CN106192001A - Caesium lead carbon oxygen iodine birefringece crystal and preparation method and purposes - Google Patents
Caesium lead carbon oxygen iodine birefringece crystal and preparation method and purposes Download PDFInfo
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Abstract
The present invention relates to a kind of caesium lead carbon oxygen iodine birefringece crystal for infrared-ultraviolet band and preparation method and purposes, this crystal-chemical formula is Cs3Pb2(CO3)3I, molecular weight 1120.04, belong to monoclinic system, space group is C2/m, and cell parameter is a=24.549 (3), b=5.4233 (8), c=12.8598 (16), β=114.533 (8) °, V=1557.5 (4)3, Z=4;This caesium lead carbon oxygen iodine birefringece crystal is positive biaxial crystal, nz-ny>ny-nx, it is 300-3000nm through scope;Birefringence is between 0.084 (3000nm)-0.374 (340nm);Crystal uses Hydrothermal Growth;The crystal obtained by the present invention is prone to growth, is prone to cut, be prone to grind, be easily polished and be prone to preserve, stable in the air, is difficult to deliquescence;Can be used for making the polarization beam splitter prisms such as Glan type prism, wollaston prism, Rochon prism or light beam separation polariser, have important application at optics and communication field.
Description
Technical field
The present invention relates to a kind of caesium lead carbon oxygen iodine birefringece crystal and preparation method and purposes, particularly one can be used in infrared-
The molecular formula of deep ultraviolet wave band is Cs3Pb2(CO3)3The caesium lead carbon oxygen iodine birefringece crystal of I and preparation thereof and purposes.
Background technology
The crystal with birefringent phenomenon becomes birefringece crystal.Birefringece crystal, as a kind of optical crystal, is lived people
And have important effect in commercial Application.Line polarized light can be obtained, it is achieved the displacement to light beam by birefringece crystal
Deng, thus made optoisolator, circulator, pattern displacement its, optics deception device and optical modulator etc..
What is birefringent phenomenon?It is the key property that light shows when propagating in dielectric crystal heterogeneous
One of, the shear wave character that can use up is explained.When light is propagated in heterogeneous body (except the crystal of cubic system), remove
Indivedual special directions (along optical axis direction) outward, can change its vibration characteristic, is decomposed into two electric field intensitys vibrations
Direction is orthogonal, and spread speed is different, the phenomenon of the two bundle polarized light that refractive index does not waits.Produce the crystalline substance of birefringent phenomenon
Body can be divided into uniaxial crystal and biaxial crystal.Uniaxial crystal: the crystal of only one of which optical axis, such as calcite, quartz, red treasured
Stone, ice etc.;Biaxial crystal: have the crystal of two optical axises, such as Muscovitum, crystallization sulfur, sapphire, olivine etc.
Conventional birefringent material mainly has α-BaB2O4Crystal, MgF2Crystal, LiNbO3Crystal, YVO4Crystal, side
Solve stone crystal and rutile crystal etc..But, these birefringent materials all also exist weak point: α-BaB2O4By
In there are solid-state phase changes, it is easy to ftracture in crystal growing process;MgF2Crystal is 110-8500nm through scope,
It is that one is applied to the good material of deep ultraviolet, but its birefringence is the least, is not suitable for use in manufacturing Glan prism,
Being only used for Rochon prism, and the light velocity angle of departure is little, device size is big, uses inconvenience;LiNbO3Crystal can be easily obtained big chi
Very little crystal, but birefringence is the least;YVO4A kind of synthetic birefringence crystal of good performance, but it through scope
It is 400-5000nm, it is impossible to for ultra-violet (UV) band, and due to YVO4Fusing point is high, it is necessary to use iridium crucible to carry out pulling growth,
And the atmosphere of growth is weak oxygen atmosphere, thus there is the problem of appraising at the current rate of iridium when growth, so that the matter of crystal
Amount declines, and is difficult to obtain high-quality crystal;Mainly with the calcite crystalline substance being naturally occurring, synthetic is more tired
Difficulty, stock size is smaller, and impurity content is higher, it is impossible to meet the requirement of large scale optics polarization element, and
And be prone to dissociate, to process relatively difficult, crystal utilization rate is low;Rutile is also main to be naturally occurring, and manually closes
Becoming relatively difficult, and size is less, hardness is big, it is difficult to processing.The Cs that the present invention provides3Pb2(CO3)3I birefringece crystal
Through wide ranges (300-3000nm), and birefringence big (0.084-0.374), is a kind of birefringence that can be used for ultraviolet
Material.
