CN1621577A - Method for preparing near-stoichiometric lithium tantalate wafer - Google Patents
Method for preparing near-stoichiometric lithium tantalate wafer Download PDFInfo
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- CN1621577A CN1621577A CN 200410067130 CN200410067130A CN1621577A CN 1621577 A CN1621577 A CN 1621577A CN 200410067130 CN200410067130 CN 200410067130 CN 200410067130 A CN200410067130 A CN 200410067130A CN 1621577 A CN1621577 A CN 1621577A
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- CN
- China
- Prior art keywords
- lithium tantalate
- litao
- tao
- tantalate wafer
- crucible
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- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000011148 porous material Substances 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910006295 Si—Mo Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 claims 8
- 239000013078 crystal Substances 0.000 abstract description 12
- 239000000843 powder Substances 0.000 abstract description 11
- 229910012463 LiTaO3 Inorganic materials 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- 229910012926 Li3TaO4 Inorganic materials 0.000 abstract 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 229910001416 lithium ion Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 230000000737 periodic effect Effects 0.000 abstract 1
- 230000010287 polarization Effects 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000011067 equilibration Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- PSVBHJWAIYBPRO-UHFFFAOYSA-N lithium;niobium(5+);oxygen(2-) Chemical compound [Li+].[O-2].[O-2].[O-2].[Nb+5] PSVBHJWAIYBPRO-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A process for preparing the near-stoichiometric lithium tantalate crystal plate features that LiTaO with air holes is put in a Pt crucible3And Li3TaO4Mixing the material blocks; placing or hanging the lithium tantalate wafer with the same composition on a platinum wire, and covering the platinum wire with LiTaO3And Li3TaO4Mixing the powder and a platinum sheet of a thermocouple, sealing the top of a crucible with a platinum cover, and placing the crucible in a resistance furnace; heating the mixture in a resistance furnace to 1000-1400 ℃, keeping the temperature for 1-200 hours, and enabling the composition of the crystal to reach a near stoichiometric ratio through diffusion of lithium ions. The near-stoichiometric lithium tantalate wafer of the invention has simple preparation process and easy operation, and has wide application prospect in the aspects of optical waveguide, electro-optical switch, periodic polarization, photoelectric device integration and the like.
Description
Technical field:
The present invention relates to lithium tantalate, its chemical formula is LiTaO
3, abbreviate LT as, particularly a kind of preparation method of near stoichiometric lithium tantalate wafer.
Background technology
The LT crystal has good piezoelectricity, electric light and thermoelectricity capability, in laser, electronics and integrated optics field wide application prospect is arranged.LT crystal and Lithium niobium trioxide (LiNbO
3Abbreviation LN) crystal is similar, present commercial LT crystal all is to utilize crystal pulling method from obtaining with growth the proportioning components melt, though the crystal that this method grows has good optical quality and consistence, but it is a kind of typical non-stoichiometric crystal, because the serious lithium that lacks in the crystal forms a large amount of native defects in crystal, performance to LT has produced many disadvantageous effects, has limited this crystalline and has used.The LT crystal of near stoichiometric proportion has been eliminated the disadvantageous effect of defective because of its lattice perfection, and the many performances of crystalline are improved, as coercive field significantly reduce, ultraviolet absorption edge blue shift, light injury threshold increase etc.
Excellent physicals, application prospects makes the preparation of near stoichiometric proportion LT crystalline research and develop mechanism extremely both at home and abroad and pays close attention in addition.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of near stoichiometric lithium tantalate wafer.This method should have simple, the easy-operating characteristics of preparation technology.
Technical solution of the present invention is as follows:
A kind of preparation method of near stoichiometric lithium tantalate wafer is characterized in that it comprises following concrete steps:
1. in platinum crucible, be placed with the LiTaO of band pore
3And Li
3TaO
4Mixture block, its LiTaO
3Content be 49～76mol%;
2. congruent lithium tantalate wafer is put or hung on the platinum wire, add to be coated with LiTaO
3And Li
3TaO
4It is airtight that the crucible platinum sheet of mixed powder and thermopair, crucible top add the platinum lid, places process furnace;
3. process furnace heat temperature raising, at 1000～1400 ℃, constant temperature 1～200 hour, Li
2O is diffused in the congruent lithium tantalate wafer, thereby has obtained near stoichiometric lithium tantalate wafer.
