CN1587187A - Lanthanum hafnate base transparent ceramics and its preparing method - Google Patents
Lanthanum hafnate base transparent ceramics and its preparing method Download PDFInfo
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- CN1587187A CN1587187A CN 200410053428 CN200410053428A CN1587187A CN 1587187 A CN1587187 A CN 1587187A CN 200410053428 CN200410053428 CN 200410053428 CN 200410053428 A CN200410053428 A CN 200410053428A CN 1587187 A CN1587187 A CN 1587187A
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Abstract
The present invention relates to lanthanum hafnate base transparent ceramic and its preparation process, and belongs to the field of ceramic technology. The present invention features that that the transparent ceramic has the composition of La2-2xRE2xHf2O7, where x is 0-0.1, x=0 means pure lanthanum hafnate, and RE is Ce, Pr, Eu, Tm, Tb or other RE ion. By means of hot compression, hot isostatic pressing, vacuum and hydrogen atmosphere sintering process, the said material may be prepared into excellent transparent ceramic. The transparent ceramic of the present invention has density, strong ray absorbing capacity, and maximum transparency in visible light band higher than 70 % when the ceramic of 1 mm thickness is polished. The present invention has latent application in radiation detection, laser material and other fields.
Description
Technical field
The present invention relates to a kind of hafnium acid lanthanum base transparent ceramic and preparation method thereof, belong to the crystalline ceramics field.
Background technology
Successfully prepare translucent alumina-ceramic (U.S.P.3026210) from R.L.Coble reported first in 1962, opened up the new Application Areas of stupalith.The development people that pass through decades can prepare the crystalline ceramics of excellent in optical properties, and the optical property of some crystalline ceramics has reached the suitable level of monocrystalline, and performances such as mechanics then obviously are better than monocrystalline.Crystalline ceramics has become a kind of important optical material and has obtained application in fields such as high temperature form, radiation detection, laser mediums.
Developed Yttralox:Nd (1973) [C.Greskovich at present, J.P.Chernoch.J.Appl.Phys., 1973,44 (10): 4599-4603.], YAG:Nd[A.Ikesue, T.Kinoshita, K.Kamata, et al., J.Am.Ceramic Soc., 1995,78 (4): 1033-1037.], Y
2O
3: Nd (2001) laser ceramicses such as [Ji.Lu, Ju.Lu, T.Murai, et al., Jpn.J Appl.Phys., 2001,40 (12A): L1277-1283.], and (Y, Gd)
2O
3: Eu[U.S.P.4421671], Gd
2O
2S:Pr, Ce, F[Ito H, Yamada H, Yoshida M, et al, Jpn.J.Appl.Phys.1988,27 (8): L1371-1373], Gd
3Ga
5O
12: Cr, Ce[U.S.P.5318722] etc. scintillating ceramic.At present, laser ceramics also is in advanced development, and some scintillating ceramics have satisfied the performance requriements of medical science X-CT basically, have progressively substituted original inorganic scintillation crystal and have been widely used in medical science X-CT detector.
Hafnium acid lanthanum (La
2Hf
2O
7) have high-density, high effective atomic number and high ray absorption capacity, and multiple active ions all have stronger luminous in hafnium acid lanthanum.Therefore, hafnium acid lanthanum (La
2Hf
2O
7) can be used as the high substrate material that absorbs heavy scintillator and be used in radiation detection field tool.But because hafnium acid lanthanum (La
2Hf
2O
7) fusing point higher (～2300 ℃), be difficult to prepare large size single crystal by traditional growing method, limited its application as scintillation crystal.
Ceramic sintering process by solid-state diffusion can will have the crystalline ceramics that cube material preparation of equal optics isotropic becomes excellent in optical properties by special sintering process being significantly less than under the temperature condition of fusing point.With respect to monocrystalline, crystalline ceramics has also that preparation time is short, cost is low, and can prepare large size and complex-shaped and advantages such as the crystalline ceramics mechanical property excellence.Hafnium acid lanthanum (La
2Hf
2O
7) below 2500K, have stable cube pyrochlore constitution, there is not birefringent phenomenon, therefore it might be prepared into crystalline ceramics.Generally adopt solid state reaction to prepare hafnium acid lanthanum (La traditionally
2Hf
2O
7) powder, be difficult to obtain the active powder of high sintering; Go back no-trump hafnium acid lanthanum (La at present
2Hf
2O
7) be prepared into the report of optical materials such as crystalline ceramics.By sintering process in hot pressing, hot isostatic pressing and vacuum, the hydrogen and the high sintering activity hafnium acid of burning synthetic lanthanum (La
2Hf
2O
7) and rare earth ion doped powder, it is prepared into crystalline ceramics, develop a kind of new optical clear stupalith with high-density, high ray absorption capacity, just draw purpose of the present invention.
