CN208776874U - A kind of crucible of lithium niobate crysal near stoichiometric ratio growth - Google Patents
A kind of crucible of lithium niobate crysal near stoichiometric ratio growth Download PDFInfo
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- CN208776874U CN208776874U CN201820333370.0U CN201820333370U CN208776874U CN 208776874 U CN208776874 U CN 208776874U CN 201820333370 U CN201820333370 U CN 201820333370U CN 208776874 U CN208776874 U CN 208776874U
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- crucible
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- lithium niobate
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Abstract
The utility model relates to field of crystal growth, and in particular to a kind of crucible of lithium niobate crysal near stoichiometric ratio growth.The utility model uses electric resistor heating type crystal growing furnace, and crucible is double-layer structure, and outer layer is platinum crucible, and internal layer is basket platinum net.Platinum net is connected with cathode, is provided with anode in platinum net, the amount of precipitation of Nb ion on cathode is controlled by controlling the electric current of positive and negative interpolar during crystal growth, to control the Li/Nb ratio in platinum net in melt.The utility model can control the Li/Nb ratio in growth district melt, to grow the lithium niobate crysal near stoichiometric ratio of high quality low defect.
Description
Technical field
The present invention relates to field of crystal growth, and in particular to a kind of earthenware of lithium niobate crysal near stoichiometric ratio growth
Crucible.
Background technique
Lithium niobate (LiNbO3) is widely used in optical transport, double-frequency laser as a kind of important photoelectric functional material
The fields such as device and optical storage.Lithium niobate generally uses Czochralski grown, the congruent point in lithia-niobium oxide binary phase diagraml
Congruent lithium columbate crystal is grown, is non-stoichiometric compound, Li/Nb ratio is 48.6/51.4, in seriously scarce lithium
State forms a large amount of intrinsic defects in crystal to reduce the performance of lithium columbate crystal.(Li/Nb ratio is 50/ to stoichiometric ratio
50) lithium columbate crystal compares more congruent lithium columbate crystal, and photoelectric coefficient and nonlinear optical coefficients increase 30% He respectively
27%, an order of magnitude can be improved in Preset grating sensitivity and photorefraotive crystal, and photoluminescence intensity can promote two quantity
Grade.
Currently, there are three types of the growing methods of near-stoichiometric ratio lithium niobate monocrystalline:
1, gas phase exchange equilibrium method
The lithium columbate crystal of traditional Czochralski grown is thinly sliced, platinum crucible is put into, in covering Li3NbO4 and
LiNbO3 mixture is heated to 1050-1100 DEG C, and constant temperature 100h is diffused into lithium in crystal, to improve LN crystal
Li/Nb ratio, Li2O content can reach 49.9mol% in crystal.The crystal chemistry homogeneity of ingredients that this method obtains
It is preferable with optical homogeneity, but be only applicable to prepare sheet sample, bulky single crystal is hardly resulted in, and the period is longer.
2, double crucible czochralski methods
1968, Bergman etc. was attempted to from rich lithium (60mol% Li2O) melt, with traditional Czochralski grown
Near-stoichiometric ratio lithium niobate monocrystalline.Double crucible device continuous charging Czochralski grown lithium niobate monocrystals are invented.Its structure is
Crucible set crucible, as crystal is constantly grown from interior crucible, charging system is according to growing the weight of crystal continuously
The raw material powder of near stoichiometric proportion is automatically added into outer crucible.The advantages of the method, is: (1) due to be equipped with it is smooth,
Continuous automatic feeding system, liquid level can remain unchanged in growth course, reduce what traditional czochralski method liquid level decline generated
It influences, crystal is enable to grow under stable heat condition；(2) control of the uniformity and stoichiometric ratio of crystal is easy to accomplish；
(3) large-size crystals can be grown in shallow crucible.But it after the powder raw material of room temperature is added, will necessarily be inhaled from interior crucible
Heat causes crystal growth temperature big fluctuation occur, to influence the normal growth of crystal.
3, flux pulling technique
K2O or excess Li2O is added in LN raw material as fluxing agent, keeps the congruent eutectic point of LN close
Stoicheiometry.The incorporation of K2O plays the role of adjusting Li/Nb ratio, effectively reduces the intrinsic defect concentration of crystal, energy
Grow the preferable crystal of optical homogeneity.But when crystal and melt separation, mechanical contraction crystalline substance, crystal are also easy to produce in crystal bottom
It is easy to crack.
China Patent Publication No. is that the patent application of 1654715. A of CN discloses a kind of suspension type crucible, has edge
Noble metal cylinder be hung vertically in the interior along upper of annulus, noble metal crucible is done with support shaft to be rotated and moves up and down, cooperation plus
Heat coil is synchronous to move up and down, and when melting sources, noble metal crucible is separated with metallic suspension cylinder, solves and melts during melt
Non-uniform problem is melted in melt area when continuous charging in change low efficiency, crystal growing process.But this method cannot be growth
Area continuously provides raw material, prevent growth course has from being continuously finished, and in crystal growing process with mechanical disturbance
The disadvantages of influencing crystal quality.
China Patent Publication No. discloses a kind of using the decline of resistance heating crucible for the patent application of CN 1216185.C
Method growth near-stoichiometric ratio lithium niobate monocrystalline makes to be to contain in sealed crucible directly using Li2CO3 and Nb2O5 as raw material
The oxidizing atmosphere of CO2 and O2 had not only avoided oxygen deficit problem during Crystal Growth of Lithium Niobate, but also has effectively overcome component Li2O
Volatilization.But since lithium niobate crystal bulk melting point is higher (generally at 1200~1300 DEG C), if closed in advance without reacting pre-
At at this temperature, it is easy to which the volatilization for causing oxide and carbonate deviates bath composition；Furthermore Li2CO3 in raw material
It is excessive, it cannot all be decomposed completely in melting process of raw material, therefore bulk gas generation is had in crystal growing process, meeting exists
Crystals form bubble, influence the quality of crystal.
