CN103696010A - Hafnium-dysprosium codoped lithium niobate crystal and preparation method thereof - Google Patents

Hafnium-dysprosium codoped lithium niobate crystal and preparation method thereof Download PDF

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CN103696010A
CN103696010A CN201310750340.1A CN201310750340A CN103696010A CN 103696010 A CN103696010 A CN 103696010A CN 201310750340 A CN201310750340 A CN 201310750340A CN 103696010 A CN103696010 A CN 103696010A
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crystal
lithium niobate
dysprosium
hafnium
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代丽
焦珊珊
赵丽丽
李大勇
林家齐
代明
徐超
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Harbin University of Science and Technology
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Abstract

The invention relates to a hafnium-dysprosium codoped lithium niobate crystal and a preparation method thereof. The crystal and the preparation method solve the problems that the existing lithium niobate crystal cannot serve as a laser crystal material and the light injury resistance of the lithium niobate crystal is low. The crystal is made from Nb2O5, LiCO3, HfO2 and Dy2O3. The method comprises the steps of 1, mixing the four raw materials, 2, growing the crystal by a lifting method and obtaining a multi-domain crystal, 3, polarizing and obtaining a polarized crystal, and 4, cutting, polishing and obtaining an Hf:Dy:LiNbO3 crystal. The Hf:Dy:LiNbO3 crystal prepared by the method is high in glossiness, uniform in component, flawless, growth-striation-free, crack-free, and higher in light injury resistance, and can serve as the laser crystal material; the preparation method is simple, convenient to operate and high in crystal growth rate; and the crystal material has a broad application prospect in preparing compact laser diode pumps and all-solid tunable laser devices.