Summary of the invention
The objective of the invention is to adopt by sintering process in hot pressing, hot isostatic pressing and vacuum, the hydrogen and prepare a kind of transparent hafnium acid lanthanum ceramic base crystalline ceramics.
Consisting of of crystalline ceramics: La
2-2xRE
2xHf
2O
70≤x＜0.1, RE is Ce, Pr, Eu, Tm, Nd, Yb, rare earth ions such as Tb are pure hafnium acid lanthanum during x=0.
The hafnium acid lanthanum crystalline ceramics of the present invention's preparation, its general formula is expressed as: La
2-2xRE
2xHf
2O
70≤x＜0.1, RE is Ce, Pr, Eu, Tm, Nd, Yb, rare earth ions such as Tb are pure hafnium acid lanthanum during x=0.This crystalline ceramics has high density and ray absorption capacity, has important application prospects at radiation detection and laser medium field.
The powder that the present invention uses is for utilizing glycine, ethylenediamine tetraacetic acid (EDTA) organic-fuel and La (NO such as (EDTA)
3)
3, HfO (NO
3)
2, RE (NO
3)
3Burning synthetic particle diameter is the 10-100 nanopowder.
Hafnium acid lanthanum crystalline ceramics provided by the invention comprises the thermal treatment of burning synthetic powder, moulding and sintering process.Sintering process is characterised in that:
(1) moulding process can adopt dry-pressing or etc. the static pressure program, sintering process can adopt sintering or HIP sintering or hot pressed sintering under vacuum or the hydrogen;
(2) at 1500-2000 ℃ of insulation 4-10 hour, furnace cooling.
Adopting glycine and ethylenediamine tetraacetic acid (EDTA) (EDTA) is the powder of fuel by the combustion reactions preparation, successfully makes the La with good transparency first by sintering process such as sintering in hot pressing, hot isostatic pressing and vacuum, the hydrogen
2Hf
2O
7Pottery is higher than 70% through the thick sample of polishing 1mm at the high permeability of visible light wave range.The ceramic sintered bodies that obtains has the cubical pyrochlore constitution.Do not detect pore in the microstructure of pottery, intercrystalline is in conjunction with tight, and crystal boundary is very thin, has the microstructure features of typical crystalline ceramics.Mix Tb
3+, Ce
3+, Pr
3+, Tm
3+, Eu
3+Under ultraviolet or excitation of X-rays, has stronger light emission Deng rare earth ion.
La provided by the invention
2Hf
2O
7The crystalline ceramics characteristics are:
(1) La
2Hf
2O
7Do not have in the crystalline ceramics to use the detected pore of scanning electron microscope, in conjunction with tight, crystal boundary is very thin between the crystal boundary.
(2) La
2Hf
2O
7Crystalline ceramics has higher transmittance at visible light wave range (380-780nm).
(3) La
2Hf
2O
7Crystalline ceramics has high density (＞7.8g/cm
3) and high ray absorption capacity.
(4) doping Tb
3+, Ce
3+, Pr
3+, Tm
3+, Eu
3+The crystalline ceramics of rare earth has strong light emission under ultraviolet or excitation of X-rays.
Description of drawings
Fig. 1 is that diameter is 1.5cm, and thickness is the transparent La of 1mm through polishing
2Hf
2O
7Ceramics sample shows that it is transparent in the visible light optical band.
Fig. 2 thickness is the transparent La of 1mm through polishing
2Hf
2O
7Pottery is at the transmittance curve of visible light wave range, and X-coordinate is a wavelength, the ordinate zou transmitance.
