CN106757344B - Two kinds of inorganic fluoriodate crystal and its preparation method and application - Google Patents
Two kinds of inorganic fluoriodate crystal and its preparation method and application Download PDFInfo
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Abstract
The invention discloses two kinds of Inorganic crystal compounds and preparation method thereof and as the application of non-linear optical crystal material, molecular formula RbBi2(IO3)2F5And CsBi2(IO3)2F5, they belong to monoclinic system P21Space group, wherein RbBi2(IO3)2F5Cell parameter beα=90 °, β=100.263 (2) °, γ=90 °, CsBi2(IO3)2F5Cell parameter beα=90 °, β=100.509 (6) °, γ=90 °.Both Inorganic crystal compounds can be synthesized at a lower temperature by hydro-thermal method, and synthetic method is simple, and crystal growth cycles are short；Its crystal has very strong second order nonlinear optical effect, and can be realized phase matched；There is wider transparency range in ultraviolet visible light region and infrared light district；With biggish band gap and higher thermal stability；They can be used as non-linear optical crystal material and are widely used in the fields such as optics.
Description
Technical field
The present invention relates to two kinds of inorganic fluoriodate non-linear optical crystal materials and its preparation method and application, belong to nothing
Chemical machine field, also belongs to materials science field and optical field.
Background technique
Second-order non-linear optical crystal material builds on the new function material on laser technology application as one kind,
The nonlinear optical effects such as frequency multiplication and frequency, difference frequency and optically erasing are in information storage, laser technology, atmospheric monitoring, communication
Value is had important application with various fields such as defense military.With regard to realizing the second-order non-linear optical crystal material of business application
For, inorganic nonlinear optical crystal material occupies leading position therein.Application according to crystal in different transparency ranges, nothing
Machine second-order non-linear optical crystal material can be divided into ultraviolet region non-linear optical crystal material, visible region non-linear optical crystal
Body material and infrared light district non-linear optical crystal material.And so far, ultraviolet region possessed beta-barium metaborate (BBO),
The inorganic nonlinear optical crystal that three lithium borates (LBO), fluoboric acid beryllium potassium (KBBF), potassium dihydrogen phosphate (KDP) etc. are had excellent performance
Material；The potassium titanium oxide phosphate (KTP) of visible region, lithium niobate (LN) etc. also can satisfy functional need.Infrared light district is corresponding
Non-linear optical crystal material such as AgGaS is commercialized2、AgGaSe2And ZnGeP2Although equal crystal have very big second nonlinear
Optical coefficient has very wide transmission range in infrared light district, but synthesis condition is harsh, it is not easy to the high big list of growing optics quality
Crystalline substance, especially laser damage threshold are lower, thus are unable to satisfy second-order non-linear optical crystal material in high intensity laser beam field
Practical demand.And infrared nonlinear optical crystal material has important answer in fields such as national economy, defense military
With value, such as realizes continuously adjustable molecular spectrum, widen the range of laser radiation wavelength, open up new laser light source etc..Cause
This has both infrared nothing in larger nonlinear optical effect and wider infrared light transmission range with high laser damage threshold again
Machine non-linear optical crystal material has particularly significant and wide application prospect in non-linear optical field.
Summary of the invention
The present invention is intended to provide outstanding Inorganic crystal compound of two kinds of comprehensive performances and preparation method thereof and described inorganic
Application of the crystalline compounds as second-order non-linear optical crystal material.
The present invention is achieved through the following technical solutions：
A kind of inorganic fluoriodate crystal, chemical formula RbBi2(IO3)2F5Belong to monoclinic system, crystal space group
For P21, cell parameter isα=90 °, β=100.263
(2) °, γ=90 °.
It is a kind of to prepare RbBi2(IO3)2F5The method of crystal, includes the following steps：It is 4 by molar ratio：1：4 RbF, Bi2O3
And H5IO6It is added in hydrothermal reaction kettle, adds hydrofluoric acid aqueous solution, stir evenly, wherein the molal quantity of HF is five times of RbF
More than；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, isothermal reaction 4 days or more, be slowly dropped to room temperature later；Instead
After answering, product is filtered, uses deionized water and ethanol washing successively then to get RbBi is arrived2(IO3)2F5Crystal.
The HF solution and water by volume 1 that the hydrofluoric acid aqueous solution is 40% by mass fraction：1~2 mixes.
The concentration of RbF is 0.667~1mol/L after addition hydrofluoric acid aqueous solution.
