CN1563518A - Crucible for lithium atmosphere gas phase transmission balancing method - Google Patents

Crucible for lithium atmosphere gas phase transmission balancing method Download PDF

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Publication number
CN1563518A
CN1563518A CN 200410017312 CN200410017312A CN1563518A CN 1563518 A CN1563518 A CN 1563518A CN 200410017312 CN200410017312 CN 200410017312 CN 200410017312 A CN200410017312 A CN 200410017312A CN 1563518 A CN1563518 A CN 1563518A
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China
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crucible
dividing plate
lithium
central dividing
angle
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CN 200410017312
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Chinese (zh)
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CN1308503C (en
Inventor
李抒智
徐军
周圣明
宋词
凌磊
严成锋
邹军
杨卫桥
夏长泰
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Priority to CNB200410017312XA priority Critical patent/CN1308503C/en
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Publication of CN1308503C publication Critical patent/CN1308503C/en
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Abstract

A crucible for the gas-phase transmission balance method in Li atmosphere is Al2O3The ceramic crucible consists of a crucible, a frame corner, a middle partition plate and a crucible cover, wherein the frame corner is arranged in the crucible, the middle partition plate is arranged on the frame corner, a plurality of vent holes and fine grooves for placing samples are formed in the middle partition plate, and an annular groove matched with the periphery of the crucible is formed in the edge of the crucible cover. The crucible has the characteristics of simple and convenient processing, low manufacturing cost, good air tightness and no pollution to a processed sample.

Description

The crucible that is used for lithium atmosphere vapor transport equilibration method
Technical field
The present invention relates to the method (Vapor TransportEquilibration is called for short the VTE technology) of the vapor transport equilibration of crystal growth, particularly a kind of crucible that is used for lithium atmosphere vapor transport equilibration method.
Technical background
Lithium atmosphere VTE technology is to utilize vapor transport equilibration, at high temperature, form rich lithium atmosphere, by the diffusion of lithium ion, the wafer top layer and the subsurface defect that are caused because of the non-stoichiometric volatilization are repaired, or generate the technology of cenotype at substrate surface generation chemical reaction.At present, the VTE technology mainly is to be used to improve LiNbO 3, LiTaO 3, LiAlO 2, LiGaO 2(Mater.Sci.Eng.B33 (1995) 91 Deng crystal mass and correlative study thereof; Optical Materials 23 (2003) 295; Appl.Phys.Lett.82 (2003) 2248).This technology also has been used to carry out LiAlO in addition 2Preparation Deng film.
In lithium atmosphere VTE experiment and production process, typically use platinum crucible at present and carry out work, so following problem in experimentation, occurred:
(1), cause experiment and production cost too high because the value of platinum is higher and the demand in experimentation is also bigger;
(2) find in the experiment that lithium can react with platinum under high temperature oxygen atmosphere.As through after the experiment of VTE several times, the crucible bottom duck eye that will be corroded out, in addition, the net of the placement sample of weaving into platinum wire in the experiment, through also becoming black powder after the experiment several times, these all cause the severe attrition of platinum, have improved experiment and production cost greatly;
(3) when the platinum consumption after a little while, with the container that platinum is made, resistance to air loss is relatively poor, is difficult to keep balanced atmosphere preferably in the experiment.
Owing to these reasons have improved the cost of lithium atmosphere VTE technology and restricted the development of lithium atmosphere VTE technology.
Summary of the invention
The technical problem to be solved in the present invention is the problems that overcome platinum crucible in the above-mentioned VTE technology, a kind of crucible that is used for lithium atmosphere vapor transport equilibration method is proposed, it should have easy, the low cost of manufacture of processing, crucible resistance to air loss good, to handling the non-staining characteristics of sample.
Basic thought of the present invention is to utilize Al 2O 3Ceramic crucible replaces platinum crucible to carry out the VTE processing.
Technical solution of the present invention is as follows:
A kind of crucible that is used for lithium atmosphere vapor transport equilibration method, this crucible is Al 2O 3Ceramic crucible, constitute by crucible, frame angle, central dividing plate and crucible cover, in this crucible, settle this angle, on this angle, place this central dividing plate, the stria that offers some ventilating pits on this central dividing plate and place for sample, the edge of crucible cover is provided with the annular recess that matches with the periphery of crucible.
Described crucible can be round shape or square box shaped, and described crucible cover matches with crucible.
Described angle both can constitute with crucible inwall one, also can be independent parts.
Technique effect of the present invention:
After placing this central dividing plate on this angle, crucible bottom is reserved certain space and is convenient to put into a certain amount of Li 2CO 3Or Li 2O or contain Li 2The mixing raw material of O.On central dividing plate, open stria, be used to lay pending wafer or substrate slice.Pending samples vertical is placed in central dividing plate, and two faces of sample fully are exposed in the atmosphere.On dividing plate, open some apertures, make things convenient for the atmosphere convection current to enter top.
Li at high temperature 2O meeting and Al 2O 3React, at Al 2O 3The inwall of ceramic crucible generates LiAlO 2Polycrystal layer, this layer LiAlO 2Polycrystal layer fine and close and highly stable in the VTE of lithium atmosphere environment, can not produce and pollute the VTE process, play the effect identical with platinum crucible.In addition, use Al 2O 3Pottery do lithium atmosphere VTE crucible process in addition easy, advantage such as interior shape is controlled easily, and the crucible resistance to air loss is good, and is with low cost.
Description of drawings
Fig. 1 is the structural representation that the present invention is used for the crucible specific embodiment of lithium atmosphere vapor transport equilibration method.
Among the figure: the 1-crucible; 2-frame angle; The 3-central dividing plate; The 4-crucible cover; Ventilating pit on the 5-dividing plate; 6-VTE raw material (Li 2CO 3Deng); The pending sample of 7-.
The specific design mode
See also Fig. 1 earlier, Fig. 1 is the structural representation that the present invention is used for the crucible specific embodiment of lithium atmosphere vapor transport equilibration method.1,2,3,4 parts are Al among the figure 2O 3Pottery is made.As seen from the figure, the present invention is used for the crucible of lithium atmosphere vapor transport equilibration method, and this crucible is Al 2O 3Ceramic crucible, constitute by crucible 1, frame angle 2, central dividing plate 3 and crucible cover 4, in this crucible 1, settle this angle 2, on this angle 2, place this central dividing plate 3, the stria that offers some ventilating pits 5 on this central dividing plate 3 and place for sample 7, the edge of crucible cover 4 is provided with the annular recess that matches with the periphery of crucible 1.After placing this central dividing plate 3 on this angle 2, reserved certain space in crucible bottom, be convenient to put into a certain amount of Li 2CO 3Or Li 2O or contain Li 2The mixing raw material 6 of O.On central dividing plate 3, open stria, be used to lay pending wafer or substrate slice 7.In the VTE process, pending sample 7 is placed perpendicular to central dividing plate 3, and two faces of sample 7 fully are exposed in the atmosphere.Several angles 2 are done in crucible 1 bottom, are used for laying and fixing central dividing plate 3.On dividing plate, open the aperture 5 of certain number, make things convenient for the atmosphere convection current to enter top.This crucible wants to put in the bottom earlier a certain amount of Li before use 2CO 3Or Li 2O, build crucible cover 4 after, the sky that under 800 ℃~1100 ℃ of high temperature crucible is carried out for some time (3~4 days) burns, and makes crucible 1 inwall generate stable LiAlO 2Layer.
Utilize this crucible, carried out in rich lithium atmosphere, improving LiNbO 3, LiTaO 3, LiAlO 2And LiGaO 2The VTE experiment of crystal mass, its effect of evidence is identical with the effect of using platinum crucible, also is better than the platinum crucible result under partial condition.In addition, also attempted carrying out VTE growth LiAlO on Sapphire Substrate with this crucible 2The test of thin film layer, test-results also come to the same thing with using platinum crucible.