Summary of the invention
It is an object of the invention to, it is provided that a kind of caesium lead carbon oxygen iodine birefringece crystal, this crystal-chemical formula is Cs3Pb2(CO3)3I,
Molecular weight 1120.04, belongs to monoclinic system, and space group is C2/m, and cell parameter is β=114.533 (8) °,Z=4;This crystal is just
Biaxial crystal, nz-ny>ny-nx, through wide ranges (300-3000nm), and birefringence is big (0.084-0.374), is one
Plant the birefringent material that can be used for ultraviolet.
Another object of the present invention is to provide described a kind of caesium lead carbon oxygen iodine birefringece crystal Cs3Pb2(CO3)3The growth side of I
Method.
It is yet a further object of the present invention to provide a kind of caesium lead carbon oxygen iodine birefringece crystal Cs3Pb2(CO3)3The purposes of I.
A kind of caesium lead carbon oxygen iodine birefringece crystal of the present invention, this crystal-chemical formula is Cs3Pb2(CO3)3I, molecular weight
1120.04, belong to monoclinic system, space group is C2/m, and cell parameter is β=114.533 (8) °,Z=4.
Described caesium lead carbon oxygen iodine birefringece crystal, it is characterised in that this crystal is positive biaxial crystal, nz-ny>ny-nx。
The preparation method of described caesium lead carbon oxygen iodine birefringece crystal, uses hydro-thermal method to prepare crystal, and following step is pressed in concrete operations
Suddenly carry out:
A, will to contain Cs compound be Cs2CO3Or CsF joins the politef of the autoclave that volume is 23-100mL
In liner, add PbO and HI or PbI2, add deionized water 2-50mL so that it is be sufficiently mixed uniformly, mixed
Solution, wherein Cs+And Pb2+Mol ratio be 1-8:1, Cs+And I-Mol ratio be 1-8:2, or add mass fraction be 45%
HI;
B, by the mixed solution of step a add mineralizer boron acid plus carbonate be lithium carbonate, sodium carbonate, potassium carbonate or carbonic acid
Rubidium, the addition of its mesoboric acid and carbonate is 4 times and 1 times of lead iodide in step a, the addition of boron acid plus carbonate
For in step a 4 times and 1 times of lead oxide;
C, the polytetrafluoroethyllining lining lid that will be equipped with mixed solution in step b screw, and load the autoclave of respective volume
In, reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to the heating rate of temperature 20-60 DEG C/h
120-200 DEG C, constant temperature 1-15 days, then with the rate of temperature fall of temperature 4-50 DEG C/h or naturally cool to room temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Solution is placed on clean free of contamination autoclave by step c.
Described caesium lead carbon oxygen iodine birefringece crystal purposes in preparing polarization beam splitter prism.
The purposes of described caesium lead carbon oxygen iodine birefringece crystal, it is characterised in that described polarization beam splitter prism be Glan type prism,
Wollaston prism, Rochon prism or light beam separation polariser.
A kind of caesium lead carbon oxygen iodine birefringece crystal of the present invention, the molecular formula of this crystal is Cs3Pb2(CO3)3I, molecular weight
1120.04, belong to monoclinic system, space group is C2/m, and cell parameter is β=114.533 (8) °,Z=4.There is wider transparency range
(300-3000nm), birefringence is between 0.084 (3000nm)-0.374 (340nm).The preparation of this crystal is simple, growth
Cycle is short, and the initiation material toxicity used is low little to human body murder by poisoning.
Method used by the present invention is hydro-thermal method, will pass through after initiation material proportionally mixes in certain temperature range
High-temperature high-voltage reaction in the reactor sealed, i.e. can get transparent Cs by the method for programmed cooling or constant temperature3Pb2(CO3)3I
Optical crystal.
