CN105133015B - One kind doping vanadic acid terbium magneto-optical crystal, growing method and its application - Google Patents

One kind doping vanadic acid terbium magneto-optical crystal, growing method and its application Download PDF

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CN105133015B
CN105133015B CN201510478490.0A CN201510478490A CN105133015B CN 105133015 B CN105133015 B CN 105133015B CN 201510478490 A CN201510478490 A CN 201510478490A CN 105133015 B CN105133015 B CN 105133015B
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magneto
crystal
optical crystal
optical
vanadic acid
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CN105133015A (en
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胡章贵
涂衡
赵营
岳银超
范飞镝
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Technical Institute of Physics and Chemistry of CAS
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The present invention relates to a kind of magneto-optical crystal, production method and its application of the vanadic acid terbium that adulterates, the molecular formula of the doping vanadic acid terbium magneto-optical crystal is CaxMyTb1‑x‑yVO4, wherein, M is rare earth element and alkali metal, 0.01≤x≤0.5,0≤y≤0.5.Serial crystal Faraday rotation angle at 1064nm is 1.3 1.5 times of TGG crystal, and the crystal is congruent melting, can use Czochralski grown, easily grow large-size crystals, cost of material is low, can effectively reduce magneto-optical crystal cost.By magneto-optical crystal device that the magneto-optical crystal makes when making magneto optic isolator due to big Verdet constant, the requirement to magneto-optical crystal length can be reduced, it is and existing;Technology is compared, and is designed more compact with device, is reduced the use number of magneto-optical crystal in isolator, the advantages of reducing cost.The present invention simultaneously can be used for photoswitch making.

Description

One kind doping vanadic acid terbium magneto-optical crystal, growing method and its application
Technical field
The invention belongs to crystalline material technical field, and in particular to one kind doping vanadic acid terbium magneto-optical crystal, growing method and It is applied.
Background technology
Magneto-optical crystal is in the ultraviolet critical function crystal to infrared band with magneto-optic effect.Utilize its Faraday effect Magneto optic isolator, magneto-optic deflector, magneto-optic shutter, magneto-optic modulator, magneto-optic circulator, magneto-optic delayer, magneto-optic can be made Fibre optic current sensor of information processing system and high-intensity magnetic field and hv transmission line etc..
At present, main flow magneto-optical crystal terbium gallium garnet (TGG) crystal of Commercialization application, the crystal is by Fujian Fu Jing sections The crystal that skill limited company developed in 2008, is mainly used in making the optimal magnetic of Faraday polarization apparatus and isolator Luminescent material, applicable wavelengths are 400-1100nm (not including 470-500nm).Its advantage is:TGG monocrystalline has larger magneto-optic normal Several, highly thermally conductive property, low light loss and high laser damage threshold, are widely used in YAG, mix the amplification of the multistage such as Ti sapphires, ring In type, seed injection laser.It has the disadvantage:At high temperature, because its component has volatility, TGG crystal is difficult to grow height The crystal of quality.
The Verdet constant of terbium aluminium garnet (TAG) and its serial crystal of doping is about 1.5 times of TGG, while also having There is higher transmitance, be the visible and near-infrared magneto-optical crystal of excellent combination property.But it is off-congruent melt when it is melted, Czochralski grown can not be used, is also difficult to obtain block high quality crystal at present.
TbVO4Crystal has been reported as the application of magneto-optical crystal, and its applicable wavelengths is 500-1500nm, and crystal exists Faraday rotation angle is 1.45 times of TGG crystal at 1064nm, but extinction ratio is 28.7dB, (>=30dB) smaller than TGG crystal, shadow The utilization of crystal is rung.
Based on this, spy proposes the present invention.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide one kind doping vanadic acid terbium magneto-optical crystal, while also carrying Method and its production of the optoisolator and photoswitch that are prepared for doping vanadic acid terbium magneto-optical crystal preparation method and using the crystal Product.
The invention provides a kind of magneto-optical crystal for the vanadic acid terbium that adulterates, its molecular formula is CaxMyTb1-x-yVO4, wherein:
M is rare earth element or alkali metal;
X is 0.01≤x≤0.5;
Y is 0≤y≤0.5.
In above-mentioned crystal:
The rare earth element includes Sc, Y, Lu, Gd, Ca, Ce, Pr, La, Nd, Sm, Er, Pm, Sm, Eu, Dy, Ho, Tm or Yb In one or more;
The alkali metal including Li, Na, K, Rb or Cs etc. in one or more;
Crystal Faraday rotation angle at 1064nm is 1.3-1.5 times of the TGG crystal of current commercialization.