Claims (3)

1, a kind of crucible that is used for lithium atmosphere vapor transport equilibration method is characterized in that this crucible is Al 2O 3Ceramic crucible, constitute by crucible (1), frame angle (2), central dividing plate (3) and crucible cover (4), in this crucible (1), settle this angle (2), go up placement this central dividing plate (3) in this angle (2), the stria that offers some ventilating pits (5) on this central dividing plate (3) and place for sample (7), the edge of crucible cover (4) is provided with the annular recess that matches with the periphery of crucible (1).
2, the crucible that is used for lithium atmosphere vapor transport equilibration method according to claim 1 is characterized in that described crucible (1) can be round shape or square box shaped, and described crucible cover (4) matches with crucible (1).
3, the crucible that is used for lithium atmosphere vapor transport equilibration method according to claim 1 is characterized in that described angle (2) and crucible (1) inwall one constitute.
CNB200410017312XA 2004-03-30 2004-03-30 Crucible for lithium atmosphere gas phase transmission balancing method Expired - Fee Related CN1308503C (en)

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CNB200410017312XA CN1308503C (en) 2004-03-30 2004-03-30 Crucible for lithium atmosphere gas phase transmission balancing method

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Application Number Priority Date Filing Date Title
CNB200410017312XA CN1308503C (en) 2004-03-30 2004-03-30 Crucible for lithium atmosphere gas phase transmission balancing method

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CN1563518A true CN1563518A (en) 2005-01-12
CN1308503C CN1308503C (en) 2007-04-04

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103420345A (en) * 2012-05-22 2013-12-04 广东先导稀材股份有限公司 Graphite crucible, heating furnace and preparation method for cadmium telluride
CN111979515A (en) * 2019-05-24 2020-11-24 南开大学 Sapphire crucible and method for preparing thallium-based high-temperature superconducting thin film

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1253125A (en) * 1999-11-08 2000-05-17 苏君道 Non-expansion lithium ceramics and process for preparing its crucible
CN1386894A (en) * 2001-05-17 2002-12-25 杜家庆 Crucible for vapor plating
CN1362546A (en) * 2001-12-17 2002-08-07 南开大学 Lithium niobate crystal chip with near stoichiometric ratio and its prepn process

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103420345A (en) * 2012-05-22 2013-12-04 广东先导稀材股份有限公司 Graphite crucible, heating furnace and preparation method for cadmium telluride
CN103420345B (en) * 2012-05-22 2015-04-22 广东先导稀材股份有限公司 Graphite crucible, heating furnace and preparation method for cadmium telluride
CN111979515A (en) * 2019-05-24 2020-11-24 南开大学 Sapphire crucible and method for preparing thallium-based high-temperature superconducting thin film

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