CN106757344A - 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
- Publication number
- CN106757344A CN106757344A CN201710047966.4A CN201710047966A CN106757344A CN 106757344 A CN106757344 A CN 106757344A CN 201710047966 A CN201710047966 A CN 201710047966A CN 106757344 A CN106757344 A CN 106757344A
- Authority
- CN
- China
- Prior art keywords
- crystal
- inorganic
- rbbi
- hydrofluoric acid
- csbi
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses two kinds of Inorganic crystal compounds and preparation method thereof and as the application of non-linear optical crystal material, its molecular formula is RbBi2(IO3)2F5And CsBi2(IO3)2F5, they belong to monoclinic systemP21Space group, wherein RbBi2(IO3)2F5Cell parameter be a=5.7357 (9), b=5.9095 (10), c=15.177 (3), α=90 °, β=100.263 (2) °, γ=90 °, CsBi2(IO3)2F5Cell parameter be a=5.750 (2), b=5.924 (2), c=15.640 (7), α=90 °, β=100.509 (6) °, γ=90 °.Both Inorganic crystal compounds can at a lower temperature be synthesized 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 realize phase matched；There is transparency range wider in ultraviolet visible light region and infrared light district；With larger band gap and heat endurance higher；They can be widely used in the fields such as optics as non-linear optical crystal material.
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, falls within material science and optical field.
Background technology
Second-order non-linear optical crystal material builds on the new function material on laser technology application as a class, its
The nonlinear optical effect such as frequency multiplication and frequency, difference frequency and optically erasing is in information Store, laser technology, atmospheric monitoring, communication
There is important application value with the various fields such as national defense and military.Just realize the second-order non-linear optical crystal material of business application
For, inorganic nonlinear optical crystal material occupies leading position therein.According to crystal different transparency ranges application, 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 of the excellent performances such as three lithium borates (LBO), fluoboric acid beryllium potassium (KBBF), potassium dihydrogen phosphate (KDP)
Material；Potassium titanium oxide phosphate (KTP), lithium niobate (LN) of visible region etc. can also meet functional need.Infrared light district is corresponding
Commercialization non-linear optical crystal material such as AgGaS2、AgGaSe2And ZnGeP2Although Deng crystal with very big second nonlinear
Optical coefficient, has transmission scope very wide in infrared light district, but synthesis condition is harsh, it is not easy to growing optics quality big list high
Crystalline substance, especially laser damage threshold is relatively low, thus cannot meet second-order non-linear optical crystal material in high intensity laser beam field
Practical demand.And infrared nonlinear optical crystal material has important answering in fields such as national economy, national defense and military
With value, the molecular spectrum of continuously adjustabe is such as realized, widen the scope of laser radiation wavelength, open up new LASER Light Source etc..Cause
This has high laser damage threshold, while having infrared nothing in larger nonlinear optical effect and infrared light transmission scope wider concurrently again
Machine non-linear optical crystal material has particularly significant and wide application prospect in non-linear optical field.
The content of the invention
The present invention is intended to provide outstanding Inorganic crystal compound of two kinds of combination properties and preparation method thereof and described inorganic
Crystalline compounds as second-order non-linear optical crystal material application.
The present invention is achieved through the following technical solutions：
A kind of inorganic fluoriodate crystal, its chemical formula is RbBi2(IO3)2F5Belong to monoclinic system, its crystal space group
It is P21, its cell parameter isα=90 °, β=100.263
(2) °, γ=90 °.
One kind prepares RbBi2(IO3)2F5The method of crystal, comprises the following steps：It is 4 by mol ratio：1：4 RbF, Bi2O3
And H5IO6Add in hydrothermal reaction kettle, add hydrofluoric acid aqueous solution, stir, 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 more than 4 days is slowly dropped to room temperature afterwards；Instead
After should terminating, then product suction filtration is washed with deionized water and ethanol successively, that is, obtain RbBi2(IO3)2F5Crystal.
The hydrofluoric acid aqueous solution is by HF solution that mass fraction is 40% and water by volume 1：1~2 mixes.
The concentration of RbF is 0.667~1mol/L after addition hydrofluoric acid aqueous solution.