A kind of inorganic fluoriodate crystal, chemical formula CsBi2(IO3)2F5, belong to monoclinic system, crystal space group
For P21, cell parameter isα=90 °, β=100.509 (6) °,
γ=90 °.
It is a kind of to prepare above-mentioned CsBi2(IO3)2F5The method of crystal, includes the following steps：It is 4 by molar ratio：4：1：4
CsIO4：CsF,Bi2O3And H5IO6It is added in hydrothermal reaction kettle, adds hydrofluoric acid aqueous solution, stir evenly, wherein mole of HF
Number is five times of CsF or more；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, isothermal reaction 4 days or more, Zhi Houhuan
Slowly it is down to room temperature；After reaction, product is filtered, uses deionized water and ethanol washing successively then to get CsBi is arrived2
(IO3)2F5Crystal.
The HF solution and water by volume 1 that the hydrofluoric acid aqueous solution is 40% by mass fraction：1~2 mixes.
The concentration of CsF is 0.667~1mol/L after addition hydrofluoric acid aqueous solution.
Above-mentioned inorganic fluoriodate crystal as non-linear optical crystal material optical field application.
The powder SHG effect of above two inorganic fluoriodate crystal：RbBi2(IO3)2F5For KDP (potassium dihydrogen phosphate)
9.5 times；CsBi2(IO3)2F5It is 7.5 times of KDP.
The transparency range and band gap of above two inorganic fluoriodate crystal：RbBi2(IO3)2F5It is 0.33-12.8 microns,
3.78eV；CsBi2(IO3)2F5It is 0.32-12.8 microns, 3.84eV.
The thermal weight loss temperature of above two inorganic fluoriodate crystal：RbBi2(IO3)2F5It is 240 DEG C, CsBi2(IO3)2F5
It is 270 DEG C.
The cooling method is to be cooled down with the rate of 1~8 DEG C/h.
The reaction kettle, liner are polytetrafluoroethylene (PTFE) material.
Inorganic crystal compound of the present invention has the following advantages and beneficial effect：
1. two kinds of inorganic fluoriodate crystal of the present invention have biggish frequency-doubled effect (SHG), Kurtz powder frequency doubling
Test result shows RbBi2(IO3)2F5Powder SHG effect be 9.5 times of KDP (potassium dihydrogen phosphate)；CsBi2(IO3)2F5For
7.5 times of KDP；
2. two kinds of inorganic fluoriodate crystal of the present invention have wider through model in visible region and mid-infrared light area
It encloses, RbBi2(IO3)2F5Preferable translucency is all had in 0.33-12.8 micron wavelength range；CsBi2(IO3)2F5In 0.32-
There is preferable translucency in 12.8 micron wavelength ranges；
3. two kinds of inorganic fluoriodate crystal of the present invention do not deliquesce air-stable without the crystallization water, and thermostabilization
Property is preferable；
4. two kinds of inorganic fluoriodate crystal of the present invention utilize Hydrothermal preparation method, it is easy to operate, raw material availability is high,
Experiment condition is mild, product purity is high；
5. inorganic fluoriodate crystal of the present invention can be realized phase as second-order non-linear optical crystal material
Match.
Detailed description of the invention
Fig. 1 is RbBi of the present invention2(IO3)2F5Crystal structure figure；
Fig. 2 is RbBi of the present invention2(IO3)2F5Ab plane mesh structure figure in crystal structure；
Fig. 3 is RbBi of the present invention2(IO3)2F5Anionic group structure chart in crystal structure；
Fig. 4 is CsBi of the present invention2(IO3)2F5Crystal structure figure；
Fig. 5 is CsBi of the present invention2(IO3)2F5Anionic group structure chart in crystal structure；
Fig. 6 is RbBi of the present invention2(IO3)2F5Solid powder UV-Vis-NIR absorb spectrogram；
Fig. 7 is CsBi of the present invention2(IO3)2F5Solid powder UV-Vis-NIR absorb spectrogram；
Fig. 8 is RbBi of the present invention2(IO3)2F5ATR-FTIR spectrogram；
Fig. 9 is CsBi of the present invention2(IO3)2F5ATR-FTIR spectrogram；
Figure 10 is RbBi of the present invention2(IO3)2F5Thermal weight loss spectrogram；
Figure 11 is CsBi of the present invention2(IO3)2F5Thermal weight loss spectrogram；
Figure 12 is the frequency-doubled effect intensity and particle size graph of relation of two kinds of inorganic fluoriodate crystal of the invention.
Specific embodiment
Combined with specific embodiments below and attached drawing is described in further detail technical solution of the present invention, but the present invention
Embodiment it is without being limited thereto.