Description

Hafnium dysprosium double doping lithium niobate crystal and preparation method thereof
Technical field
The invention belongs to material technology field, be specifically related to hafnium dysprosium double doping lithium niobate crystal and preparation method thereof.
Background technology
In recent years, along with the fast development of optical fiber technology and integrated optics technique, lithium niobate crystals (LiNbO 3) with its unique premium properties, become in optical waveguide material one of crystal that tool further investigation is worth.Especially by rare earth luminous doping, period polarized and optical waveguides combines, and can develop the solid statelaser of more premium propertiess and frequency inverted device etc.Thus, at present, rare earth ion doped lithium niobate crystals also more and more causes investigators' close attention.But the photo-damage resistance of lithium niobate crystals, lower than other crystal, has therefore seriously limited its application in real life is produced.
At present, lithium niobate crystals can not be as laser crystal material, and has the weak problem of photodamage resistant performance.
Summary of the invention
The present invention seeks to can not be as laser crystal material and the low problem of lithium niobate crystals photo-damage resistance in order to solve existing lithium niobate crystals, and hafnium dysprosium double doping lithium niobate crystal and preparation method thereof is provided.
Hafnium dysprosium double doping lithium niobate crystal, it is by Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3make; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities.
The preparation method of above-mentioned hafnium dysprosium double doping lithium niobate crystal, carries out according to the following steps:
One, mix: take four kinds of raw materials, be respectively Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3, then mix, obtain compound; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities;
Two, adopt Czochralski grown crystal: gained compound in step 1 is put into Pt crucible, then sintering 2～6h at 710～740 ℃, be warming up to again 1160～1180 ℃ and continue sintering 1～2h, be cooled to subsequently room temperature, then adopt crystal pulling method to carry out crystal growth, pass through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and anneal, obtain multidomain crystal; The pull rate of wherein said crystal pulling method is 0.7～1.3mm/h, and axial-temperature gradient is 35～40 ℃/cm, and speed of rotation is 12～15r/min;
Three, polarization: it is 1160～1210 ℃ that gained multidomain crystal in step 2 is placed in to temperature, and current density is 5mA/cm 2condition under the 28～32min that polarizes, the crystal after being polarized;
Four, cutting, polishing: the crystal after gained polarization in step 3 is cut, and then effects on surface carries out the polishing of optical quality level, obtains Hf:Dy:LiNbO 3crystal, completes the preparation of hafnium dysprosium double doping lithium niobate crystal.
Doping with rare-earth ions Dy in the present invention 3+be mainly reflected in the application of opticfiber communication aspect, and utilize the good non-linear optical property of lithium niobate crystals and electro-optical properties, it is combined with the characteristics of luminescence, can develop the optical integrated device of excellent property.And Hf 4+mix the photo-damage resistance that can effectively promote crystal.
Advantage of the present invention:
One, the Hf:Dy:LiNbO that prepared by the present invention 3crystal glossiness is high, uniform component, indefectible, without striation and flawless, produce, photodamage resistant performance is higher, can be as laser crystal material;
Two, Hf:Dy:LiNbO of the present invention 3the preparation method of crystal is simple, convenient operation, and crystalline growth velocity is fast;
Three, the Hf:Dy:LiNbO that prepared by the present invention 3crystal, to exploring a kind of novel complex function laser crystal material, has very important value.This crystalline material can be preparing compact type, laser diode-pumped, all solid state tunable laser has a extensive future, in addition to high-density storage, to prepare integrated optical device, infrared acquisition also significant.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of gained sample Hf8 crystal in embodiment;
Fig. 2 is the wafer shape appearance figure of gained sample Hf8 crystal in embodiment;
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure of gained sample Hf2 crystal in embodiment;
Fig. 4 is the ultraviolet-visible absorption spectroscopy figure of gained sample Hf4 crystal in embodiment;
Fig. 5 is the ultraviolet-visible absorption spectroscopy figure of gained sample Hf6 crystal in embodiment;
Fig. 6 is the ultraviolet-visible absorption spectroscopy figure of gained sample Hf8 crystal in embodiment.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment hafnium dysprosium double doping lithium niobate crystal, it is by Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3make; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities.
Embodiment two: that present embodiment is different from embodiment one is described Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3purity be 99.99%.Other is identical with embodiment one.
Embodiment three: that present embodiment is different from embodiment one or two is described HfO 2doping molar weight account for 2% of four kinds of raw material integral molar quantities.Other is identical with embodiment one or two.
Embodiment four: that present embodiment is different from one of embodiment one to three is described HfO 2doping molar weight account for 4% of four kinds of raw material integral molar quantities.Other is identical with one of embodiment one to three.
Embodiment five: that present embodiment is different from one of embodiment one to four is described HfO 2doping molar weight account for 6% of four kinds of raw material integral molar quantities.Other is identical with one of embodiment one to four.
Embodiment six: that present embodiment is different from one of embodiment one to four is described HfO 2doping molar weight account for 8% of four kinds of raw material integral molar quantities.Other is identical with one of embodiment one to four.