Summary of the invention
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
In conjunction with Fig. 1, for crucible 5 on high temperature resistant pallet 9, pallet connects elevating lever 10, which is adjusted crucible in crystal
Height in growth furnace.Platinum net 7 is fixed in crystal growing furnace by cathode 4, and anode 3 is arranged on the inside of platinum net, and not
It is contacted with platinum net.
Specific step is as follows for this implementation column:
(1) seed crystal 2 is fixed on seed rod 1.
(2) it by a certain proportion of LiCO3 and Nb2O5 mix, is sufficiently mixed for 24 hours on earthquake machine, it is ensured that mixing is equal
It is even, it is then placed in crucible, is placed in crystal growing furnace；
(3) heat temperature raising makes melt temperature reach the fusing point (about 1250 DEG C) of lithium columbate crystal or more, completely molten to raw material
Change, constant temperature 2-3h.
(4) enter platinum net in melt 8 crucible raising by elevating lever, as shown in Figure 1.
(5) seeding temperature adjustment is carried out, temperature is adjusted to be suitble to lower brilliant temperature, completes seeding necking down technique.
(6) crystal 6 during the growth process, adjusts revolving speed, the rate of pulling and crucible fall off rate, grows crystal slowly,
The ratio of the Li/Nb in melt is controlled by adjusting constant current, constant current range is in 2.6-3.6A.
(7) after the completion of growing, crucible height is reduced, into annealing stage, completes crystal growth.
The above content is the further descriptions done in conjunction with specific preferred embodiment to the utility model, cannot
Assert that specific implementation of the invention is only limited to these explanations.For the personnel with fields rudimentary knowledge of the present invention,
It can be easy to that the present invention is changed and modified, these change and modification all shall be regarded as belonging to the power that the present invention is submitted
The scope of patent protection that sharp claim determines.
Detailed description of the invention
Fig. 1 is the front view of the utility model
Fig. 2 is the top view of the utility model
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
In conjunction with Fig. 1, for crucible 5 on high temperature resistant pallet 9, pallet connects elevating lever 10, which is adjusted crucible in crystal
Height in growth furnace.Platinum net 7 is fixed in crystal growing furnace by cathode 4, and anode 3 is arranged on the inside of platinum net, and not
It is contacted with platinum net.
Specific step is as follows for this implementation column:
(1) seed crystal 2 is fixed on seed rod 1.
(2) it by a certain proportion of LiCO3 and Nb2O5 mix, is sufficiently mixed for 24 hours on earthquake machine, it is ensured that mixing is equal
It is even, it is then placed in crucible, is placed in crystal growing furnace；
(3) heat temperature raising makes melt temperature reach the fusing point (about 1250 DEG C) of lithium columbate crystal or more, completely molten to raw material
Change, constant temperature 2-3h.
(4) enter platinum net in melt 8 crucible raising by elevating lever, as shown in Figure 1.
(5) seeding temperature adjustment is carried out, temperature is adjusted to be suitble to lower brilliant temperature, completes seeding necking down technique.
(6) crystal 6 during the growth process, adjusts revolving speed, the rate of pulling and crucible fall off rate, grows crystal slowly,
The ratio of the Li/Nb in melt is controlled by adjusting constant current, constant current range is in 2.6-3.6A.
(7) after the completion of growing, crucible height is reduced, into annealing stage, completes crystal growth.
The above content is the further descriptions done in conjunction with specific preferred embodiment to the utility model, cannot
Assert that specific implementation of the invention is only limited to these explanations.For the personnel with fields rudimentary knowledge of the present invention,
It can be easy to that the present invention is changed and modified, these change and modification all shall be regarded as belonging to the power that the present invention is submitted
The scope of patent protection that sharp claim determines.
Claims (3)
1. a kind of crucible of lithium niobate crysal near stoichiometric ratio growth, it is characterised in that use electric resistor heating type crystal growth
Furnace, the crucible are double-layer structure, and outer layer is platinum crucible, and internal layer is basket platinum net.
2. a kind of crucible of lithium niobate crysal near stoichiometric ratio growth according to claim 1, it is characterised in that institute
State basket platinum net be it is basket, basket platinum net is connected with cathode to be suspended in furnace body, and basket platinum net inside is provided with anode.
3. the crucible of a kind of lithium niobate crysal near stoichiometric ratio growth according to claim 1, it is characterized in that crucible
Bottom bracket is high-temperature refractory.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201820333370.0U CN208776874U (en) | 2018-03-12 | 2018-03-12 | A kind of crucible of lithium niobate crysal near stoichiometric ratio growth |
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| CN201820333370.0U CN208776874U (en) | 2018-03-12 | 2018-03-12 | A kind of crucible of lithium niobate crysal near stoichiometric ratio growth |
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| CN208776874U true CN208776874U (en) | 2019-04-23 |
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| CN201820333370.0U Expired - Fee Related CN208776874U (en) | 2018-03-12 | 2018-03-12 | A kind of crucible of lithium niobate crysal near stoichiometric ratio growth |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114635182A (en) * | 2022-03-30 | 2022-06-17 | 福建福晶科技股份有限公司 | Crystal production and lifting device and method convenient for discharging crystals |
-
2018
- 2018-03-12 CN CN201820333370.0U patent/CN208776874U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114635182A (en) * | 2022-03-30 | 2022-06-17 | 福建福晶科技股份有限公司 | Crystal production and lifting device and method convenient for discharging crystals |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190423 Termination date: 20200312 |
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| CF01 | Termination of patent right due to non-payment of annual fee |