The magneto-optical crystal, preferably Ca0.1Tb0.9VO4, it is TGG crystal at 1064nm that its Faraday rotation angle, which is, 1.4 again;Preferably Ca0.2Y0.1Tb0.7VO4, its Verdet constant is -58rad/mT at 1064nm.
Present invention also offers a kind of growing method of magneto-optical crystal, the growing method is czochralski method.
Preferably, the growing method comprises the following steps:
(1) Ca is pressedxMyTb1-x-yVO4Crystal stoichiometry ratio weighs raw materials of Ca CO3、Tb4O7, V2O5, doping M metal oxidations Thing, raw material is well mixed, and is fitted into mould and is put into crucible after briquetting and is sintered, 800-1300 DEG C of sintering temperature is mixed Miscellaneous vanadic acid terbium magneto-optical crystal polycrystal material;
(2) doping vanadic acid terbium magneto-optical crystal polycrystal material will be obtained to be put into Iridium Crucible, Iridium Crucible is put into single crystal growing furnace It is interior, vacuumize and be filled with protective gas, heated using Frequency Induction Heating mode, until polycrystal material fusing, makes melt mixed equal It is even;
(3) YVO is used4Or TbVO4For seed crystal, in seed crystal tripping in melt, will sequentially pass through wash it is brilliant, receive neck, it is shouldering, isometrical And finishing phase;
(4) after crystal growth terminates, by crystal pull to depart from melt, and slowly temperature is reduced to room temperature, and take Go out crystal.
(5) crystal-cut is annealed into after device, being put into annealing furnace.
In aforementioned production method:
In step (1):
The time of sintering is 2-20 hours;
Step (2):
Described protective gas is argon gas or nitrogen.
In step (3):
The seed crystal direction is<100>、<001>With<111>Direction;
The technological parameter controlled during crystal growth is:45-90 ° of shouldering angle, pull rate 0.3-2mm/h, rotating speed 12-30 Rev/min, 0-20 DEG C of rate of temperature fall/h;
In the step (4):
The speed of cooling is 10-80 DEG C/h.
In the step (5):
Crystal annealing can be carried out in atmosphere, under oxidizing atmosphere or reducing atmosphere.
Annealing can effectively improve the quality of crystal, improve the uniformity of crystal color.
The invention also discloses crystal in terms of prepare magneto optic isolator, magneto-optical crystal device and photoswitch on application.
The magneto-optical crystal that the present invention is provided has the advantages that:
1st, it is produced by the present invention doping vanadic acid terbium magneto-optical crystal, with stablizing at room temperature, do not decompose, not deliquescence the advantages of.
Present invention doping vanadic acid terbium magneto optical single crystal has congruent melting characteristic, is adapted to use Czochralski grown, easily growth Go out large-size crystals.Growth cycle is short, and cost of material is low, can realize large-scale batch production, can effectively reduce crystal The cost of device.
2nd, present invention doping vanadic acid terbium magneto-optical crystal Faraday rotation angle 1064nm at is 1.3-1.5 times of TGG crystal, With existing TbVO4Crystal phase ratio, present invention gained crystal is more easy to grow the crystal of high-quality, crystal extinction ratio it is higher (>= 32dB).It is brilliant to magneto-optic because it has big Verdet constant during the magneto optic isolator made using the magneto-optical crystal of the present invention The requirement of body length is relatively low, compared with prior art, and more compact, the use number of magneto-optical crystal in isolator is designed with device Less, the more low advantage of cost.
Brief description of the drawings
Fig. 1 is the Ca prepared0.1Tb0.9VO4Polycrystal material X-ray powder diffraction pattern;
Fig. 2 is polarization relationship type optoisolator schematic diagram of the present invention, wherein 1:The polarizer;2:Faraday rotator; 3:Analyzer, B is complementary field, and L is light path;
Fig. 3 is 1 in polarization independent type optical isolator schematic diagram of the present invention, figure:Polarization beam apparatus;2:Faraday rotation Device;3:The wave plate of λ/2;4:Polarization beam apparatus, B is complementary field, and L is light path;
Fig. 4 is 1 in photoswitch schematic diagram of the present invention, figure:The polarizer;2:Faraday rotator;3:Analyzer, 4:Electricity Flow impulse generator;B is complementary field, and L is light path.