Embodiment seven: present embodiment is prepared the method for hafnium dysprosium double doping lithium niobate crystal, carry out according to the following steps:
One, mix: take four kinds of raw materials, be respectively Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3, then mix, obtain compound; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities;
Two, adopt Czochralski grown crystal: gained compound in step 1 is put into Pt crucible, then sintering 2～6h at 710～740 ℃, be warming up to again 1160～1180 ℃ and continue sintering 1～2h, be cooled to subsequently room temperature, then adopt crystal pulling method to carry out crystal growth, pass through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and anneal, obtain multidomain crystal; The pull rate of wherein said crystal pulling method is 0.7～1.3mm/h, and axial-temperature gradient is 35～40 ℃/cm, and speed of rotation is 12～15r/min;
Three, polarization: it is 1160～1210 ℃ that gained multidomain crystal in step 2 is placed in to temperature, and current density is 5mA/cm 2condition under the 28～32min that polarizes, the crystal after being polarized;
Four, cutting, polishing: the crystal after gained polarization in step 3 is cut, and then effects on surface carries out the polishing of optical quality level, obtains Hf:Dy:LiNbO 3crystal, completes the preparation of hafnium dysprosium double doping lithium niobate crystal.
Nb described in present embodiment 2o 5, LiCO 3, HfO 2and Dy 2o 3purity be 99.99%.
Embodiment eight: what present embodiment was different from embodiment seven is that in step 2, compound is put into Pt crucible, sintering 4h at 730 ℃ then, then be warming up to 1170 ℃ and continue sintering 1.5h.Other step and parameter are identical with embodiment seven.
Embodiment nine: present embodiment is different from embodiment seven or eight is that the pull rate of crystal pulling method described in step 2 is 1.0mm/h, and axial-temperature gradient is 38 ℃/cm, and speed of rotation is 13r/min.Other is identical with embodiment seven or eight.
Embodiment ten: present embodiment is different from one of embodiment seven to nine be in step 3 multidomain crystal to be placed in temperature be 1190 ℃, current density is 5mA/cm 2condition under the 30min that polarizes.Other is identical with one of embodiment seven to nine.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment:
The method of preparing hafnium dysprosium double doping lithium niobate crystal, carry out according to the following steps:
One, mix: take four kinds of raw materials, be respectively Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3, then mix, obtain compound; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities;
Two, adopt Czochralski grown crystal: gained compound in step 1 is put into Pt crucible, then sintering 4h at 730 ℃, be warming up to again 1180 ℃ and continue sintering 1h, be cooled to subsequently room temperature, then adopt crystal pulling method to carry out crystal growth, pass through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and anneal, obtain multidomain crystal; The pull rate of wherein said crystal pulling method is 1.2mm/h, and axial-temperature gradient is 37 ℃/cm, and speed of rotation is 13r/min;
Three, polarization: it is 1200 ℃ that gained multidomain crystal in step 2 is placed in to temperature, and current density is 5mA/cm 2condition under the 32min that polarizes, the crystal after being polarized;
Four, cutting, polishing: the crystal after gained polarization in step 3 is cut, and then effects on surface carries out the polishing of optical quality level, obtains Hf:Dy:LiNbO 3crystal, completes the preparation of hafnium dysprosium double doping lithium niobate crystal.
Nb described in the present embodiment 2o 5, LiCO 3, HfO 2and Dy 2o 3purity be 99.99%.
HfO in the present embodiment 2doping molar weight account for 2%, 4%, 6%, 8% of four kinds of raw material integral molar quantities, obtain successively four samples, called after Hf2, Hf4, Hf6 and Hf8;
The crystal morphology of the present embodiment gained sample Hf8 as shown in Figure 1, visible, crystal glossiness is high, uniform component, indefectible, without striation and flawless, produce.
The wafer pattern of the crystal of the present embodiment gained sample Hf8 as shown in Figure 2.
The present embodiment gained sample Hf2, Hf4, Hf6 and Hf8, its crystal is all cut into wafer according to 10mm * 10mm * 2.5mm (Z * X * Y) and carries out ultraviolet-visible absorption spectroscopy test, as shown in Fig. 3,4,5 and 6, can find out Hf:Dy:LiNbO 3crystal is at 428nm, 452nm, 472nm, 756nm, 806nm, 907nm, 1116nm, 1290nm and 1663nm place.The formation of each absorption peak is due to Dy 3+from ground state, to a state transition, cause.Along with the raising of Hf doping content, Dy 3+the peak position of term of spectrum transition do not change, and the intensity of absorption peak also changes not quite.
The present embodiment gained sample Hf2, Hf4, Hf6 and Hf8 adopt the photo-damage resistance of photic scattering threshold value exposure energy stream method test crystal, and experimental data is as shown in table 1.The photo-damage resistance that the photo-damage resistance of present embodiment gained Hf4 crystal prototype is compared Hf2 crystal prototype has improved 2 orders of magnitude.
Table 1Hf:Dy:LiNbO 3the light scattering exposure energy flow threshold value of crystal
Sample Hf2 Hf4 Hf6 Hf8
R(J/cm 2) 0.624 51.322 58.364 60.185
The present embodiment gained sample Hf2, Hf4, Hf6 and Hf8, the lower appropriate crystal of cutting, cleans up sample with acetone, alcohol etc. respectively, then wafer is smashed to pieces, is positioned in agate mortar and grinds into about 200 object powder; On polycrystalline diffractometer, test its X-ray powder diffraction peak, the experimental data that XRD is recorded calculates the lattice parameter of each sample by method of least squares, and result is as shown in table 2, and has calculated unit cell volume V:V=a with reference to formula below 2c * cos30 °.
Table 2Hf:Dy:LiNbO 3the lattice parameter of crystal
Figure BDA0000451113830000051

