C hot pressing 1 hour, and hot pressing pressure is 20MPa; Finally obtain the Y of pure densification 4Al 2O 9Pottery.The block materials that obtains is single-phase Y through X-ray diffraction analysis 4Al 2O 9(YAM) pottery, substantially free of impurities.The density of measuring is 98.15%.
Embodiment 3
A kind of single-phase block lower thermal conductivity pottery Y of the present invention 4Al 2O 9The preparation method, it comprises the steps:
(1) with size range is 300～500 purpose Y 2O 3Powder 45.0 gram and Al 2O 3Powder 10.2 restrains in the mixing tank of packing into, take deionized water as medium, mixes 12 hours, then takes out and oven dry under 80 degree.
(2) powder that mixes and dry in the step (1) is packed in the alumina crucible, under air atmosphere, be warmed up to 1500 ° of C and be incubated 2 hours with 15 ° of C/min, furnace cooling subsequently, thus synthesize single-phase Y 4Al 2O 9Ceramics powder;
(3) with the Y that is synthesized in the step (2) 4Al 2O 9Ceramics powder is put into ball grinder, take alcohol as the medium ball milling 20 hours, then takes out oven dry under 50 degree;
(4) with the Y of drying in the step (3) 4Al 2O 9The ceramics powder diameter of packing into is that the inwall of 50mm scribbles in the graphite jig of BN, colds pressing 2 minutes with the pressure of 10MPa, and under the argon shield of flowing, the temperature rise rate with 15 ° of C/min in hot pressing furnace rises to 1800 ° of C hot pressing 1.5 hours, and hot pressing pressure is 30MPa; Finally obtain the Y of pure densification 4Al 2O 9Pottery.The block materials that obtains is single-phase Y through X-ray diffraction analysis 4Al 2O 9(YAM) pottery, substantially free of impurities.The density of measuring is 99.6% (such as Fig. 2), three-point bending strength is 252.5 ± 7.3MPa, and Vickers' hardness is 11.0 ± 0.3GPa, fracture toughness property 3.4 ± 0.2MPam1/2, Young's modulus is 204GPa, and good high temperature rigid can reach 1400 ℃ (such as Fig. 3).

Claims (4)

1. single-phase block ceramic Y 4Al 2O 9The preparation method, it is characterized in that: the method comprises the steps:
(1) with Y 2O 3Powder and Al 2O 3Powder is raw material, is Y in molar ratio 2O 3: Al 2O 3=2:(0.8～1.2) weighing; Two kinds of powder are packed in the mixing tank, and take deionized water as medium, then mechanically mixing 2～30 hours takes out oven dry;
(2) powder that mixes and dry in the step (1) is packed in the alumina crucible, under air atmosphere, be warmed up to 1200～1600 ° of C and be incubated 1～4 hour with 2～20 ° of C/min, thereby synthesize single-phase Y 4Al 2O 9Ceramics powder;
(3) with the Y that is synthesized in the step (2) 4Al 2O 9Ceramics powder is put into ball grinder, take alcohol as the medium ball milling 2～30 hours, then takes out oven dry;
(4) with the Y of drying in the step (3) 4Al 2O 9Ceramics powder is packed in the graphite jig, colds pressing 1～5 minute with the pressure of 10～15MPa, and the temperature rise rate with 5～40 ° of C/min in the hot pressing furnace that is connected with protection of inert gas atmosphere rises to 1600～2000 ° of C hot pressing 1～3 hour, and hot pressing pressure is 20～40MPa; Finally obtain the Y of pure densification 4Al 2O 9Pottery.
2. a kind of single-phase block ceramic Y according to claim 1 4Al 2O 9The preparation method, it is characterized in that: Y in the step (1) 2O 3Powder and Al 2O 3The Powder Particle Size scope is 300～500 orders.
3. a kind of single-phase block ceramic Y according to claim 1 4Al 2O 9The preparation method, it is characterized in that: the described rare gas element of step (4) is argon gas, helium or neon.
4. a kind of single-phase block ceramic Y according to claim 1 4Al 2O 9The preparation method, it is characterized in that: described graphite jig inwall scribbles boron nitride.
CN2012104470882A 2012-11-09 2012-11-09 Preparation method of single-phase monolithic ceramic Y4Al2O9 Pending CN102976742A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553615A (en) * 2013-08-28 2014-02-05 航天材料及工艺研究所 Method for preparing YAM ceramic through loose sintering technology
CN105481361A (en) * 2015-12-30 2016-04-13 中国工程物理研究院化工材料研究所 YAM low-dielectric microwave dielectric ceramics and preparation method thereof
CN106007728A (en) * 2016-05-19 2016-10-12 航天材料及工艺研究所 Thermal-shock-resistant ultrahigh-temperature ceramic and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1398817A (en) * 2002-08-28 2003-02-26 中国科学院上海硅酸盐研究所 Prepn of ion doped yttrium aluminium garnet nano-powder
CN101486574A (en) * 2009-03-03 2009-07-22 陕西科技大学 Method for preparing YAG transparent ceramic powder by solid-phase reaction
JP2011037691A (en) * 2009-08-18 2011-02-24 Toshiba Corp Highly heat-conductive aluminum nitride sintered compact, substrate using this, circuit board, semiconductor device, and method for manufacturing highly heat-conductive aluminum nitride sintered compact

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1398817A (en) * 2002-08-28 2003-02-26 中国科学院上海硅酸盐研究所 Prepn of ion doped yttrium aluminium garnet nano-powder
CN101486574A (en) * 2009-03-03 2009-07-22 陕西科技大学 Method for preparing YAG transparent ceramic powder by solid-phase reaction
JP2011037691A (en) * 2009-08-18 2011-02-24 Toshiba Corp Highly heat-conductive aluminum nitride sintered compact, substrate using this, circuit board, semiconductor device, and method for manufacturing highly heat-conductive aluminum nitride sintered compact

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《硅酸盐学报》 20101215 李长青等 "Y2O3-Al2O3粉体固相反应制备Y-Al-O体系陶瓷的对比研究" 第38卷, 第12期 *
李长青等: ""Y2O3-Al2O3粉体固相反应制备Y-Al-O体系陶瓷的对比研究"", 《硅酸盐学报》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553615A (en) * 2013-08-28 2014-02-05 航天材料及工艺研究所 Method for preparing YAM ceramic through loose sintering technology
CN103553615B (en) * 2013-08-28 2015-05-27 航天材料及工艺研究所 Method for preparing YAM ceramic through loose sintering technology
CN105481361A (en) * 2015-12-30 2016-04-13 中国工程物理研究院化工材料研究所 YAM low-dielectric microwave dielectric ceramics and preparation method thereof
CN106007728A (en) * 2016-05-19 2016-10-12 航天材料及工艺研究所 Thermal-shock-resistant ultrahigh-temperature ceramic and preparation method thereof
CN106007728B (en) * 2016-05-19 2019-01-25 航天材料及工艺研究所 A kind of anti-thermal shock superhigh temperature ceramics and preparation method thereof

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Application publication date: 20130320