Fig. 3 is transparent La
2Hf
2O
7The X-ray diffraction spectrum of pottery shows that it is the La of purified cube of pyrochlore constitution
2Hf
2O
7
Fig. 4 is transparent La
2Hf
2O
7The SEM photo of pottery fracture does not detect pore, and intercrystalline is in conjunction with tight, and crystal boundary is very thin, has the microstructure features of typical crystalline ceramics.
Fig. 5 is La
2Hf
2O
7: 1%Eu
3+(a) transmittance curve of crystalline ceramics and (b) fluorescence spectrum.The X-coordinate of Fig. 5 (b) is a wavelength, the ordinate zou luminous intensity.
Fig. 6 is La
2Hf
2O
7: (a) transmittance curve of 1%Tb crystalline ceramics and (b) fluorescence spectrum.
Fig. 7 is La
2Hf
2O
7: (a) transmittance curve of 1%Tm crystalline ceramics and (b) fluorescence spectrum.
Fig. 8 is La
2Hf
2O
7: (a) transmittance curve of 1%Ce crystalline ceramics and (b) fluorescence spectrum.
Fig. 9 is La
2Hf
2O
7: (a) transmittance curve of %1.5Pr crystalline ceramics and (b) fluorescence spectrum.
Embodiment
Further illustrate substantial characteristics of the present invention and obvious improvement below by embodiment, yet the present invention absolutely not only is confined to described embodiment.
Embodiment 1
0.02 the HfO (NO of mole
3)
2And La (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Through calcination processing burning synthetic La
2Hf
2O
7Through waiting axial compression, the compact density behind the 180MPa isostatic pressing is 35% to powder more earlier.The goods of isostatic pressing are incubated 6 hours in 1850 ℃ of hydrogen atmospheres.
The transmittance curve of the crystalline ceramics that obtains is shown in Fig. 2 (b).Performance is as follows:
Density (g/cm
3)＞7.8
Crystalline phase (X diffraction analysis) La
2Hf
2O
7
Void content (%)＜0.1
380-780nm wave band maximum transmission (%)＞60
From the analysis of SEM fracture apperance as seen, La
2Hf
2O
7The grain size distribution of pottery is inhomogeneous, is made up of the big crystal grain of diameter～1 and the big crystal grain of diameter～5 μ m basically, but closely arranges between crystal grain, and crystal boundary is very thin, does not observe pore under the scanning electron microscope, thereby causes material transparent, shown in Fig. 4 (a).
Embodiment 2
0.02 the HfO (NO of mole
3)
2And La (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Through calcination processing burning synthetic La
2Hf
2O
7Powder is earlier through waiting axial compression, after the compact density behind the 180MPa isostatic pressing is 35%.The goods of isostatic pressing are incubated 6 hours in 1750 ℃ of hydrogen atmospheres.The transmittance curve of the crystalline ceramics that obtains shown in Fig. 2 (a), the transparent La that makes
2Hf
2O
7Ceramic performance is as follows:
Density (g/cm
3)＞7.5
Crystalline phase (X diffraction analysis) La
2Hf
2O
7
Void content (%)＜0.1
380-780nm wave band maximum transmission (%)＞40
Embodiment 3
0.02 the HfO (NO of mole
3)
2And La (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Through calcination processing burning synthetic La
2Hf
2O
7Powder is earlier through waiting axial compression, after the compact density behind the 180MPa isostatic pressing is 35%.The goods of isostatic pressing are incubated 6 hours in 1900 ℃ of hydrogen atmospheres.The transmittance curve of the crystalline ceramics that obtains shown in Fig. 2 (c), the transparent La that makes
2Hf
2O
7Ceramic performance is as follows:
Density (g/cm
3)＞7.5
Crystalline phase (X diffraction analysis) La
2Hf
2O
7
Void content (%)＜0.1
380-780nm wave band maximum transmission (%)＞60
Embodiment 4
0.02 the HfO (NO of mole
3)
2And La (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Through calcination processing burning synthetic La
2Hf
2O
7Through waiting axial compression, the compact density behind the 180MPa isostatic pressing is 35% to powder more earlier.The goods of isostatic pressing are incubated 12 hours in 1850 ℃ of hydrogen atmospheres.The transmittance curve of the crystalline ceramics that obtains shown in Fig. 2 (d), the transparent La that makes
2Hf
2O
7Ceramic performance is as follows:
Density (g/cm
3)＞7.8
Crystalline phase (X diffraction analysis) La
2Hf
2O
7
Void content (%)＜0.1
380-780nm wave band maximum transmission (%)＞70
Embodiment 5
0.02 the HfO (NO of mole
3)
2And La (NO
3)
3Calcine under 1000 ℃ of conditions with 0.013 moles of ethylene diamine tetraacethyl (EDTA) burning synthetic powder and to remove residual carbon and organism in 2 hours.Through calcination processing burning synthetic La
2Hf
2O
7Powder is earlier through waiting axial compression, after behind the 180MPa isostatic pressing.The goods of isostatic pressing are incubated 6 hours in 1850 ℃ of hydrogen atmospheres.
