CN1654715A - Suspension crucible for growth of lithium niobate crystal with near stoichiometric ratio and its growth process - Google Patents
Suspension crucible for growth of lithium niobate crystal with near stoichiometric ratio and its growth process Download PDFInfo
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- CN1654715A CN1654715A CN 200410024543 CN200410024543A CN1654715A CN 1654715 A CN1654715 A CN 1654715A CN 200410024543 CN200410024543 CN 200410024543 CN 200410024543 A CN200410024543 A CN 200410024543A CN 1654715 A CN1654715 A CN 1654715A
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Abstract
The present invention belongs to the field of crystal material technology, and includes mainly setting one support disc inside ceramic crucible, setting one refractory cylinder vertically on the disc, fixing one noble metal ring horizontally on the cylinder, hanging one noble metal cylinder on inner edge of the ring, and making the noble metal crucible rotate around the support shaft and move up and down and the heating winding move up and down with the crucible. During melting material, the noble metal crucible is separated from the noble metal cylinder; and during growing crystal, the noble metal cylinder separates the noble metal crucible into two regions, growth region and melt region. The present invention has the advantages of high material melting efficiency, homogeneous stirring, less volatilization of lithium oxide, easy regulation of temperature field, being favorable to stable crystal growth, etc.
Description
(1) technical field
The present invention relates to a kind of suspension crucible that is used for the lithium niobate crysal with near stoichiometric ratio growth, belong to the crystalline material technical field.
(2) background technology
As everyone knows, as a kind of important photoelectric functional material, lithium niobate crystals is widely used in fields such as light transmission, video and audio parts, frequency double laser and optical storage.
Lithium niobium trioxide generally adopts crystal pulling method (Czochralski method) growth, and the congruent point in Lithium Oxide 98min columbium monoxide binary phase diagram grows congruent lithium niobate crystals.Because congruent lithium niobate crystals is the non-stoichiometric compound, [lithium]/[niobium] is about 48.6/51.4, seriously lacks lithium, forms a large amount of native defects in crystal, and the Lithium niobium trioxide performance has been produced many disadvantageous effects, limited this crystalline and used.Compare with congruent Lithium niobium trioxide, the electro-optic coefficient and the nonlinear optical coefficients of near stoichiometric proportion crystal ([lithium]/[niobium] is about 50/50) have increased 30% and 27% respectively; Period polarized reversal voltage can reduce by two magnitudes; Light sells off sensitivity and the photon-induced refractive index variation can improve a magnitude; The time of response of non-volatile Hologram Storage can shorten two magnitudes; The intensity of photoluminescence can improve two magnitudes; The anti-light ability of hindering can improve four more than the magnitude after mixing a small amount of MgO; Mixing under small amounts of iron and the strong reductive state, the time of response that holography writes reaches the submicrosecond level, has shortened four magnitudes than congruent doped iron lithium niobate crystal.So, multi-functional crystal as a kind of excellent performance, lithium niobate crysal with near stoichiometric ratio will have great application prospect in many fields such as microelectronics, photoelectron, communication and laser, and, as the preferred material of massage storage of new generation, near-stoichiometric ratio lithium niobate has immeasurable application prospect especially.Therefore the near-stoichiometric ratio lithium niobate problem that become the many countries in the whole world competitively to study.
By LiO
2-Nb
2O
5Phasor is found out, stoichiometric proportion lithium niobate (Li
2O/[Li
2O+Nb
2O
5]=50%) growth of monocrystalline must be at the rich lithium liquation (Li of non-congruent melting point
2O/[Li
2O+Nb
2O
5]=58.5%) carries out in.Yet, when carrying out in the rich lithium liquation of crystal growth 58.5%, along with temperature reduction and crystalline are separated out, the composition of liquation is descending along liquidus line, because solidus curve is a curve, so the crystal of separating out is formed and will be changed along with proceeding of process of growth.So, if in crystal growth, can become 50% stoichiometric proportion lithium niobate raw material by the amount of separating out supplementation group, can make the chemical constitution of liquation maintain 58.5%, just can the stable growth stoichiometric ratio lithium niobate crystal.
