CN102295455A - Preparation method of LaAlO3 ceramic substrate material - Google Patents
Preparation method of LaAlO3 ceramic substrate material Download PDFInfo
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- CN102295455A CN102295455A CN2011101525855A CN201110152585A CN102295455A CN 102295455 A CN102295455 A CN 102295455A CN 2011101525855 A CN2011101525855 A CN 2011101525855A CN 201110152585 A CN201110152585 A CN 201110152585A CN 102295455 A CN102295455 A CN 102295455A
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- powder
- laalo
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- ceramic
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Abstract
The invention relates to a LaAlO3 ceramic substrate material and a preparation method thereof, and belongs to the technical field of special ceramic manufacture technology. In the invention, high-purity alpha-Al2O3 and La2O3 are employed as raw materials and prepared into the LaAlO3 ceramic substrate material at a low temperature by a solid phase sintering method. Aiming at a problem that a prior crystal growth technology still needs expensive equipment, a long production period and high costs, and is not apt to preparation of a large size crystal, the invention provides a polycrystalline ceramic preparation technology, which employs the La2O3 ceramic material as a film substrate for high temperature superconductivity, ferroelectric and semiconductor, etc., to broaden substrate material varieties.
Description
Technical field
The present invention relates to a kind of LaAlO
3Ceramic substrate material and technology of preparing thereof belong to the special cermacis manufacturing process technology field.
Background technology
LaAlO
3Has perovskite structure.LaAlO
3Crystal is pseudo-cubic structure, belongs to trigonal system, and spacer is R3M, at high temperature forms isometric system.Transformation temperature from the trigonal system of room temperature to the pyritous isometric system is 25 ℃ of 435 scholars.
LaAlO
3Crystalline specific inductivity higher (ε=25), dielectric loss is very low (under the room temperature less than 5 * 10
-4), be suitable as very much the substrate material of high-temperature superconductor microwave device, especially as the substrate material of high-temperature superconducting thin film.Although some other crystalline material also can be used as the film-substrate of high-temperature superconductor, weigh LaAlO with overall targets such as lattice match, thermal expansivity, chemical stability, specific inductivity and losses
3Crystal has its unique status in the high-temperature superconductor substrate material.
Simultaneously, because its excellent lattice matching and lower thermal expansivity (9.2 * 10
-6K), LaAlO
3Or a kind of extraordinary ferroelectric membranc substrate material.Especially use the sedimentary method of chemical solution at LaAlO
3(001) SFMO (Sr that grows on the substrate
2FeMoO
6) ferroelectric membranc, its Curie temperature obviously reduces.In addition, people such as J.J. Lee is also at LaAlO
3On crystalline (001) the face substrate with molecular beam epitaxial growth the GaN semiconductor material of wurtzite, its lattice mismatch only differs 3%.So LaAlO
3Crystal also is a kind of very promising GaN thin film substrate material.This has widened LaAlO
3The range of application of substrate material.
But, above said all be about LaAlO
3Crystal is as the research of substrate material.And about LaAlO
3The ceramic substrate material is not reported at present as yet.Because the crystal growth cycle is long, and utilization ratio is not high, compare with crystal, stupalith can carry out sintering being lower than under the temperature of fusing point, cost is low, the efficient height, easily processing, large size and complex-shaped sample can be made, and the heavy doping and the adulterated homogeneity of active ion, suitable batch production can be realized.
Summary of the invention
Based on present crystal growth technique also need expensive equipment, production cycle long, cost is high, is difficult for the preparation large size.The special proposition of the present invention adopted polycrystalline ceramics preparation technology, uses LaAlO
3Stupalith is as high-temperature superconductor, the substrate of films such as ferroelectric and semi-conductor, the kind that has expanded substrate material.
The present invention adopts high-purity α Al
2O
3, La
2O
3Powder is a raw material, under lower temperature conditions, adopts solid sintering technology to prepare LaAlO
3The ceramic substrate material.
