CN101876086A - Preparation method of Zr and Mg co-doped iron lithium niobate crystal - Google Patents

Preparation method of Zr and Mg co-doped iron lithium niobate crystal Download PDF

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CN101876086A
CN101876086A CN 201010234894 CN201010234894A CN101876086A CN 101876086 A CN101876086 A CN 101876086A CN 201010234894 CN201010234894 CN 201010234894 CN 201010234894 A CN201010234894 A CN 201010234894A CN 101876086 A CN101876086 A CN 101876086A
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lithium niobate
niobate crystal
iron lithium
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doped
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徐超
冷雪松
许磊
孙婷
徐玉恒
孙亮
杨春晖
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention discloses a preparation method of a Zr and Mg co-doped iron lithium niobate crystal, relating to a preparation method of an iron lithium niobate crystal and solving the problem of lower signal-to-noise ratio caused by weak photoinduced scattering resistant power of the iron lithium niobate crystal. The preparation method comprises the steps of: weighting MgO, ZrO2, Fe2O3, Nb2O5 and Li2CO3, and then mixing to obtain a mixture; drying the mixture and then placing into a platinum crucible, calcining for 3 hours at 750 DEG C and then calcining for 4 hours at 1150 DEG C to obtain a polycrystal raw material doped with lithium niobate; and placing the platinum crucible loading with the polycrystal raw material doped with the lithium niobate into a intermediate frequency furnace, and pulling to obtain the Zr and Mg co-doped iron lithium niobate crystal under the conditions that the pulling speed is 0.3-1.8mm/h, the axial temperature gradient is 40-50 DEG C/cm and the rotation speed is 15-25r/min. The Zr and Mg co-doped iron lithium niobate crystal of the invention has the photoinduced scattering resistant power reaching 4.8-104W/cm<2>.

Description

The preparation method of Zr, Mg co-doped iron lithium niobate crystal
Technical field
The present invention relates to a kind of preparation method of iron lithium niobate crystal.
Background technology
Along with the arrival of information age, the developing rapidly of multimedia technology, people need to use with canned data quantity and unprecedentedly increase.Yet traditional magnetic storage and CD storage technique have approached the limit of memory capacity owing to be subjected to the restriction of storage principle, more and more can not satisfy people to the demand of big capacity storage.But the holographic optical memory technology since have storage capacity big, can carry out the memory technology of new generation that content addressed, advantages such as addressing speed is fast, the long diamagnetism interference of storage life are considered to tool potentiality by parallel mode.The performance of holographic optical storage depends on storage medium material again to a great extent.
In numerous optical storage medias, iron lithium niobate (Fe:LiNbO 3) crystal because have the diffraction efficiency height, storage advantages such as dynamicrange is big are considered to one of ideal material of body holographic optical storage.Weak (the Fe:LiNbO of anti-photic scattering power but iron lithium niobate crystal also exists 3The anti-photic scattering power of crystalline only is 3.7 * 10W/cm 2) and the lower problem of the signal to noise ratio that causes, this has limited the practical application of iron lithium niobate crystal in the holographic optical storage to a certain extent.
Summary of the invention
To the objective of the invention is in order solving a little less than the anti-photic scattering power of iron lithium niobate crystal and the lower problem of signal to noise ratio that causes, the preparation method of a kind of Zr, Mg co-doped iron lithium niobate crystal to be provided.
The preparation method of Zr of the present invention, Mg co-doped iron lithium niobate crystal is as follows: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.946～1.400 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Mixture; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.3～1.8mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 15～25r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal; The purity of MgO described in the step 1 is 99.99%; ZrO described in the step 1 2Purity be 99.99%; Fe described in the step 1 2O 3Purity be 99.99%; Nb described in the step 1 2O 5Purity be 99.99%; Li described in the step 1 2CO 3Purity be 99.99%.
The present invention is two anti-light loss damage element Zr and Mg of mixing in lithium columbate crystal, adopt the Czochralski grown crystal that improves Li/Nb ratio growth means, obviously improved the ability of Zr, Mg co-doped iron lithium niobate crystal photo scattering resistance, the Photo scattering resistance ability of Zr, Mg co-doped iron lithium niobate crystal can reach 4.8 * 10 4W/cm 2Zr of the present invention, Mg co-doped iron lithium niobate crystal are light brown, and diameter is approximately 30mm, highly about 20mm, and do not have wrap, no striped, flawless.
Description of drawings
Fig. 1 is an iron lithium niobate crystal pre-irradiation hot spot; Fig. 2 is a hot spot behind the iron lithium niobate crystal irradiation; Fig. 3 is gained Zr in the embodiment 21, Mg co-doped iron lithium niobate crystal pre-irradiation hot spot; Fig. 4 is a hot spot behind gained Zr in the embodiment 21, the Mg co-doped iron lithium niobate crystal irradiation.
Embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.946～1.400 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Mixture; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.3～1.8mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 15～25r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
Zr, the Mg co-doped iron lithium niobate crystal of present embodiment preparation are light brown, and diameter is approximately 30mm, highly about 20mm, and do not have wrap, no striped, flawless.
Is that 1180 ℃, current density are 5mA/cm with the Zr of present embodiment preparation, Mg co-doped iron lithium niobate crystal in temperature 2Polarize under the condition, (size of Z * X * Y) is cut into wafer according to 20mm * 10mm * 2mm then, and carrying out high-precision optical grade polishing, the semiconductor laser with 532nm is that incident light source (output rating can reach 90mW) has been tested the anti-photic scattering property through polishing back wafer again.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal can reach 4.8 * 10 4W/cm 2
Embodiment two: present embodiment and embodiment one are different is that the purity of MgO described in the step 1 is 99.99%.Other is identical with embodiment one.
Embodiment three: that present embodiment and embodiment one are different is ZrO described in the step 1 2Purity be 99.99%.Other is identical with embodiment one.
The specific embodiment four: that present embodiment and the specific embodiment one are different is Fe described in the step 1 2O 3Purity be 99.99%.Other is identical with embodiment one.
The specific embodiment five: that present embodiment and the specific embodiment one are different is Nb described in the step 1 2O 5Purity be 99.99%.Other is identical with embodiment one.
Embodiment six: that present embodiment and embodiment one are different is Li described in the step 1 2CO 3Purity be 99.99%.Other is identical with embodiment one.
Embodiment seven: present embodiment is different with one of embodiment one to six is that Li element and Nb element mol ratio are 1 ﹕ 1 in the step 1.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment and embodiment seven were different is that pull rate described in the step 3 is 0.5～1.5mm/h.Other is identical with embodiment seven.
Embodiment nine: what present embodiment and embodiment seven were different is that pull rate described in the step 3 is 1mm/h.Other is identical with embodiment seven.
Embodiment ten: what present embodiment was different with one of embodiment one to nine is that speed of rotation described in the step 3 is 20r/min.Other is identical with one of embodiment one to nine.
The specific embodiment 11: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.946 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 1.8mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 15r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 1.6 * 10 3W/cm 2
The specific embodiment 12: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 1.400 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.3mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 25r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 4.8 * 10 4W/cm 2
The specific embodiment 13: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.950 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 1.7mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 16r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 2.1 * 10 3W/cm 2
The specific embodiment 14: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.960 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 1.5mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 17r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 3.1 * 10 3W/cm 2
The specific embodiment 15: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.970 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 1.4mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 18r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 5.3 * 10 3W/cm 2
The specific embodiment 16: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.980 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 1.1mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 19r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 7.8 * 10 3W/cm 2
The specific embodiment 17: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.990 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 1.0mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 20r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 9.2 * 10 3W/cm 2
The specific embodiment 18: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 1 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.9mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 21r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 1.9 * 10 4W/cm 2
The specific embodiment 19: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 1.100 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.7mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 22r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 2.3 * 10 4W/cm 2
The specific embodiment 20: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 1.200 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.6mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 23r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 2.9 * 10 4W/cm 2
The specific embodiment 21: the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows in the present embodiment: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 1.300 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Gross weight be the mixture of 200g; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.4mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 24r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
The Zr of present embodiment preparation, the Photo scattering resistance ability of Mg co-doped iron lithium niobate crystal are 3.6 * 10 4W/cm 2