Embodiment
The embodiment to the present invention is described in further detail with reference to the accompanying drawings and examples.Following examples For illustrating the present invention, but it is not limited to the scope of the present invention.
Embodiment 1:Ca0.2Y0.1Tb0.7VO4The preparation of monocrystalline
(1) high pure raw material CaCO is weighed3、Tb4O7、V2O5And Y2O3, load weighted raw material is well mixed, is fitted into mould Crucible is put into after briquetting to be sintered, 1200 DEG C of sintering temperature, sintered 12 hours or so, obtain Y and Ca doping TbVO4Polycrystalline Material;
(2) take in 650 grams of the polycrystal material that step (1) is obtained, the Iridium Crucible for putting it into a diameter of 60 millimeters, then by iridium Golden crucible, which is put into single crystal growing furnace, to be vacuumized, and is filled with protective gas nitrogen, and using Frequency Induction Heating mode, rise temperature is extremely 1740 degree or so, polycrystal material fusing, then temperature is improved into 8 DEG C, and constant temperature ten minutes, make melt mixed uniform.
(2) use<100>Direction TbVO4As seed crystal, it is slowly dropped on melt near 0.5-1.5 centimeters and is stopped Stay 1 minute, then seed crystal is quickly fallen into melt to 1-1.5 centimetres, and rapidly propose seed crystal from melt, crystalline substance is washed in completion;Directly Reduction melt temperature is connect to 1735 degree or so, seed crystal top is slowly fallen into melt, makes seed crystal top slow mechanism dissolved.Start drop Warm pulling growth, sequentially passes through receipts neck, shouldering, isometrical and finishing phase.Wherein:
When receiving neck, pull rate is 1.5mm/h, keeps melt temperature constant, is gradually reduced crystal diameter, when a diameter of During 1.5mm, start, with 5-15 DEG C/h of cooling, to carry out shouldering, pull rate is reduced into 1mm/h, when crystal diameter is 20- During 30mm, isodiametric growth is carried out.When crystal length reaches 20-40mm, crystal is pulled by improving pull rate.
(3) setting cooling and cycle of annealing, be properly filled into air, with 10 DEG C/h cooling 8 hours, then with 20 DEG C/it is small When be cooled to 500 DEG C, be finally cooled to room temperature with 30 DEG C/h.Obtain Y0.1Tb0.9VO4Monocrystal, crystalline size be Ф 26 × 30mm。
Embodiment 2:Ca0.1Tb0.9VO4The preparation of monocrystalline
Consistent with the operating procedure of embodiment one, difference is:
Without blended metal oxide, in crystal growth phase, use<001>Direction TbVO4As seed crystal, grow Crystal be Ca0.1Tb0.9VO4, symmetrically, crystalline size is 21 × 26mm of Ф to habit.
Wherein Ca0.1Tb0.9VO4Polycrystal material X-ray powder diffraction pattern is as shown in Figure 1.
Embodiment 3:Polarize the preparation of relationship type optoisolator
Optoisolator schematic diagram as shown in Figure 2, using 1064nm lasers as light source, embodiment 1 is made Ca0.2Y0.1Tb0.7VO4Magneto-optical crystal device is inserted in magnetic field, front and rear to be respectively put into polarizer and analyzer, analyzer polarization side To with polarizer polarization direction angle at 45 °.Optical direction is parallel with magnetic direction.
Under magnetic field condition, after the 1064nm laser beams sent by laser are by the polarizer, as polarised light, by magnetic Luminescent crystal device polarization direction have rotated 45 °, and analyzer polarization direction and the polarizer polarization direction angle at 45 ° so that light Pass through, and the polarised light reflected continues to rotate 45 ° in the same direction after analyzer, magneto-optical crystal device, I.e. polarization direction is just vertical with polarizer polarization direction, then light can not be back through.
Embodiment 4:The preparation of polarization independent type optical isolator
Polarization independent type optical isolator schematic diagram as shown in Figure 3, using 1064nm lasers as light source, along light path Direction is respectively magneto-optical crystal device, the wave plate of λ/2 and the polarization beam apparatus that polarization beam apparatus, embodiment 2 make.