Embodiment 1
The hydrofluoric acid and distilled water volume ratio for preparing mass fraction 40% in advance are 1：2 mixed solution, by 2mmol
RbF、0.5mmol Bi2O3With 2mmol H5IO6It is added in the hydrothermal reaction kettle of 23mL, adds the hydrofluoric acid dilutions of 3mL,
Make the ultimate density 0.667mol/L of RbF；Closed hydrothermal reaction kettle is put into Muffle furnace, is heated to 230 DEG C through 3h, perseverance
Temperature reaction is cooled to room temperature again with the rate of temperature fall of 8 DEG C/h in 4 days；After reaction, product is filtered and uses deionized water and second
Alcohol washs to arrive inorganic fluoriodate crystal RbBi2(IO3)2F5。
Embodiment 2
The hydrofluoric acid and distilled water volume ratio for preparing mass fraction 40% in advance are 1：1 mixed solution, by 2mmol
RbF、0.5mmol Bi2O3With 2mmol H5IO6It is added to the hydrothermal reaction kettle of 23mL, adds the hydrofluoric acid dilutions of 2mL
Make the ultimate density 1mol/L of RbF；Closed hydrothermal reaction kettle is put into Muffle furnace, is heated to 230 DEG C through 3h, constant temperature is anti-
It answers 4 days and room temperature is cooled to the rate of temperature fall of 8 DEG C/h again；After reaction, product is filtered and is washed with deionized water and ethyl alcohol
It washs to get inorganic fluoriodate crystal RbBi is arrived2(IO3)2F5。
Embodiment 3
The hydrofluoric acid and distilled water volume ratio for preparing mass fraction 40% in advance are 1:1 mixed solution, by 10mmol
RbF、2.5mmol Bi2O3With 10mmol H5IO6It is added to the hydrothermal reaction kettle of 100mL, the hydrofluoric acid for adding 10mL is dilute
Releasing liquid makes the ultimate density 1mol/L of RbF；Closed hydrothermal reaction kettle is put into Muffle furnace, is heated to 210 DEG C through 3h, perseverance
Temperature reaction is cooled to room temperature again with the rate of temperature fall of 1 DEG C/h in 4 days；After reaction, product is filtered and uses deionized water and second
Alcohol washs to arrive inorganic fluoriodate crystal RbBi2(IO3)2F5。
Embodiment 4
The hydrofluoric acid and distilled water volume ratio for preparing mass fraction 40% in advance are 1:1 mixed solution, by 2mmol
CsF、2mmol CsIO4、0.5mmol Bi2O3And 2mmol H5IO6It is added to the hydrothermal reaction kettle of 23mL, adds 2mL's
Hydrofluoric acid dilutions make the ultimate density 1mol/L of CsF；Closed hydrothermal reaction kettle is put into Muffle furnace, is heated to through 3h
210 DEG C, room temperature is cooled to the rate of temperature fall of 8 DEG C/h again within isothermal reaction 4 days；After reaction, product is filtered and spend from
Sub- water and ethanol washing are to get arriving inorganic fluoriodate crystal CsBi2(IO3)2F5。
Embodiment 5
The hydrofluoric acid and distilled water volume ratio for preparing mass fraction 40% in advance are 1:2 mixed solution, by 2mmol
CsF、2mmol CsIO4、0.5mmol Bi2O3And 2mmol H5IO6It is added to the hydrothermal reaction kettle of 23mL, adds 3mL's
Hydrofluoric acid dilutions make the ultimate density 0.667mol/L of CsF；Closed hydrothermal reaction kettle is put into Muffle furnace, through 3h plus
Heat is cooled to room temperature again to 230 DEG C with the rate of temperature fall of 8 DEG C/h in isothermal reaction 4 days；After reaction, product is filtered and is used in combination
Deionized water and ethanol washing are to get arriving inorganic fluoriodate crystal CsBi2(IO3)2F5。
Embodiment 6
The hydrofluoric acid and distilled water volume ratio for preparing mass fraction 40% in advance are 1:1 mixed solution, by 10mmol
CsF、10mmol CsIO4、2.5mmol Bi2O3And 10mmol H5IO6It is added to the hydrothermal reaction kettle of 100mL, adds
The hydrofluoric acid dilutions of 10mL make the ultimate density 1mol/L of CsF；Closed hydrothermal reaction kettle is put into Muffle furnace, through 3h
210 DEG C are heated to, room temperature is cooled to the rate of temperature fall of 1 DEG C/h again within isothermal reaction 4 days；After reaction, product is filtered simultaneously
With deionized water and ethanol washing to get arrive inorganic fluoriodate crystal CsBi2(IO3)2F5。
Frequency doubling property test：
Frequency-doubled effect and the phase matched test of inorganic fluoriodate crystal prepared by the present invention pass through Kurtz powder times
Frequency test method obtains.Concrete operation step is as follows：Resulting inorganic fluoriodate crystal is ground and is sieved into respectively first