Claims (10)

1.Zr, the preparation method of Mg co-doped iron lithium niobate crystal, it is characterized in that the preparation method of Zr, Mg co-doped iron lithium niobate crystal is as follows: be the 1%(mole according to the MgO doping one), ZrO 2Doping is the 1%(mole), Fe 2O 3Doping is the 0.03%(quality) and Li element and Nb element mol ratio be that the ratio of 0.946～1.400 ﹕ 1 takes by weighing MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3, mix then, obtain MgO, ZrO 2, Fe 2O 3, Nb 2O 5And Li 2CO 3Mixture; Two, will put into platinum crucible after the oven dry of the mixture of step 1, then 750 ℃ of calcinings 3 hours, again 1150 ℃ of sintering 4 hours, obtain the polycrystal raw material of doped lithium columbate; The platinum crucible that three, the polycrystal raw material of doped lithium columbate will be housed is put into intermediate frequency furnace, be that 0.3～1.8mm/h, axial-temperature gradient are that 40～50 ℃/cm, rotary speed are to lift under the condition of 15～25r/min in pull rate then, namely get Zr, Mg co-doped iron lithium niobate crystal.
2. according to the preparation method of the described Zr of claim 1, Mg co-doped iron lithium niobate crystal, the purity that it is characterized in that MgO described in the step 1 is 99.99%.
3. according to the preparation method of the described Zr of claim 1, Mg co-doped iron lithium niobate crystal, it is characterized in that ZrO described in the step 1 2Purity be 99.99%.
4. according to the preparation method of the described Zr of claim 1, Mg co-doped iron lithium niobate crystal, it is characterized in that Fe described in the step 1 2O 3Purity be 99.99%.
5. according to the preparation method of the described Zr of claim 1, Mg co-doped iron lithium niobate crystal, it is characterized in that Nb described in the step 1 2O 5Purity be 99.99%.
6. according to the preparation method of the described Zr of claim 1, Mg co-doped iron lithium niobate crystal, it is characterized in that Li described in the step 1 2CO 3Purity be 99.99%.
7. according to the preparation method of claim 1,2,3,4,5 or 6 described Zr, Mg co-doped iron lithium niobate crystal, it is characterized in that Li element and Nb element mol ratio are 1 ﹕ 1 in the step 1.
8. according to the preparation method of the described Zr of claim 7, Mg co-doped iron lithium niobate crystal, it is characterized in that pull rate described in the step 3 is 0.5～1.5mm/h.
9. according to the preparation method of the described Zr of claim 7, Mg co-doped iron lithium niobate crystal, it is characterized in that pull rate described in the step 3 is 1mm/h.
10. according to the preparation method of claim 1,2,3,4,5,6,8 or 9 described Zr, Mg co-doped iron lithium niobate crystal, it is characterized in that speed of rotation described in the step 3 is 20r/min.
CN 201010234894 2010-07-23 2010-07-23 Preparation method of Zr and Mg co-doped iron lithium niobate crystal Pending CN101876086A (en)

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CN106929917A (en) * 2017-04-25 2017-07-07 南开大学 A kind of 90 ° of double-doped lithium niobate crystals of phase matched of room temperature

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