The present invention is a kind of LaAlO
3The ceramic substrate preparation methods is characterized in that it has following technological process and step:
(1), LaAlO
3The preparation of ceramic powder
A. adopt high-purity 99.95% Al
2O
3With 99.99% La
2O
3Be raw material, carry out weigh batching according to both mol ratios in the chemical formula; Al wherein
2O
3With La
2O
3Mol ratio be 1:1;
B. will be by the good Al of above-mentioned formulated
2O
3Powder and La
2O
3Powder is put into ball grinder and is carried out ball milling, and ratio of grinding media to material is 2:1, and the mass ratio of etoh solvent and powder is 2:1; The ball grinder rotating speed is 50 rev/mins, and the ball milling time is 24h;
C. ball milling is good powder takes out, granulation;
D. powder mix is calcined in retort furnace, sintering temperature is 1200 degrees centigrade, obtains LaAlO
3Powder;
(2), LaAlO
3The preparation of pottery
A. with the above-mentioned LaAlO that sinters
3Ceramic powder is put into ball grinder, carries out ball milling; The ball grinder rotating speed is 50 rev/mins, and the ball milling time is 24h;
B. ball milling is good powder takes out, granulation;
C. dry-pressing formed; Depress to sample in the 200MPa isostatic cool pressing;
D. sample is calcined at vacuum oven, 1750 degrees centigrade of sintering temperatures finally obtain LaAlO
3Pottery.
The present invention's high pure raw material adopts ceramic process to prepare LaAlO
3The ceramic substrate material.Material preparation process of the present invention is simple, and low cost of manufacture helps realizing industrial scale production.
Description of drawings
Fig. 1 is LaAlO among the present invention
3Powder and the pottery XRD figure.
Fig. 2 is LaAlO among the present invention
3The micro-structure diagram of pottery.
Embodiment
After now specific embodiments of the invention being described in.
(1), LaAlO
3The preparation of ceramic powder
Obtained well behaved with Al by powder preparing technology
2O
3And La
2O
3LaAlO for raw material
3Ceramic powder, its preparation method is as follows:
A. adopt high-purity 99.95% Al
2O
3With 99.99% La
2O
3Be raw material, carry out weighing, batching according to both mol ratios in the chemical formula; Al wherein
2O
3With La
2O
3Mol ratio be 1:1;
B. the Al that will obtain by said ratio
2O
3Powder and La
2O
3Powder is put into ball grinder and is carried out ball milling, and ratio of grinding media to material is 2:1, and the mass ratio of etoh solvent and powder is 2:1; The ball grinder rotating speed is 50 rev/mins, and the ball milling time is 24h;
C. ball milling is good powder is dried under 95 degree celsius temperature, takes out granulation;
D. powder mix is calcined in retort furnace, sintering temperature is 1200 degrees centigrade, obtains LaAlO
3Powder;
(2), LaAlO
3The preparation of pottery
A. with the above-mentioned LaAlO that sinters
3Ceramic powder is put into ball grinder, carries out ball milling; The rotating speed of ball grinder is 50 rev/mins, and the ball milling time is 24h;
B. ball milling is good powder is dried under 95 degree celsius temperature, takes out granulation;
C. dry-pressing formed; Depress to sample in the 200MPa isostatic cool pressing;
D. sample is calcined at vacuum oven, 1750 degrees centigrade of sintering temperatures finally obtain LaAlO
3Pottery.
The present invention's high pure raw material adopts ceramic process to prepare LaAlO
3The ceramic substrate material.Material preparation process of the present invention is simple, and low cost of manufacture helps realizing industrial scale production.The LaAlO of gained of the present invention
3The powder crystallinity is good, and inclusion-free.Fig. 1 is prepared LaAlO
3The XRD figure of powder and pottery, as seen from the figure, powder is consistent with the PDF card (JCPDS card 31-0022) of XRD diffraction peak and the standard of pottery, and the nothing peak of mixing.Fig. 2 is LaAlO
3The micro-structure diagram of pottery.As shown in Figure 2, LaAlO
3Ceramic structure is very fine and close, uniform crystal particles, and the residue pore is few, and crystal grain is no abnormal grows up.