A kind of inorganic fluoriodate crystal, its chemical formula is CsBi2(IO3)2F5, belong to monoclinic system, its crystal space group
It is P21, its cell parameter isα=90 °, β=100.509 (6) °,
γ=90 °.
One kind prepares above-mentioned CsBi2(IO3)2F5The method of crystal, comprises the following steps：It is 4 by mol ratio：4：1：4
CsIO4：CsF、Bi2O3And H5IO6Add hydrothermal reaction kettle in, add hydrofluoric acid aqueous solution, stir, wherein HF mole
Number is more than five times of CsF；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, isothermal reaction more than 4 days, Zhi Houhuan
Slowly it is down to room temperature；After reaction terminates, then product suction filtration is washed with deionized water and ethanol successively, that is, obtain CsBi2
(IO3)2F5Crystal.
The hydrofluoric acid aqueous solution is by HF solution that mass fraction is 40% and water by volume 1：1~2 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 the inorganic fluoriodate crystal of above two：RbBi2(IO3)2F5It is KDP (potassium dihydrogen phosphate)
9.5 times；CsBi2(IO3)2F5It is 7.5 times of KDP.
The transparency range and band gap of the inorganic fluoriodate crystal of above two：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 the inorganic fluoriodate crystal of above two：RbBi2(IO3)2F5It is 240 DEG C, CsBi2(IO3)2F5
It is 270 DEG C.
Described cooling method is to be lowered the temperature with the speed of 1~8 DEG C/h.
Described reactor, its liner is polytetrafluoroethylene (PTFE) material.
Inorganic crystal compound of the present invention has advantages below and beneficial effect：
1. two kinds of the present invention inorganic fluoriodate crystal have larger frequency-doubled effect (SHG), Kurtz powder frequency doublings
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 the present invention inorganic fluoriodate crystal have transmission model wider in visible region and mid-infrared light area
Enclose, RbBi2(IO3)2F5Preferable translucency is respectively provided with 0.33-12.8 micron wavelength ranges；CsBi2(IO3)2F5In 0.32-
There is preferable translucency in 12.8 micron wavelength ranges；
3. two kinds of the present invention inorganic fluoriodate crystal are free of the crystallization water, to air-stable, not deliquescence, and it is thermally-stabilised
Property is preferable；
4. two kinds of the present invention inorganic fluoriodate crystal utilize Hydrothermal preparation method, simple to operate, raw material availability is high,
Experiment condition is gentle, product purity is high；
5. inorganic fluoriodate crystal of the present invention can realize phase as second-order non-linear optical crystal material
Match somebody with somebody.
Brief description of the drawings
Fig. 1 is RbBi of the present invention2(IO3)2F5Crystal structure figure；
Fig. 2 is RbBi of the present invention2(IO3)2F5Ab plane mesh structures 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 spectrograms；
Fig. 9 is CsBi of the present invention2(IO3)2F5ATR-FTIR spectrograms；
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 two kinds of the invention frequency-doubled effect intensity of inorganic fluoriodate crystal and particle size graph of relation.
Specific embodiment
Technical scheme is described in further detail with reference to specific embodiment and accompanying drawing, but the present invention
Implementation method not limited to this.