Different grain size range powder (20~40,40~60,60~80,80~100,100~125,125~150,150~200,
200~300,300~400 microns), being then charged into two sides has in the sample cell of windowpane, and sample cell is placed in Nd later:YAG
Pulse laser is as in the laser optical path of light source, the fundamental frequency light irradiating sample pond for being 1064 nanometers using wavelength, frequency-doubled signal
It is shown on oscillograph through photomultiplier tube.Frequency-doubled effect intensity maps to partial size, if intensity first becomes larger with the increase of partial size
Then tend to platform, then illustrates phase matched；If intensity then reduces as the increase of partial size first becomes larger, do not illustrate phase not
Match.Using the KDP monocrystal of same particle size as standard specimen, the sample and KDP of the partial size after taking frequency-doubled effect to reach platform are surveyed
The frequency-doubled signal intensity obtained compares to obtain the relative size of frequency-doubled effect.
Crystal structure test：
The structure of prepared inorganic fluoriodate crystal is measured by Advances in crystal X-ray diffraction structural analysis.Both nothings
Machine fluoriodate crystal belongs to monoclinic system P21Space group, RbBi2(IO3)2F5Cell parameter be： α=90 °, β=100.263 (2) °, γ=90 °.CsBi2(IO3)2F5Structure cell ginseng
Number is：α=90 °, β=100.509 (6) °, γ=90 °.
RbBi2(IO3)2F5Crystal structure in, in single structure cell contain a Rb atom, two kinds of Bi atoms, five F atoms, two kinds
I atom and 6 O atoms.Fig. 1 is schematic diagram of the crystal structure in ac plane, in its crystal structure, Bi atom, F atom, I
Atom and O atom, which interconnect, constitutes two-dimension plane structure, and Rb atom is filled between planar structure, together constitutes RbBi2
(IO3)2F5Three-D space structure.Fig. 2 is the planar structure schematic diagram being made of in structure Bi, F, I, O, and Bi atom and Bi are former
Son is connect with I atom by sharing O atom by sharing F atom connection, Bi atom, constitutes a plane reticular in ab plane
Structure.Fig. 3 is the schematic diagram of anionic group in the structure, centered on heavy atom Bi and I, one of Bi atom and five
F atom bonding constitutes the BiF with a pair of of lone pair electrons5Group, Bi-F key bond distance areAnother Bi is former
Son and four F atoms and two kinds of O atom keys even constitute BiO2F4Distortion structure, Bi-O key bond distance areBi-F key
Bond distance isTwo kinds of I atoms form the IO for having lone pair electrons with three O atom bondings respectively3Structure, I-O key
Bond distance isIn the crystal structure of the compound, the BiF of lone pair electrons5Group, BiO2F4Distortion structure
With the IO for having lone pair electrons3Three kinds of anionic groups of structure all have biggish structural aberration, and IO3Structure is in b axis direction
On the superposition for being arranged with a dipole moment；BiF5Group shows in the distribution of b axis direction, two kinds shorter of Bi-F key and two kinds
Longer Bi-F key is distributed in the two sides of Bi atom, therefore BiF respectively5Group also has microcosmic dipole moment in b axis direction；Together
Reason, BiO2F4The key distribution of structure also shows it has microcosmic dipole moment in b axis direction.And BiF5Group, BiO2F4Structure
And IO3The arrangement mode of structure is overlapped mutually their microcosmic dipole moment, directly result in the structure in b axis direction compared with
Big dipole moment, to make RbBi2(IO3)2F5Crystal is macroscopically showing very strong second order nonlinear optical effect.
CsBi2(IO3)2F5Crystal structure and RbBi2(IO3)2F5Crystal structure it is similar, as shown in figure 4, and former by Bi atom, F
Son, I atom and O atom, which interconnect, constitutes two-dimension plane structure, and Cs atom, which is filled between planar structure, constitutes three-dimensional space
Structure.Fig. 5 is CsBi2(IO3)2F5Crystal structure in anionic group schematic diagram, with RbBi2(IO3)2F5Crystal structure class
Seemingly, the BiF in structure5Group, BiO2F4Structure and IO3The arrangement mode of structure is but also they are microcosmic in b axis direction
Dipole moment is overlapped mutually, to make CsBi2(IO3)2F5Crystal also shows stronger second order nonlinear optical effect.