Claims (1)
1. LaAlO
3The ceramic substrate preparation methods is characterized in that it has following technological process and step:
(1), LaAlO
3The preparation of ceramic powder
Adopt high-purity 99.95% Al
2O
3With 99.99% La
2O
3Be raw material, carry out weigh batching according to both mol ratios in the chemical formula; Al wherein
2O
3With La
2O
3Mol ratio be 1:1;
Will be by the good Al of above-mentioned formulated
2O
3Powder and La
2O
3Powder is put into ball grinder and is carried out ball milling, and ratio of grinding media to material is 2:1, and the mass ratio of etoh solvent and powder is 2:1, and the ball grinder rotating speed is 50 rev/mins, and the ball milling time is 24h;
The powder that ball milling is good takes out, granulation;
Powder mix is calcined in retort furnace, and 1200 degrees centigrade of sintering temperatures obtain LaAlO
3Powder;
(2), LaAlO
3The preparation of pottery
A. with the above-mentioned LaAlO that sinters
3Ceramic powder is put into ball grinder, carries out ball milling; The ball grinder rotating speed is 50 rev/mins, and the ball milling time is 24h;
B. ball milling is good powder takes out, granulation;
C. dry-pressing formed; Depress to sample in the 200MPa isostatic cool pressing;
D. sample is calcined at vacuum oven, 1750 degrees centigrade of sintering temperatures finally obtain LaAlO
3Pottery.
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|---|---|---|---|
| CN2011101525855A CN102295455A (en) | 2011-06-09 | 2011-06-09 | Preparation method of LaAlO3 ceramic substrate material |
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|---|---|---|---|
| CN2011101525855A CN102295455A (en) | 2011-06-09 | 2011-06-09 | Preparation method of LaAlO3 ceramic substrate material |
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| CN102295455A true CN102295455A (en) | 2011-12-28 |
Family
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701723A (en) * | 2012-06-21 | 2012-10-03 | 上海大学 | Preparation method of Ce-doped LaAlO3 flickering ceramic material |
Citations (4)
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|---|---|---|---|---|
| CN1974484A (en) * | 2006-12-15 | 2007-06-06 | 重庆工学院 | Microwave dielectric ceramic and its prepn process |
| CN101182196A (en) * | 2007-11-21 | 2008-05-21 | 内蒙古科技大学 | Method for preparing magnesium-based lanthanum aluminate thermal barrier coating |
| CN101280459A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method of lanthanum aluminate crystal |
| CN101935208A (en) * | 2010-08-06 | 2011-01-05 | 中国科学院理化技术研究所 | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof |
-
2011
- 2011-06-09 CN CN2011101525855A patent/CN102295455A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974484A (en) * | 2006-12-15 | 2007-06-06 | 重庆工学院 | Microwave dielectric ceramic and its prepn process |
| CN101182196A (en) * | 2007-11-21 | 2008-05-21 | 内蒙古科技大学 | Method for preparing magnesium-based lanthanum aluminate thermal barrier coating |
| CN101280459A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method of lanthanum aluminate crystal |
| CN101935208A (en) * | 2010-08-06 | 2011-01-05 | 中国科学院理化技术研究所 | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof |
Non-Patent Citations (6)
| Title |
|---|
| 《J. Am.Ceram. Soc.》 20001231 Qiwu Zhang et cl. "Mechanochemical Synthesis of Lanthanum Aluminate by Grinding Lanthanum Oxide with Transition Alumina" 第83卷, 第2期 * |
| 《影像科学与光化学》 20091130 莎仁 等 "纳米晶LaAlO3掺Eu3+的复合沉淀法" 第27卷, 第6期 * |
| 《粉末冶金技术》 20091031 田丁 等 "铝酸镧超细粉体的制备方法" 第27卷, 第5期 * |
| QIWU ZHANG ET CL.: ""Mechanochemical Synthesis of Lanthanum Aluminate by Grinding Lanthanum Oxide with Transition Alumina"", 《J. AM.CERAM. SOC.》, vol. 83, no. 2, 31 December 2000 (2000-12-31) * |
| 田丁 等: ""铝酸镧超细粉体的制备方法"", 《粉末冶金技术》, vol. 27, no. 5, 31 October 2009 (2009-10-31) * |
| 莎仁 等: ""纳米晶LaAlO3掺Eu3+的复合沉淀法"", 《影像科学与光化学》, vol. 27, no. 6, 30 November 2009 (2009-11-30) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701723A (en) * | 2012-06-21 | 2012-10-03 | 上海大学 | Preparation method of Ce-doped LaAlO3 flickering ceramic material |
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Application publication date: 20111228 |