In recent years, (the National Institute for Research inInorganic Materials of a kind of Japan state-run inorganic materials institute, NIRIM) proposed the growth that two crucible growing methods are used for near-stoichiometric ratio lithium niobate (JP-A-57-183392, JP-A-47-10355).This method is the two crucible growth methods that developed silicon monocrystal growth, uses it for the growth of near-stoichiometric ratio lithium niobate monocrystalline.The crucible of growing crystal is made bilayer structure, promptly in the step end of big crucible central position, vertical weld connect a diameter less than the cylinder of big crucible as inner crucible, form the double crucible structure.Inner crucible is as the crystal growth district, be used for crystal growth, it between outer crucible and the internal layer melt district, be mainly used in continuous supplementation stoichiometric proportion lithium niobate raw material, bottom in inner crucible, open an aperture, be used for the inside crucible diffusion of melt in the melt district, with consumption of raw materials in the crucible in replenishing.In the crystal growing process, the crystalline increment is weighed in real time by weighing-appliance, and corresponding signal is passed to the continuous charging system, and the addition of raw material equates with the crystal growth amount, so just can guarantee that crystal grows under the condition of constant level, permanent component.
Double crucible method all has certain shortcoming in melt and process of growth.Because have one deck precious metal to isolate between interior crucible and the outer crucible, raw material is not easy to be heated in the interior crucible.Can only be in the melt process by raw material is placed in the outer crucible, the heating back forms melt and flows into interior crucible.The melt process that need carry out for a long time just can obtain desired liquid level like this, has increased melt running cost and operating time.In addition, because outer crucible is interior without any the stirring measure, and volume between the outer crucible is narrow and small relatively in outer, the melt in the melting area is difficult to make component even by thermal convection, the needed component of component deviation in the melt in the crucible influence crystalline and grows in causing easily.In addition when powder stock joins the melt district by filling tube, because the raw material that adds concentrates on the same position in the crucible, the floating crystalline substance that causes because of local cooling appears easily, improve the operation easier of whole growth process and influence the stability of crystal growth.Even crucible is applied a rotating operation,, can not play that liquation is acted on uniformly because the liquation in the outer crucible does not have relative movement with crucible run-in synchronism yet.In addition, because outer crucible continuous high temperature always, long-time crystal growth meeting makes that lithium content reduces in the melt under the environment that opens wide, and the crystal that grows is difficult to obtain the composition of stable and consistent.
Although double crucible system provides a kind of feasible method of the near-stoichiometric ratio lithium niobate of growing, because the existence of these shortcomings, the stable batch growth of lithium niobate crysal with near stoichiometric ratio is still very difficult.
(3) summary of the invention
In order to solve the deficiency that prior art exists, the present invention has designed a kind of crucible system that is used for the growth of near stoichiometric proportion Niobium acid crystalline lithium, can make raw material fusing equably rapidly, keeps making the bath component uniformity in the continuous charging process.
The present invention is realized by following technical scheme:
One fire-resistant disk 2 is arranged at the bottom of ceramic crucible 1, disk 2 centers have circular hole, fire-resistant support cylinder 3 of vertical placement on disk 2, upper end in fire-resistant support cylinder 3, fix the passive precious metal annulus 4 of a horizontal positioned, the precious metal cylinder 5 that has the edge is hung vertically on the internal diameter of annulus 4, precious metal crucible 6 lies in a horizontal plane on the fire-proof supporting support plate 7, supporting disk 7 connects together by back shaft 8 and the rotating lifting gear that passes ceramic crucible 1 bottom surface circular hole, the crown after-heater 9 of center drilling is fixed on the upper end of fire-resistant support cylinder 3, the outside of after-heater is a lagging material 10, the seed rod 12 that has a seed crystal 11 enters in the precious metal crucible by the centre hole of after-heater 9, filling tube 13 passes lagging material 10, after-heater 9, precious metal annulus 4 enters in the precious metal crucible 6, there is heater coil device 14 outside of ceramic crucible 1, and it and precious metal crucible 6 keep moving up and down synchronously.
Between disk 2 and ceramic crucible 1 bottom is lagging material 10.
Cylinder 3 is made by refractory materials, is lagging material between cylinder 3 and the ceramic crucible 1.