Described LiTaO
3And Li
3TaO
4Mixture block is by LiTaO
3And Li
3TaO raw material sintering forms, wherein Li
2CO
3Content be 49～76mol%.
Described process furnace is a resistance furnace, or silicon carbide rod furnace, or the Si-Mo rod stove.
The inventive method can also prepare adulterated near stoichiometric proportion LT wafer, and doping comprises one or more in magnesium, zinc, indium, scandium, iron, copper, manganese, cerium, ytterbium, chromium, erbium or the neodymium, and wherein: the doping content of MgO or ZnO is: 0～5mol%, In
2O
3Or Sc
2O
3Doping content be: 0～3mol%, Fe
2O
3, CuO, Mn
2O
3, Ce
2O
3, Yb
2O
3, Cr
2O
3, Er
2O
3Or Nd
2O
3Doping content be: 0～1mol%.
Vapor transport equilibration (VTE) technology is a kind of mass transport process, so the crucible planted agent guarantees to have enough Li
2The O supply, secondly, the balance of gas phase is to rely on Li
2O is continuously from LiTaO
3And Li
3TaO
4Volatilization is kept in the mixture block, for preventing mixture block Surface L i
2O exhausts the balance that causes to be destroyed, and should make mixture block have vesicular structure, to increase Li as far as possible
2The evaporation surface of O.
Li in the near stoichiometric proportion LT wafer of the inventive method preparation
2The content of O can reach more than the 49mol%, and good uniformity, and preparation technology is simple, easy to operate.In optical waveguides, electrooptical switching, period polarized, the aspect is widely used prospect such as photoelectric device is integrated.
Description of drawings
Fig. 1 is the vapor transport equilibration experimental installation synoptic diagram that the present invention uses.
Embodiment
The invention will be further described below by embodiment, but should not limit protection scope of the present invention with this.
The embodiment for preparing near stoichiometric proportion LT wafer with above-mentioned vapor transport equilibration experimental installation and concrete technical process is described below:
Embodiment 1:
Take by weighing [Li
2CO
3]/[Ta
2O
5The powder of]=69: 31, ground and mixed is at 800 ℃ of constant temperature 4h.Again with above-mentioned powder at 1000 ℃ of sintering 5h, make its fully be reacted into the band pore 2 LiTaO
3And Li
3TaO
4The polycrystal piece.With above-mentioned band pore polycrystal piece 3 with place or be suspended from congruent LT wafer on the platinum wire 4 (10 *, 10 * 0.5mm) 5 together in the Fang Yu gold crucible 1, adds to be coated with LiTaO3And Li
3TaO
4The sheet 6 of mixed powder 7 and thermopair 8, crucible top add platinum and cover 9 airtightly, place resistance furnace.The heating resistor stove is warming up to 1200 ℃, constant temperature 60 hours, Li
2O is diffused in the congruent LT wafer, thereby has obtained near stoichiometric proportion LT wafer.
Embodiment 2:
Take by weighing [Li
2CO
3]/[Ta
2O
5The powder of]=60: 40, ground and mixed, at 800 ℃ of left and right sides constant temperature 6h, again with above-mentioned powder at 1000 ℃ of sintering 5h, make its fully be reacted into the band pore 2 LiTaO
3And Li
3TaO
4Polycrystal piece 3.With above-mentioned band pore polycrystal piece 3 with place or be suspended from congruent on the platinum wire 4 and mix magnesium (1mol%) LT wafer (10 *, 10 * 0.5mm) 5 together in the Fang Yu gold crucible, adds to be coated with LiTaO3And Li
3TaO
4The crucible disc 6 of mixed powder 7 and thermopair 8, crucible top add platinum and cover 9 airtightly, place resistance furnace.The heating resistor stove is warming up to 1200 ℃, constant temperature 100 hours, Li
2O is diffused in the congruent LT wafer.Obtain magnesium-doped near stoichiometric ratio LT wafer.