The transparent La that makes
2Hf
2O
7Pottery has good light transmittance, and performance is as follows:
Density (g/cm
3)＞7.8
Crystalline phase (X diffraction analysis) La
2Hf
2O
7
Void content (%)＜0.1
380-780nm wave band maximum transmission (%)＞40
Analyze as seen La from SEM fracture apperance (Fig. 4 (b))
2Hf
2O
7The grain size distribution of pottery is even, size of microcrystal～4 μ m, but closely arrange between crystal grain, crystal boundary is very thin, does not observe pore under the scanning electron microscope, thereby causes material transparent.
Embodiment 6
0.02 the HfO (NO of mole
3)
2, 0.0198 mole of La (NO
3)
3, 0.0002 mole of Eu (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Through calcination processing burning synthetic La
2Hf
2O
7Powder is earlier through waiting axial compression, back 180MPa isostatic pressing.The goods of isostatic pressing are incubated 6 hours in 1900 ℃ of hydrogen atmospheres.The transparent La that makes
2Hf
2O
7: 380-780nm wave band maximum transmission＞40% of 1%Eu pottery, transmittance curve and fluorescence spectrum are seen Fig. 5.
Embodiment 7
0.02 the HfO (NO of mole
3)
2, 0.0198 mole of La (NO
3)
3, 0.0002 mole of Tb (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Other is with embodiment 3.The transparent La that makes
2Hf
2O
7: 380-780nm wave band maximum transmission＞40% of 1%Tb pottery, transmittance curve and fluorescence spectrum are seen Fig. 6.
Embodiment 8
0.02 the HfO (NO of mole
3)
2, 0.0198 mole of La (NO
3)
3, 0.0002 mole of Tm (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Other is with embodiment 3.The transparent La that makes
2Hf
2O
7: 380-780nm wave band maximum transmission＞40% of 1%Tm pottery, transmittance curve and fluorescence spectrum are seen Fig. 7.
Embodiment 9
0.02 the HfO (NO of mole
3)
2, 0.0198 mole of La (NO
3)
3, 0.0002 mole of Ce (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Other is with embodiment 3.The transparent La that makes
2Hf
2O
7: 380-780nm wave band maximum transmission＞40% of 1%Ce pottery, transmittance curve and fluorescence spectrum are seen Fig. 8.
HfO (the NO that difference is 0.02 mole
3)
2, 0.0197 mole of La (NO
3)
3, 0.0003 mole of Pr (NO
3)
3Calcine under 800 ℃ of conditions with the powder of 0.054 mole of glycine combustion reactions preparation and to remove residual carbon and organism in 2 hours.Other is with embodiment 3.The transparent La that makes
2Hf
2O
7: 380-780nm wave band maximum transmission＞40% of 1.5%Pr pottery, transmittance curve and fluorescence spectrum are seen Fig. 9.
Claims (6)
1, a kind of hafnium acid lanthanum ceramic base crystalline ceramics is characterized in that group of ceramics becomes La
2-2xRE
2xHf
2O
70≤x＜0.1, RE is Ce, Pr, Eu, Tm, Nd, Yb, rare earth ions such as Tb.
2, by the preparation method of the described a kind of hafnium acid lanthanum ceramic base crystalline ceramics of claim 1, it is characterized in that adopting burning synthetic particle diameter is 10-100 nanometer La
2Hf
2O
7Powder is through powder thermal treatment, moulding and sintering process.
3, by preparation method by the described a kind of hafnium acid of claim 2 lanthanum ceramic base crystalline ceramics, it is characterized in that moulding process can adopt dry-pressing or etc. the static pressure program.