The same with general Czochralski grown process, before the crystal growth, seed crystal 11 is fixed on the seed rod 12.Begin precious metal 6 and heater coil device 14 are dropped to bottom disc 2 positions of ceramic crucible 1, in this position polycrystal raw material is melted, because melting process is identical with general crystal pulling method, when this had just been avoided the double crucible method melt, oversize and melt convection of the polycrystal thawing time that causes because of the too little and shielding effect internal crucible of outer crucible of melt district volume between the interior outer crucible freely was not difficult to the shortcoming of homogenizing.After melt finishes, precious metal crucible 6 is risen to the top of ceramic crucible 1 by jacking system, the precious metal annulus 5 that is suspended on the precious metal annulus 4 is vertically stretched in the melt of precious metal crucible 6, and and the bottom of precious metal crucible 6 leave the slit, thereby two distinct area have been formed, i.e. melt district and vitellarium.The melt district is exactly the space by the inboard relative closure of forming of the downside of the outside of precious metal cylinder 5, precious metal annulus 4 and precious metal crucible 6 ground.It is higher to be used in the melt district temperature, and the Lithium Oxide 98min volatilization is violent, and this enclosed construction helps the volatilization of inhibited oxidation lithium, prevents the variation of bath component in the process of growth, and process of growth is stable carries out thereby make.The vitellarium is the relatively independent space that the upside by the inboard of precious metal cylinder 5 and after-heater 9, precious metal annulus 4 forms, and this design and adjusting to vitellarium temperature is very favourable.Process is operations such as seed crystal 11, necking down, expansion shoulder down, crystal 15 sustainable isodiametric growths.In the process of growth, precious metal crucible 6 under the driving of back shaft 8 with seed rod 12 equidirectional rotations, when crystal 15 began to grow, polycrystal raw material joined in the melt district by filling tube 13.Because precious metal crucible 6 rotation drives the solution rotating in the melt district, make the raw material of adding be dispersed in molten surface uniformly, thereby avoided the local overcooling that may occur in common two crucible process of growth and the floating brilliant phenomenon that produces.Because the precious metal cylinder 5 that hangs is immobilized, when precious metal crucible 6 rotates, its outer wall makes the melt in 5 pairs of melt districts of precious metal cylinder play a kind of stirring action to the viscous resistance of liquation, and this stirring action makes that the solution in the precious metal crucible 6 is easier evenly.In whole growth process, last weighing-appliance is weighed in real time, accurately measures the weightening finish of crystal 15, with control crystal 15 isodiametric growths.Measuredly after handling, control device passes to charging system to weight signal, by its weighing system and the collaborative realization of charging system self-feeding, it is identical with the weight strictness of pulling crystal promptly to realize replenishing raw material weight, thereby guarantee that the liquid level of crucible inner melt and composition are constant, thereby realize the growth of near stoichiometric proportion crystalline continous-stable.
When desired length is arrived in crystal growth 15, crystal 15 is proposed, precious metal crucible 6 and heater coil 14 descend synchronously, and precious metal hangs the liquid level that cylinder 5 breaks away from crucibles 6, and cooling is cooled off then.Because remainder melt is at precious metal crucible 6 internal cooling, precious metal hangs cylinder 5 and can not cause whole crucible system to be out of shape because of the bigger stress that complicated crystallisation process produces the interior crucible in double crucible system.In addition, cooled product is handled easily in this single crucible, can guarantee that crucible is repeatedly used, and reduces the expense of making crucible.Advantage of the present invention is the melt district that relative closure has been formed in the inboard of outer wall, support annulus 4 ground downsides and the precious metal crucible 6 of suspension precious metal cylinder 5, isolate fully with the vitellarium of forming by suspension precious metal cylinder 5 inwalls, after-heater 9 and annulus 4, thereby reduced the volatilization of Lithium Oxide 98min, helped the stable growth of near stoichiometric proportion Niobium acid crystalline lithium.In addition because the rotation of precious metal crucible 6, the raw material that charging system is replenished in real time can be in ablation zone uniform distribution, prevent constitutional supercooling and floating brilliant appearance, being used to hang precious metal cylinder 5 simultaneously is fixed, when 6 rotations of precious metal crucible, produce relative movement between the melt of ablation zone and the cylinder 5, thereby generation stirring action, overcome the uneven phenomenon of bath component that does not freely cause because of the convection current of melt district in the static pair of crucible, also overcome the defective of the mixing effect difference that the two crucibles of rotation cause because of interior outer crucible is synchronized with the movement.
The present invention also has an advantage to be, crown after-heater 9 has better boosting effect, overcome because of the precious metal crucible to hanging the too low phenomenon of vitellarium temperature that causes of shielding effect of tube.Because after-heater 9 precious metal cylinders 5 and precious metal support vitellarium and melt district relative separation that annulus is formed, help the control and the adjusting of temperature field, vitellarium.
(4) description of drawings
Accompanying drawing is the structural representation that is used for the suspension crucible of near stoichiometric proportion Niobium acid crystalline lithium growth.