Claims (10)

1. hafnium dysprosium double doping lithium niobate crystal, is characterized in that it is by Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3make; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities.
2. hafnium dysprosium double doping lithium niobate crystal according to claim 1, is characterized in that described Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3purity be 99.99%.
3. hafnium dysprosium double doping lithium niobate crystal according to claim 1 and 2, is characterized in that described HfO 2doping molar weight account for 2% of four kinds of raw material integral molar quantities.
4. hafnium dysprosium double doping lithium niobate crystal according to claim 3, is characterized in that described HfO 2doping molar weight account for 4% of four kinds of raw material integral molar quantities.
5. hafnium dysprosium double doping lithium niobate crystal according to claim 4, is characterized in that described HfO 2doping molar weight account for 6% of four kinds of raw material integral molar quantities.
6. hafnium dysprosium double doping lithium niobate crystal according to claim 5, is characterized in that described HfO 2doping molar weight account for 8% of four kinds of raw material integral molar quantities.
7. the method for preparation hafnium dysprosium double doping lithium niobate crystal as claimed in claim 1, is characterized in that it carries out according to the following steps:
One, mix: take four kinds of raw materials, be respectively Nb 2o 5, LiCO 3, HfO 2and Dy 2o 3, then mix, obtain compound; Wherein said LiCO 3in Li and Nb 2o 5in the mol ratio of Nb be 0.946:1, Dy 2o 3doping molar weight account for 0.5% of four kinds of raw material integral molar quantities, HfO 2doping molar weight account for 2%～8% of four kinds of raw material integral molar quantities;
Two, adopt Czochralski grown crystal: gained compound in step 1 is put into Pt crucible, then sintering 2～6h at 710～740 ℃, be warming up to again 1160～1180 ℃ and continue sintering 1～2h, be cooled to subsequently room temperature, then adopt crystal pulling method to carry out crystal growth, pass through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and anneal, obtain multidomain crystal; The pull rate of wherein said crystal pulling method is 0.7～1.3mm/h, and axial-temperature gradient is 35～40 ℃/cm, and speed of rotation is 12～15r/min;
Three, polarization: it is 1160～1210 ℃ that gained multidomain crystal in step 2 is placed in to temperature, and current density is 5mA/cm 2condition under the 28～32min that polarizes, the crystal after being polarized;
Four, cutting, polishing: the crystal after gained polarization in step 3 is cut, and then effects on surface carries out the polishing of optical quality level, obtains Hf:Dy:LiNbO 3crystal, completes the preparation of hafnium dysprosium double doping lithium niobate crystal.
8. the preparation method of hafnium dysprosium double doping lithium niobate crystal according to claim 7, is characterized in that in step 2, compound is put into Pt crucible, sintering 4h at 730 ℃ then, then be warming up to 1170 ℃ and continue sintering 1.5h.
9. the preparation method of hafnium dysprosium double doping lithium niobate crystal according to claim 8, the pull rate that it is characterized in that crystal pulling method described in step 2 is 1.0mm/h, and axial-temperature gradient is 38 ℃/cm, and speed of rotation is 13r/min.
10. the preparation method of hafnium dysprosium double doping lithium niobate crystal according to claim 9, is characterized in that in step 3 that it is 1190 ℃ that multidomain crystal is placed in temperature, and current density is 5mA/cm 2condition under the 30min that polarizes.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106012019A (en) * 2016-06-12 2016-10-12 哈尔滨理工大学 Hafnium and dysprosium double-doped lithium niobate crystal and preparation method thereof
CN106087057A (en) * 2016-06-12 2016-11-09 哈尔滨理工大学 Hafnium neodymium ytterbium thulium four doped lithium columbate crystal and preparation method thereof
CN110230098A (en) * 2018-03-06 2019-09-13 哈尔滨理工大学 Ytterbium europium double doping lithium niobate crystal and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106012019A (en) * 2016-06-12 2016-10-12 哈尔滨理工大学 Hafnium and dysprosium double-doped lithium niobate crystal and preparation method thereof
CN106087057A (en) * 2016-06-12 2016-11-09 哈尔滨理工大学 Hafnium neodymium ytterbium thulium four doped lithium columbate crystal and preparation method thereof
CN110230098A (en) * 2018-03-06 2019-09-13 哈尔滨理工大学 Ytterbium europium double doping lithium niobate crystal and preparation method thereof

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Application publication date: 20140402