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 H5IO6Add in the hydrothermal reaction kettle of 23mL, add the hydrofluoric acid dilutions of 3mL,
The ultimate density for making RbF is 0.667mol/L；Closed hydrothermal reaction kettle is put into Muffle furnace, 230 DEG C, perseverance are heated to through 3h
Temperature reaction is cooled to room temperature in 4 days with the rate of temperature fall of 8 DEG C/h again；After reaction terminates, by product suction filtration and with deionized water and second
Alcohol is washed, that is, obtain inorganic fluorine acid iodide salt 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 H5IO6Add to the hydrothermal reaction kettle of 23mL, add the hydrofluoric acid dilutions of 2mL
The ultimate density for making RbF is 1mol/L；Closed hydrothermal reaction kettle is put into Muffle furnace, 230 DEG C are heated to through 3h, constant temperature is anti-
Answer 4 days and room temperature is cooled to the rate of temperature fall of 8 DEG C/h again；After reaction terminates, washed by product suction filtration and with deionized water and ethanol
Wash, that is, obtain inorganic fluorine acid iodide salt crystal RbBi2(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 H5IO6Add to the hydrothermal reaction kettle of 100mL, the hydrofluoric acid for adding 10mL is dilute
Releasing liquid makes the ultimate density of RbF be 1mol/L；Closed hydrothermal reaction kettle is put into Muffle furnace, 210 DEG C, perseverance are heated to through 3h
Temperature reaction is cooled to room temperature in 4 days with the rate of temperature fall of 1 DEG C/h again；After reaction terminates, by product suction filtration and with deionized water and second
Alcohol is washed, that is, obtain inorganic fluorine acid iodide salt 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 H5IO6Add to the hydrothermal reaction kettle of 23mL, add 2mL's
Hydrofluoric acid dilutions make the ultimate density of CsF be 1mol/L；Closed hydrothermal reaction kettle is put into Muffle furnace, is heated to through 3h
210 DEG C, isothermal reaction is cooled to room temperature in 4 days with the rate of temperature fall of 8 DEG C/h again；Reaction terminate after, by product suction filtration and spend from
Sub- water and ethanol are washed, that is, obtain inorganic fluorine acid iodide salt 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 H5IO6Add to the hydrothermal reaction kettle of 23mL, add 3mL's
Hydrofluoric acid dilutions make the ultimate density of CsF be 0.667mol/L；Closed hydrothermal reaction kettle is put into Muffle furnace, through 3h plus
To 230 DEG C, isothermal reaction is cooled to room temperature in 4 days to heat with the rate of temperature fall of 8 DEG C/h again；After reaction terminates, product suction filtration is used in combination
Deionized water and ethanol are washed, that is, obtain inorganic fluorine acid iodide salt 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 H5IO6Add to the hydrothermal reaction kettle of 100mL, add
The hydrofluoric acid dilutions of 10mL make the ultimate density of CsF be 1mol/L；Closed hydrothermal reaction kettle is put into Muffle furnace, through 3h
210 DEG C are heated to, isothermal reaction is cooled to room temperature in 4 days with the rate of temperature fall of 1 DEG C/h again；After reaction terminates, by product suction filtration simultaneously
Washed with deionized water and ethanol, that is, obtain inorganic fluorine acid iodide salt crystal CsBi2(IO3)2F5。
Frequency doubling property is tested：
Frequency-doubled effect and the phase matched test of the inorganic fluoriodate crystal prepared by the present invention are by Kurtz powder times
Frequency method of testing is obtained.Concrete operation step is as follows：The inorganic fluoriodate crystal of gained is ground and is sieved into respectively first
Different grain size scope 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 into Nd afterwards:YAG
During pulse laser is as the laser optical path of light source, using the fundamental frequency light irradiating sample pond that wavelength is 1064 nanometers, frequency-doubled signal
It is shown on oscillograph through photomultiplier.Frequency-doubled effect intensity is mapped to particle diameter, if intensity first becomes big with the increase of particle diameter
Then tend to platform, then illustrate phase matched；If intensity then reduces greatly as the increase of particle diameter first becomes, do not illustrate phase not
Match somebody with somebody.Using the KDP monocrystals of same particle size as standard specimen, take frequency-doubled effect and reach the sample and KDP of the particle diameter after platform and surveyed
The frequency-doubled signal intensity for obtaining carries out contrasting the relative size for obtaining frequency-doubled effect.