The following is several and typically can obtain Cs3Pb2(CO3)3The chemical equation of I:
(1)Cs2CO3+PbI2+H3BO3+Rb2CO3+H2O→Cs3Pb2(CO3)3I+Rb++H3BO3+H2O
(2)Cs2CO3+PbI2+H3BO3+K2CO3+H2O→Cs3Pb2(CO3)3I+K++H3BO3+H2O
(3)Cs2CO3+PbI2+H3BO3+Na2CO3+H2O→Cs3Pb2(CO3)3I+Na++H3BO3+H2O
(4)Cs2CO3+PbO+HI+H3BO3+Li2CO3+H2O→Cs3Pb2(CO3)3I+Li++H3BO3+H2O
(5)Cs2CO3+PbO+HI+H3BO3+Rb2CO3+H2O→Cs3Pb2(CO3)3I+Rb++H3BO3+H2O
(6)CsF+PbI2+H3BO3+Rb2CO3+H2O→Cs3Pb2(CO3)3I+Rb++H3BO3+F-+H2O
(7)CsF+PbI2+H3BO3+K2CO3+H2O→Cs3Pb2(CO3)3I+K++H3BO3+F-+H2O
Accompanying drawing explanation
Fig. 1 is the structure chart of the present invention;
Fig. 2 is the XRD figure of the present invention;
Fig. 3 is crystal pattern of the present invention;
Fig. 4 is birefringent wedge crystal polarization beam apparatus schematic diagram of the present invention;
Fig. 5 is optoisolator schematic diagram of the present invention;
Fig. 6 is pattern displacement device schematic diagram of the present invention, and wherein 1 is incident illumination, and 2 is o light, and 3 is e light, and 4 is optical axis,
5 is Cs3Pb2(CO3)3I crystal, 6 printing opacity directions, 7 axial planes.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail:
Embodiment 1:
With chemical equation Cs2CO3+PbI2+H3BO3+Rb2CO3+H2O→Cs3Pb2(CO3)3I+Rb++H3BO3+H2O
Preparing crystal, concrete operation step is as follows:
A, in molar ratio Cs2CO3∶PbI2=4:1, by Cs2CO3Join the polytetrafluoro of the autoclave that volume is 23mL
In ethylene liner, add PbI2, add deionized water 2mL so that it is be sufficiently mixed uniformly, obtain mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And Rb2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition be PbI in step a24 times, Rb2CO3Addition be PbI in step a21 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with step b mixed solution screw, and load in the autoclave of respective volume,
Reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 150 DEG C with the heating rate of 20 DEG C/h of temperature,
Constant temperature 5 days, then it is down to room temperature with the rate of temperature fall of 10 DEG C/h of temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 2:
With chemical equation Cs2CO3+PbI2+H3BO3+K2CO3+H2O→Cs3Pb2(CO3)3I+K++H3BO3+H2O
Preparing crystal, concrete operation step is as follows:
A, in molar ratio Cs2CO3∶PbI2=1:1, by Cs2CO3Join the polytetrafluoro of the autoclave that volume is 23mL
In ethylene liner, add PbI2, add deionized water 10mL so that it is be sufficiently mixed uniformly, obtain mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And K2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition be PbI in step a24 times, K2CO3Addition be PbI in step a21 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with step b mixed solution screw, and load in the autoclave of respective volume,
Reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 200 DEG C with the heating rate of 30 DEG C/h of temperature,
Constant temperature 3 days, naturally cools to room temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 3:
With chemical equation Cs2CO3+PbI2+H3BO3+Na2CO3+H2O→Cs3Pb2(CO3)3I+Na++H3BO3+H2O system
Standby crystal, concrete operation step is as follows:
A, in molar ratio Cs2CO3∶PbI2=3:1, by Cs2CO3Join the polytetrafluoro of the autoclave that volume is 50mL
In ethylene liner, add PbI2, add deionized water 20mL so that it is be sufficiently mixed uniformly, obtain mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And Na2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition be PbI in step a24 times, Na2CO3Addition be PbI in step a21 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with mixed solution in step b screw, and load the autoclave of respective volume
In, reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 180 DEG C with the heating rate of temperature 50 C/h,
Constant temperature 10 days, then it is down to room temperature with the rate of temperature fall of 25 DEG C/h of temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 4:
With chemical equation Cs2CO3+PbO+HI+H3BO3+Li2CO3+H2O→Cs3Pb2(CO3)3I+Li++H3BO3+H2O
Preparing crystal, concrete operation step is as follows:
A, in molar ratio Cs2CO3: PbO=2.5:1, by Cs2CO3Join poly-the four of the autoclave that volume is 75mL
In fluorothene liner, add deionized water 25mL, add the hydroiodic acid that 1mL mass fraction is 45% so that it is the most mixed
Close uniformly, obtain mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And Li2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition is PbO in step a 4 times, Li2CO3Addition is PbO in step a 1 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with step b mixed solution screw, and load in the autoclave of respective volume,
Reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 130 DEG C with the heating rate of 20 DEG C/h of temperature,
Constant temperature 15 days, then it is down to room temperature with the rate of temperature fall of 6 DEG C/h of temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 5:
With chemical equation Cs2CO3+PbO+HI+H3BO3+Rb2CO3+H2O→Cs3Pb2(CO3)3I+Rb++H3BO3+H2O
Preparing crystal, concrete operation step is as follows:
A, in molar ratio Cs2CO3: PbO=3:1, by Cs2CO3Join the polytetrafluoro of the autoclave that volume is 75mL
In ethylene liner, add deionized water 30mL, add the hydroiodic acid that mass fraction is 45% of 0.5mL so that it is fully
Mix homogeneously, obtains mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And Rb2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition is PbO in step a 4 times, Rb2CO3Addition is PbO in step a 1 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with step b mixed solution screw, and load in the autoclave of respective volume,
Reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 200 DEG C with the heating rate of 30 DEG C/h of temperature,
Constant temperature 3 days, then it is down to room temperature with the rate of temperature fall of 15 DEG C/h of temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 6:
With chemical equation CsF+PbI2+H3BO3+Rb2CO3+H2O→Cs3Pb2(CO3)3I+Rb++H3BO3+F-+
H2O prepares crystal, and concrete operation step is as follows:
A, in molar ratio 5CsF: PbI2=4:1, joins the polytetrafluoroethyl-ne of the autoclave that volume is 50mL by CsF
In alkene liner, add PbI2, add deionized water 25mL so that it is be sufficiently mixed uniformly, obtain mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And Rb2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition be PbI in step a24 times, Rb2CO3Addition be PbI in step a21 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with step b mixed solution screw, and load in the autoclave of respective volume,
Reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 180 DEG C with the heating rate of 20 DEG C/h of temperature,
Constant temperature 5 days, naturally cools to room temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 7:
With chemical equation CsF+PbI2+H3BO3+K2CO3+H2O→Cs3Pb2(CO3)3I+K++H3BO3+F-+H2O
Preparing crystal, concrete operation step is as follows:
A, in molar ratio 7CsF: PbI2=4:1, joins the polytetrafluoroethyl-ne of the autoclave that volume is 100mL by CsF
In alkene liner, add PbI2, add deionized water 50mL so that it is be sufficiently mixed uniformly, obtain mixed solution;
B, will in the mixed solution of step a add mineralizer H3BO3And K2CO3, stir, obtain mixed liquor, wherein press
Mol ratio H3BO3Addition be PbI in step a24 times, K2CO3Addition be PbI in step a21 times;
C, the polytetrafluoroethyllining lining lid that will be equipped with step b mixed solution screw, and load in the autoclave of respective volume,
Reactor piston is screwed;
D, the autoclave in step c is placed in calorstat, rises to 200 DEG C with the heating rate of temperature 50 C/h,
Constant temperature 5 days, then it is down to room temperature with the rate of temperature fall of 20 DEG C/h of temperature;
E, open autoclave, the solution containing crystal filtered, through X-ray single crystal diffractometer resolve determine obtain transparent
Cs3Pb2(CO3)3I birefringece crystal.