Among the figure, 1. ceramic crucible, 2. fire-resistant disk 3. supports fire-resistant cylinder, 4. precious metal annulus, 5. precious metal crucible, 7. support disk, 8 back shafts, 9. crown after-heater, 10. lagging material; 11. seed crystal; 12. seed rod; 13. filling tube; 14 heater coils; 15. crystal.
(5) embodiment
Accompanying drawing is exactly a most preferred embodiment of the present invention.One fire-resistant disk 2 is arranged at the bottom of ceramic crucible 1, disk 2 centers have circular hole, fire-resistant support cylinder 3 of vertical placement on disk 2, upper end in fire-resistant support cylinder 3, fix the passive precious metal annulus 4 of a horizontal positioned, the precious metal cylinder 5 that has the edge is hung vertically on the internal diameter of annulus 4, precious metal crucible 6 lies in a horizontal plane on the fire-proof supporting support plate 7, supporting disk 7 connects together by back shaft 8 and the rotating lifting gear that passes ceramic crucible 1 bottom surface circular hole, the crown after-heater 9 of center drilling is fixed on the upper end of fire-resistant support cylinder 3, the outside of after-heater is a lagging material 10, the seed rod 12 that has a seed crystal 11 enters in the precious metal crucible by the centre hole of after-heater 9, filling tube 13 passes lagging material 10, after-heater 9, precious metal annulus 4 enters in the precious metal crucible 6, there is heater coil device 14 outside of ceramic crucible 1, and it and precious metal crucible 6 keep moving up and down synchronously.
Between disk 2 and ceramic crucible 1 bottom is lagging material 10.
Cylinder 3 is made by refractory materials, is lagging material between cylinder 3 and the ceramic crucible 1.
Claims (3)
1. one kind is used for the suspension crucible that lithium niobate crysal with near stoichiometric ratio is grown, it is characterized in that, one fire-resistant support disk is arranged at the bottom in the ceramic crucible, disc centre has circular hole, fire-resistant cylinder of vertical placement on disk, at precious metal annulus of the upper end of cylinder horizontal positioned, the precious metal cylinder that has the edge is hung vertically on the internal diameter of annulus, the precious metal crucible lies in a horizontal plane on the support disk, support disk connects together by back shaft and the rotating lifting gear that passes ceramic crucible bottom surface circular hole, the after-heater of center drilling is fixed on the upper end of fire-resistant cylinder, the upper end of after-heater is a lagging material, filling tube passes lagging material, after-heater and precious metal annulus enter the precious metal crucible, in the outside of ceramic crucible heater coil device are arranged, and it and precious metal crucible move up and down synchronously.
2. the suspension crucible that is used for the lithium niobate crysal with near stoichiometric ratio growth according to claim 1 is characterized in that between disk and ceramic crucible lagging material being arranged.
3. the suspension crucible that is used for the lithium niobate crysal with near stoichiometric ratio growth according to claim 1 is characterized in that cylinder has fire-resistant making, and between cylinder and the ceramic crucible inwall lagging material is arranged.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100245433A CN1329559C (en) | 2004-08-10 | 2004-08-10 | Suspension crucible for growth of lithium niobate crystal with near stoichiometric ratio and its growth process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100245433A CN1329559C (en) | 2004-08-10 | 2004-08-10 | Suspension crucible for growth of lithium niobate crystal with near stoichiometric ratio and its growth process |
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| CN1654715A true CN1654715A (en) | 2005-08-17 |
| CN1329559C CN1329559C (en) | 2007-08-01 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147127A (en) * | 2013-03-11 | 2013-06-12 | 东南大学 | Apparatus for growing moisture-absorbing monocrystals |
| CN103643292A (en) * | 2013-12-27 | 2014-03-19 | 中国工程物理研究院化工材料研究所 | Method and device for growing near-stoichiometric-ratio lithium niobate crystals |