Embodiment 3:
Take by weighing [Li
2CO
3]/[Ta
2O
5The powder of]=68: 32, ground and mixed is at 800 ℃ of left and right sides constant temperature 6h.Again with above-mentioned powder at 1050 ℃ of sintering 4h, make its fully be reacted into the band pore LiTaO
3And Li
3TaO
4The polycrystal piece.With above-mentioned band pore polycrystal piece with place or be suspended from congruent on the platinum wire and mix indium (1mol%) LT wafer (10 *, 10 * 0.5mm) together in the Fang Yu gold crucible, adds to be coated with LiTaO3And Li
3TaO
4It is airtight that the crucible disc of mixed powder and thermopair, crucible top add the platinum lid, places resistance furnace.The heating resistor stove is warming up to 1100 ℃, constant temperature 80 hours, Li
2O is diffused in the congruent LT wafer.Thereby obtained mixing indium near stoichiometric proportion LT wafer.
Embodiment 4:
Take by weighing [Li
2CO
3]/[Ta
2O
5The powder of]=65: 35, ground and mixed is at 900 ℃ of left and right sides constant temperature 3h.Again with above-mentioned powder at 1050 ℃ of sintering 4h, make its fully be reacted into the band pore LiTaO
3And Li
3TaO
4The polycrystal piece.With above-mentioned band pore polycrystal piece with place or be suspended from congruent er-doped (0.5mol%) LT wafer on the platinum wire (10 *, 10 * 0.5mm) together in the Fang Yu gold crucible, adds to be coated with LiTaO3And Li
3TaO
4It is airtight that the crucible disc of mixed powder and thermopair, crucible top add the platinum lid, places resistance furnace.The heating resistor stove is warming up to 1300 ℃, constant temperature 80 hours, Li
2O is diffused in the congruent LT wafer.Thereby obtained er-doped near stoichiometric proportion LT wafer.
Embodiment 5:
Take by weighing [Li
2CO
3]/[Ta
2O
5The powder of]=68: 32, ground and mixed is at 800 ℃ of left and right sides constant temperature 3h.Again with above-mentioned powder at 1050 ℃ of sintering 4h, make its fully be reacted into the band pore LiTaO
3And Li
3TaO
4The polycrystal piece.With above-mentioned band pore polycrystal piece with place or be suspended from congruent on the platinum wire and mix chromium (0.25mol%) LT wafer (10 *, 10 * 0.5mm) together in the Fang Yu gold crucible, adds to be coated with LiTaO3And Li
3TaO
4It is airtight that the crucible disc of mixed powder and thermopair, crucible top add the platinum lid, places resistance furnace.The heating resistor stove is warming up to 1150 ℃, constant temperature 60 hours, Li
2O is diffused in the congruent LT wafer.Thereby obtained mixing chromium near stoichiometric proportion LT wafer.
Claims (4)
1, a kind of preparation method of near stoichiometric lithium tantalate wafer is characterized in that it comprises following concrete steps:
1. in platinum crucible (1), be placed with the LiTaO of band pore (2)
3And Li
3TaO
4Mixture block (3), its LiTaO
3Content be 49～76mol%;
2. congruent lithium tantalate wafer (5) is put or hung on the platinum wire (4), add to be coated with LiTaO
3And Li
3TaO
4It is airtight that the crucible platinum sheet (6) of mixed powder (7) and thermopair (8), crucible top add platinum lid (9), places process furnace;
3. process furnace heat temperature raising, at 1000～1400 ℃, constant temperature 1～200 hour, Li
2O is diffused in the congruent lithium tantalate wafer, thereby has obtained near stoichiometric lithium tantalate wafer.
2, the preparation method of near stoichiometric lithium tantalate wafer according to claim 1 is characterized in that described LiTaO
3And Li
3TaO
4Mixture block (3) is by LiTaO
3And Li
3TaO raw material sintering forms, wherein [Li
2CO
3] content be 49～76) mol%.