Embodiment 8
By arbitrary for embodiment 1-7 gained Cs3Pb2(CO3)3I crystal, be used for preparing birefringent wedge crystal polarization beam apparatus (as
Shown in Fig. 4), the birefringece crystal of a wedge shape, the orientation of optical axis as shown in Figure 4, through crystal after a branch of natural light incidence
Being segmented into two bunch polarized light, birefringence is the biggest, and two-beam can be separate the most remote, it is simple to the separation of light beam.
Embodiment 9
By arbitrary for embodiment 1-7 gained Cs3Pb2(CO3)3I crystal, is used for preparing optoisolator, by an incident beam
Plane of polarization rotate the Faraday optical rotator of 45 ° be placed in a pair each other 45 ° intersect between the birefringece crystal deflector placed,
Then may make up an optoisolator, it only allow the light beam of forward-propagating by this system, and by the beam blockage of back propagation,
Fig. 5 a represents that incident light beam can pass through, and Fig. 5 b represents that reflection light is prevented from.
Embodiment 10
By the arbitrary Cs of embodiment 1-7 gained3Pb2(CO3)3I crystal, is used for preparing pattern displacement device.Process one two-fold
Penetrate crystal, make its axial plane and rib θ at an angle (as shown in Figure 6 a), when after natural light vertical incidence, be segmented into two
The bundle mutually perpendicular line polarized light of direction of vibration (as shown in Figure 6 b), is o light and e light respectively, and two-fold rate is the biggest, two bundles
Light can be separate the most remote, it is simple to the separation of light beam.
Claims (6)
1. a caesium lead carbon oxygen iodine birefringece crystal, this crystal-chemical formula is Cs3Pb2(CO3)3I, molecular weight 1120.04, belong to monoclinic system, space group is C2/m, and cell parameter is a=24.549 (3), b=5.4233 (8), c=12.8598 (16), β=114.533 (8) °, V=1557.5 (4)3, Z=4.
2. a caesium lead carbon oxygen iodine birefringece crystal as claimed in claim 1, it is characterised in that this crystal is positive biaxial crystal, nz-ny>ny-nx。
3. the preparation method of a caesium lead carbon oxygen iodine birefringece crystal as claimed in claim 1, it is characterised in that using hydro-thermal method to prepare crystal, concrete operations follow these steps to carry out:
A, will to contain Cs compound be Cs2CO3Or CsF joins in the polytetrafluoroethyllining lining of the autoclave that volume is 23-100mL, add PbO and HI or PbI2, add deionized water 2-50 mL so that it is be sufficiently mixed uniformly, obtain mixed solution, wherein Cs+And Pb2+Mol ratio be 1-8:1, Cs+And I-Mol ratio be 1-8:2, or add mass fraction be the HI of 45%;
B, by the mixed solution of step a add mineralizer boron acid plus carbonate be lithium carbonate, sodium carbonate, potassium carbonate or rubidium carbonate, the addition of its mesoboric acid and carbonate is 4 times and 1 times of lead iodide in step a, and the addition of boron acid plus carbonate is 4 times and 1 times of lead oxide in step a;
C, the polytetrafluoroethyllining lining lid that will be equipped with mixed solution in step b screw, and load in the autoclave of respective volume, are screwed by reactor piston;
D, the autoclave in step c is placed in calorstat, rises to 120-200 DEG C with the heating rate of temperature 20-60 DEG C/h, constant temperature 1-15 days, then with the rate of temperature fall of temperature 4-50 DEG C/h or naturally cool to room temperature;
E, open autoclave, the solution containing crystal is filtered, resolve through X-ray single crystal diffractometer and determine and obtain transparent Cs3Pb2(CO3)3I birefringece crystal.
Method the most according to claim 3, it is characterised in that solution is placed on clean free of contamination autoclave by step c.
5. a caesium lead carbon oxygen iodine birefringece crystal as claimed in claim 1 purposes in preparing polarization beam splitter prism.
The purposes of caesium lead carbon oxygen iodine birefringece crystal the most according to claim 5, it is characterised in that described polarization beam splitter prism is Glan type prism, wollaston prism, Rochon prism or light beam separation polariser.
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