| CN104294353A (en) * | 2013-07-19 | 2015-01-21 | 山东省科学院新材料研究所 | Method for improving homogeneity of potassium tantalate niobate crystal through double-crucible real-time material-feeding technology |
| CN104911697A (en) * | 2015-07-06 | 2015-09-16 | 中国电子科技集团公司第二十六研究所 | Constant-component crystal growth control system and method for lifting single-crystal furnace |
| CN105019024A (en) * | 2015-07-09 | 2015-11-04 | 山东大学 | Method for growing near-stoichiometric lithium niobate crystals by utilizing temperature gradient adjustable temperature field device |
| CN109210946A (en) * | 2018-09-27 | 2019-01-15 | 深圳市和胜金属技术有限公司 | A kind of smelting furnace auxiliary device |
| CN111485283A (en) * | 2020-05-15 | 2020-08-04 | 广东先导稀材股份有限公司 | Crystal growth device and method |
| CN113574341A (en) * | 2019-03-19 | 2021-10-29 | 赛峰集团陶瓷 | Support tool for infiltrating porous preforms and oven using same |
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| JPS57183392A (en) * | 1981-05-01 | 1982-11-11 | Tohoku Metal Ind Ltd | Apparatus for preparation of single crystal |
| JPS62246895A (en) * | 1986-04-18 | 1987-10-28 | Sumitomo Electric Ind Ltd | Crucible for manufacturing crystal |
| JPH05148077A (en) * | 1991-11-27 | 1993-06-15 | Nikko Kyodo Co Ltd | Production of single crystal and apparatus therefor |
| JPH06206788A (en) * | 1993-01-12 | 1994-07-26 | Kobe Steel Ltd | Crucible for producing single crystal and production of single crystal |
| JPH10338593A (en) * | 1997-06-03 | 1998-12-22 | Fuji Elelctrochem Co Ltd | Noble metal crucible for signal crystal growth by pulling up method |
| US6673330B1 (en) * | 1999-03-26 | 2004-01-06 | National Institute For Research In Inorganic Materials | Single crystal of lithium niobate or tantalate and its optical element, and process and apparatus for producing an oxide single crystal |
| TWI236455B (en) * | 2002-02-27 | 2005-07-21 | Univ Nat Taiwan | Method for growing stoichiometric lithium niobate and lithium tantalate single crystals and apparatus thereof |
| CN1216185C (en) * | 2003-07-11 | 2005-08-24 | 中国科学院上海光学精密机械研究所 | Method of growing near chemical gauge ratio lithium niobate monocrystal using crucible lowering method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103147127B (en) * | 2013-03-11 | 2016-02-10 | 东南大学 | A kind of equipment growing easy moisture absorption single crystal |
| CN103147127A (en) * | 2013-03-11 | 2013-06-12 | 东南大学 | Apparatus for growing moisture-absorbing monocrystals |
| CN104294353A (en) * | 2013-07-19 | 2015-01-21 | 山东省科学院新材料研究所 | Method for improving homogeneity of potassium tantalate niobate crystal through double-crucible real-time material-feeding technology |
| CN103643292A (en) * | 2013-12-27 | 2014-03-19 | 中国工程物理研究院化工材料研究所 | Method and device for growing near-stoichiometric-ratio lithium niobate crystals |
| CN103643292B (en) * | 2013-12-27 | 2016-07-06 | 中国工程物理研究院化工材料研究所 | A kind of method growing lithium niobate crysal with near stoichiometric ratio |
| CN104911697A (en) * | 2015-07-06 | 2015-09-16 | 中国电子科技集团公司第二十六研究所 | Constant-component crystal growth control system and method for lifting single-crystal furnace |
| CN104911697B (en) * | 2015-07-06 | 2017-10-20 | 中国电子科技集团公司第二十六研究所 | Czochralski furnace crystal perseverance component growth control system and method |
| CN105019024A (en) * | 2015-07-09 | 2015-11-04 | 山东大学 | Method for growing near-stoichiometric lithium niobate crystals by utilizing temperature gradient adjustable temperature field device |
| CN105019024B (en) * | 2015-07-09 | 2018-02-06 | 山东大学 | A kind of method that lithium niobate crysal near stoichiometric ratio is grown using the adjustable thermal field device of thermograde |
| CN109210946A (en) * | 2018-09-27 | 2019-01-15 | 深圳市和胜金属技术有限公司 | A kind of smelting furnace auxiliary device |
| CN109210946B (en) * | 2018-09-27 | 2023-11-14 | 深圳市和胜金属技术有限公司 | Auxiliary device of smelting furnace |
| CN113574341A (en) * | 2019-03-19 | 2021-10-29 | 赛峰集团陶瓷 | Support tool for infiltrating porous preforms and oven using same |
| CN113574341B (en) * | 2019-03-19 | 2023-10-27 | 赛峰集团陶瓷 | Support tool for infiltration of porous preforms and oven using said tool |
| CN111485283A (en) * | 2020-05-15 | 2020-08-04 | 广东先导稀材股份有限公司 | Crystal growth device and method |
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