3, the preparation method of near stoichiometric lithium tantalate wafer according to claim 1 is characterized in that described process furnace is a resistance furnace, or silicon carbide rod furnace, or the Si-Mo rod stove.
4, according to the preparation method of claim 1 or 2 or 3 described near stoichiometric lithium tantalate wafers, it is characterized in that this method prepares adulterated near stoichiometric lithium tantalate wafer, be doped in magnesium, zinc, indium, scandium, iron, copper, manganese, cerium, ytterbium, chromium, erbium or the neodymium one or more, wherein: the doping content of MgO or ZnO is: 0～5mol%, In
2O
3Or Sc
2O
3Doping content be: 0～3mol%, Fe
2O
3, CuO, Mn
2O
3, Ce
2O
3, Yb
2O
3, Cr
2O
3, Er
2O
3Or Nd
2O
3Doping content be: 0～1mol%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067130 CN1621577A (en) | 2004-10-13 | 2004-10-13 | Method for preparing near-stoichiometric lithium tantalate wafer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067130 CN1621577A (en) | 2004-10-13 | 2004-10-13 | Method for preparing near-stoichiometric lithium tantalate wafer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1621577A true CN1621577A (en) | 2005-06-01 |
Family
ID=34765005
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410067130 Pending CN1621577A (en) | 2004-10-13 | 2004-10-13 | Method for preparing near-stoichiometric lithium tantalate wafer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1621577A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319391B (en) * | 2008-06-06 | 2010-11-03 | 中电科技德清华莹电子有限公司 | Synthesis of constituent-homogeneous spherical lithium tantalite doping polycrystal raw material |
| CN101225545B (en) * | 2007-10-25 | 2011-07-20 | 宁夏东方钽业股份有限公司 | Method for preparing near-stoichiometric lithium tantalate crystals |
| CN102689928A (en) * | 2012-06-19 | 2012-09-26 | 南开大学 | Preparation method of near-stoichiometric lithium tantalate crystals |
| CN106192007A (en) * | 2016-08-12 | 2016-12-07 | 天通控股股份有限公司 | A kind of manufacture method mixing ferrum lithium tantalate |
| CN107429425A (en) * | 2015-04-16 | 2017-12-01 | 信越化学工业株式会社 | Monocrystalline lithium tantalate substrate and its engagement substrate, the manufacture method of the engagement substrate and surface acoustic wave device using the substrate |
| CN109576791A (en) * | 2018-12-07 | 2019-04-05 | 河南工程学院 | A kind of polarization method of near stoichiometric lithium tantalate wafer |
-
2004
- 2004-10-13 CN CN 200410067130 patent/CN1621577A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225545B (en) * | 2007-10-25 | 2011-07-20 | 宁夏东方钽业股份有限公司 | Method for preparing near-stoichiometric lithium tantalate crystals |
| CN101319391B (en) * | 2008-06-06 | 2010-11-03 | 中电科技德清华莹电子有限公司 | Synthesis of constituent-homogeneous spherical lithium tantalite doping polycrystal raw material |
| CN102689928A (en) * | 2012-06-19 | 2012-09-26 | 南开大学 | Preparation method of near-stoichiometric lithium tantalate crystals |
| CN102689928B (en) * | 2012-06-19 | 2013-12-11 | 南开大学 | Preparation method of near-stoichiometric lithium tantalate crystals |
| CN107429425A (en) * | 2015-04-16 | 2017-12-01 | 信越化学工业株式会社 | Monocrystalline lithium tantalate substrate and its engagement substrate, the manufacture method of the engagement substrate and surface acoustic wave device using the substrate |
| CN106192007A (en) * | 2016-08-12 | 2016-12-07 | 天通控股股份有限公司 | A kind of manufacture method mixing ferrum lithium tantalate |
| CN109576791A (en) * | 2018-12-07 | 2019-04-05 | 河南工程学院 | A kind of polarization method of near stoichiometric lithium tantalate wafer |
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