The performance test results：
RbBi2(IO3)2F5Crystal and CsBi2(IO3)2F5The UV-Vis-NIR abosrption spectrogram of crystal is respectively such as Fig. 6 and Fig. 7
Shown, two kinds of inorganic fluoriodate crystal all have biggish optical band gap, RbBi2(IO3)2F5About 3.78eV, CsBi2
(IO3)2F5About 3.84eV；The ATR-FTIR spectrogram of two kinds of compounds is respectively such as Fig. 8 and as shown in figure 9, their infrared absorption
Side is up to 12.8 microns；Thermal weight loss spectrogram distinguishes as shown in Figure 10 and Figure 11, RbBi2(IO3)2F5Crystal is opened at 240 DEG C
Beginning thermal weight loss, CsBi2(IO3)2F5Crystal all has excellent thermostabilization in 270 DEG C of beginning thermal weight losses, two kinds of compound crystals
Property；The relation curve of their frequency-doubled effect (SHG) intensity and sample particle diameter is as shown in figure 12, both inorganic fluoriodates are brilliant
Body all has stronger second order nonlinear optical effect and can be realized phase matched, wherein RbBi2(IO3)2F5The frequency multiplication of crystal
Effect is about 9.5 times of KDP, CsBi2(IO3)2F5The frequency-doubled effect of crystal is about 7.5 times of KDP.
In short, both Inorganic crystal compounds all have excellent comprehensive performance, second nonlinear optic crystalline substance can be used as
Body material is applied.
Embodiments of the present invention are explained in detail above in conjunction with attached drawing, but the present invention is not limited to the implementations
Mode, can within the knowledge of one of ordinary skill in the art and without departing from the purpose of the present invention
It makes a variety of changes.
Claims (9)
1. a kind of inorganic fluoriodate crystal, it is characterised in that：Its chemical formula is RbBi2(IO3)2F5, belong to monoclinic system, it is brilliant
Body space group is P21, cell parameter isα=90 °, β=
100.263 (2) °, γ=90 °.
2. a kind of method for preparing inorganic fluoriodate crystal described in claim 1, which is characterized in that include the following steps：
It is 4 by molar ratio：1：4 RbF, Bi2O3And H5IO6It is added in hydrothermal reaction kettle, adds hydrofluoric acid aqueous solution, stir evenly,
Wherein, the molal quantity of HF is five times of RbF or more；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, isothermal reaction 4
More than it, it is slowly dropped to room temperature later；After reaction, product is filtered, then successively uses deionized water and ethanol washing, i.e.,
Obtain RbBi2(IO3)2F5Crystal.
3. according to the method described in claim 2, it is characterized in that：The HF that the hydrofluoric acid aqueous solution is 40% by mass fraction
Solution and water by volume 1：1~2 mixes.
4. according to the method in claim 2 or 3, it is characterised in that：The concentration of RbF is after addition hydrofluoric acid aqueous solution
0.667~1mol/L.
5. a kind of inorganic fluoriodate crystal, it is characterised in that：Its chemical formula is CsBi2(IO3)2F5, belong to monoclinic system, it is brilliant
Body space group is P21, cell parameter isα=90 °, β=
100.509 (6) °, γ=90 °.
6. a kind of method for preparing inorganic fluoriodate crystal described in claim 5, which is characterized in that include the following steps：
It is 4 by molar ratio：4: 1: 4 CsIO4：CsF,Bi2O3And H5IO6It is added in hydrothermal reaction kettle, adds hydrofluoric acid aqueous solution, stir
It mixes uniformly, wherein the molal quantity of HF is five times of CsF or more；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, constant temperature
Reaction 4 days or more, it is slowly dropped to room temperature later；After reaction, product is filtered, is then successively washed with deionized water and ethyl alcohol
It washs to get CsBi is arrived2(IO3)2F5Crystal.
7. according to the method described in claim 6, it is characterized in that：The HF that the hydrofluoric acid aqueous solution is 40% by mass fraction
Solution and water by volume 1：1~2 mixes.
8. method according to claim 6 or 7, it is characterised in that：The concentration of CsF is after addition hydrofluoric acid aqueous solution
0.667~1mol/L.
9. the answering in optical field as non-linear optical crystal material of inorganic fluoriodate crystal described in claim 1 or 5
With.
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