Under magnetic field condition, the 1064nm laser beams sent by laser are separated by a polarization beam apparatus, are changed into vertical Polarised light and parallel polarized light.This two-beam rotates 45 ° by Faraday rotator in the same direction, then is revolved by the wave plate of λ/2 Turn 45 °, orthogonal polarized light is changed into parallel polarized light, and parallel polarized light is changed into orthogonal polarized light, and one is combined into by polarization beam apparatus Beam light output.During reverse transfer, its light path is identical with positive light, main difference is that the direction and half rotated by magneto-optical crystal Wave plate direction of rotation contrast, deviates forward entrance light in two beam reversal's light outgoing in the presence of beam splitter, so that real Now polarize unrelated optically isolated.
Embodiment 5:Magneto-optic shutter
Magneto-optic shutter structural representation as shown in Figure 4, using 1064nm lasers as light source, embodiment 1 is made The magneto-optical crystal device of work is inserted in magnetic field, front and rear to be respectively put into polarizer and analyzer, analyzer polarization direction and the polarizer Polarization direction is into 0 ° of angle.
Optical direction is parallel with magnetic direction.Magnetic field break-make is controlled with current pulser.If there is no magnetic field, by swashing After the 1064nm laser beams that light device is sent are by the polarizer, as polarised light, do not rotated by magneto-optical crystal device polarization direction, It can be projected by analyzer, photoswitch is in opened condition.If produce external magnetic field by current pulser, light passes through Magneto-optical crystal device polarization direction is rotated by 90 °, and light beam can not be by analyzer, and photoswitch is in closed mode.
The magneto-optical crystal device that the magneto-optical crystal of the doping vanadic acid terbium provided using the present invention is made is making magneto-optic isolation Due to big Verdet constant, the requirement to magneto-optical crystal length can be reduced during device, compared with prior art, with device Part design is more compact, reduces isolator and light and opens the light the use number of middle magneto-optical crystal, the advantages of reducing cost.
Although above having made to retouch in detail to the present invention with general explanation, embodiment and experiment State, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art 's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, are belonged to claimed Scope.

Claims (7)

1. a kind of magneto-optical crystal for the vanadic acid terbium that adulterates, it is characterised in that its molecular formula is CaxMyTb1-x-yVO4, wherein:
M is rare earth element y;
X is 0.01≤x < 0.5;
Y is 0≤y < 0.5;
Magneto-optical crystal Faraday rotation angle at 1064nm is 1.3-1.5 times of TGG crystal.
2. magneto-optical crystal according to claim 1, it is characterised in that the magneto-optical crystal is Ca0.1Tb0.9VO4, its farad The anglec of rotation is 1.4 times for TGG crystal at 1064nm.
3. magneto-optical crystal according to claim 1, it is characterised in that the magneto-optical crystal is Ca0.2Y0.1Tb0.7VO4, its takes Your moral constant is -58rad/mT at 1064nm.
4. the growing method of the magneto-optical crystal described in claim any one of 1-3, it is characterised in that this method is czochralski method.
5. growing method according to claim 4, it is characterised in that the growing method comprises the following steps:
(1) Ca is pressedxMyTb1-x-yVO4Crystal stoichiometry ratio weighs raw materials of Ca CO3、Tb4O7, V2O5, adulterate M metal oxides, will Raw material is well mixed, and is sintered after briquetting, 800-1300 DEG C of sintering temperature, obtains the vanadic acid terbium magneto-optical crystal polycrystal material that adulterates;
(2) the doping vanadic acid terbium magneto-optical crystal polycrystal material that step (1) is obtained is put into Iridium Crucible, Iridium Crucible is put into list In brilliant stove, vacuumize and be filled with protective gas, heated using Frequency Induction Heating mode, until polycrystal material fusing, mixes melt Close uniform;
(3) with YVO4Or TbVO4For seed crystal, it is put into melt, sequentially passes through and wash brilliant, receipts neck, shouldering, isometrical and ending completion list Crystalline substance lifting;
(4) by crystal pull to depart from melt, and temperature is slowly reduced to room temperature, and take out crystal;
(5) by crystal-cut into after device, annealing.
6. growing method according to claim 5, it is characterised in that in the step (1):The time of sintering is that 2-20 is small When;In the step (3):The technological parameter controlled during crystal growth is:45-90 ° of shouldering angle, pull rate 0.3-2mm/h, turn Fast 12-30 revs/min, 0-20 DEG C of rate of temperature fall/h.
7. magneto-optical crystal described in claim any one of 1-3 in terms of prepare optoisolator and photoswitch on application.
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