4, by the preparation method of the described a kind of hafnium acid lanthanum ceramic base crystalline ceramics of claim 2, it is characterized in that sintering process can adopt sintering or HIP sintering or hot pressed sintering under vacuum or the hydrogen.
5,, it is characterized in that sintering condition is 1500-2000 ℃ of insulation 4-10 hour, furnace cooling by the preparation method of the described a kind of hafnium acid lanthanum ceramic base crystalline ceramics of claim 2.
6, by the preparation method of the described a kind of hafnium acid lanthanum ceramic base crystalline ceramics of claim 2, the powder that it is characterized in that using is for utilizing glycine, ethylenediamine tetraacetic acid (EDTA) organic-fuel and La (NO such as (EDTA)
3)
3, HfO (NO
3)
2, RE (NO
3)
3Burning synthetic particle diameter is the 10-100 nanopowder.
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|---|---|---|---|
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|---|---|---|---|---|
| CN100391896C (en) * | 2005-05-13 | 2008-06-04 | 中国科学院上海硅酸盐研究所 | Hafnium oxide-gadolinium oxide solid solution transparent ceramic glaring material and its preparation method and uses |
| CN101445725B (en) * | 2008-12-30 | 2012-05-09 | 华东师范大学 | Hafnate luminescent material and preparation method thereof |
| CN101580393B (en) * | 2009-05-21 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent yttrium hafnate ceramics |
| CN102674837A (en) * | 2012-05-22 | 2012-09-19 | 长春理工大学 | Er<3+>:Lu2O3 transparent ceramic |
| CN102838352A (en) * | 2005-12-13 | 2012-12-26 | 通用电气公司 | Polycrystalline transparent ceramic articles and method of making same |
| CN101343173B (en) * | 2007-05-08 | 2013-09-11 | 肖特公开股份有限公司 | Optoceramics, optical elements manufactured thereof and their use as imaging optics |
| US8872119B2 (en) | 2008-12-30 | 2014-10-28 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| US8877093B2 (en) | 2008-12-30 | 2014-11-04 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| CN104535117A (en) * | 2015-01-29 | 2015-04-22 | 中国科学院上海硅酸盐研究所 | Compound sensor and preparation method thereof |
| US9175216B2 (en) | 2008-12-30 | 2015-11-03 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| US9183962B2 (en) | 2008-12-30 | 2015-11-10 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| CN113045316A (en) * | 2021-04-29 | 2021-06-29 | 中国科学院上海硅酸盐研究所 | Transparent ceramic material capable of absorbing ultraviolet light and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391896C (en) * | 2005-05-13 | 2008-06-04 | 中国科学院上海硅酸盐研究所 | Hafnium oxide-gadolinium oxide solid solution transparent ceramic glaring material and its preparation method and uses |
| CN102838352A (en) * | 2005-12-13 | 2012-12-26 | 通用电气公司 | Polycrystalline transparent ceramic articles and method of making same |
| CN101343173B (en) * | 2007-05-08 | 2013-09-11 | 肖特公开股份有限公司 | Optoceramics, optical elements manufactured thereof and their use as imaging optics |
| CN101445725B (en) * | 2008-12-30 | 2012-05-09 | 华东师范大学 | Hafnate luminescent material and preparation method thereof |
| US8872119B2 (en) | 2008-12-30 | 2014-10-28 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| US8877093B2 (en) | 2008-12-30 | 2014-11-04 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| US9175216B2 (en) | 2008-12-30 | 2015-11-03 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| US9183962B2 (en) | 2008-12-30 | 2015-11-10 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic scintillator body and scintillation device |
| CN101580393B (en) * | 2009-05-21 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent yttrium hafnate ceramics |
| CN102674837A (en) * | 2012-05-22 | 2012-09-19 | 长春理工大学 | Er<3+>:Lu2O3 transparent ceramic |
| CN104535117A (en) * | 2015-01-29 | 2015-04-22 | 中国科学院上海硅酸盐研究所 | Compound sensor and preparation method thereof |
| CN113045316A (en) * | 2021-04-29 | 2021-06-29 | 中国科学院上海硅酸盐研究所 | Transparent ceramic material capable of absorbing ultraviolet light and preparation method thereof |
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