Crystal structure is tested：
The structure of prepared inorganic fluoriodate crystal is determined 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 its single structure cell contain a Rb atom, two kinds of Bi atoms, five F atoms, two kinds
I atoms and 6 O atoms.Fig. 1 is schematic diagram of the crystal structure in ac planes, in its crystal structure, Bi atoms, F atom, I
Atom and O atom are interconnected and constitute two-dimension plane structure, and Rb atoms are filled between planar structure, together constitute RbBi2
(IO3)2F5Three-D space structure.Fig. 2 is the planar structure schematic diagram being made up of Bi, F, I, O in structure, and Bi atoms are former with Bi
Son is connected by sharing F atom, and Bi atoms are connected with I atoms by sharing O atom, and a plane reticular is constituted in ab planes
Structure.Fig. 3 is the schematic diagram of anionic group in the structure, centered on heavy atom Bi and I, one of Bi atoms and five
F atom bonding is constituted with a pair of BiF of lone pair electrons5Group, Bi-F key bond distances areAnother Bi is former
Son and four F atoms and two kinds of O atoms are bonded composition BiO2F4Distortion structure, Bi-O key bond distances areBi-F keys
Bond distance isTwo kinds of I atoms form the IO with lone pair electrons with three O atom bondings respectively3Structure, I-O keys
Bond distance isIn the crystal structure of the compound, the BiF of lone pair electrons5Group, BiO2F4Distortion structure
With the IO with lone pair electrons3Three kinds of anionic groups of structure all have larger structural aberration, and IO3Structure is in b direction of principal axis
On be arranged with a superposition for dipole moment；BiF5Group shows in the distribution of b direction of principal axis, two kinds shorter of Bi-F keys and two kinds
Bi-F keys more long are distributed in the both sides of Bi atoms, therefore BiF respectively5Group also has microcosmic dipole moment in b direction of principal axis；Together
Reason, BiO2F4The key distribution of structure displays that it has microcosmic dipole moment on b direction of principal axis.And BiF5Group, BiO2F4Structure
And IO3The arrangement mode of structure causes that their microcosmic dipole moment is overlapped mutually, directly results in the structure on b direction of principal axis compared with
Big dipole moment, so that RbBi2(IO3)2F5Crystal is macroscopically showing very strong second order nonlinear optical effect.
CsBi2(IO3)2F5Crystal structure and RbBi2(IO3)2F5Crystal structure be similar to, as shown in figure 4, being also former by Bi atoms, F
Son, I atoms and O atom are interconnected and constitute two-dimension plane structure, and Cs atoms constitute three dimensions between being filled in planar structure
Structure.Fig. 5 is CsBi2(IO3)2F5Crystal structure in anionic group schematic diagram, with RbBi2(IO3)2F5Crystal structure class
Seemingly, the BiF in its structure5Group, BiO2F4Structure and IO3The arrangement mode of structure also causes that they are microcosmic on b direction of principal axis
Dipole moment is overlapped mutually, so that 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 spectrograms of crystal are respectively such as Fig. 6 and Fig. 7
Shown, two kinds of inorganic fluoriodate crystal are respectively provided with larger optical band gap, RbBi2(IO3)2F5About 3.78eV, CsBi2
(IO3)2F5About 3.84eV；Two kinds of ATR-FTIR spectrograms of compound such as Fig. 8 and as shown in figure 9, their INFRARED ABSORPTION respectively
Side is up to 12.8 microns；Thermal weight loss spectrogram is distinguished as shown in Figure 10 and Figure 11, RbBi2(IO3)2F5Crystal is opened at 240 DEG C
Beginning thermal weight loss, CsBi2(IO3)2F5Crystal starts thermal weight losses at 270 DEG C, and two kinds of compound crystals are respectively provided with excellent thermally-stabilised
Property；With the relation curve of sample particle diameter as shown in figure 12, both inorganic fluoriodates are brilliant for their frequency-doubled effect (SHG) intensity
Body is respectively provided with stronger second order nonlinear optical effect and can realize 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 a word, both Inorganic crystal compounds are respectively provided with excellent combination property, can be brilliant as second nonlinear optic
Body material is applied.
Embodiments of the present invention are explained in detail above in conjunction with accompanying drawing, but the present invention is not limited to the implementation
Mode, can be in the ken that possesses of one skilled in the relevant art and on the premise of present inventive concept is not departed from
Make 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, belonging to monoclinic system, it is brilliant
Body space group is P21, its cell parameter isα=90 °, β=
100.263 (2) °, γ=90 °.
2. a kind of RbBi prepared described in claim 12(IO3)2F5The method of crystal, it is characterised in that comprise the following steps：Will
Mol ratio is 4：1：4 RbF, Bi2O3And H5IO6Add in hydrothermal reaction kettle, add hydrofluoric acid aqueous solution, stir, its
In, the molal quantity of HF is more than five times of RbF；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, isothermal reaction 4 days
More than, room temperature is slowly dropped to afterwards；After reaction terminates, then product suction filtration is washed with deionized water and ethanol successively, obtained final product
To RbBi2(IO3)2F5Crystal.
3. the method according to claims 2, it is characterised in that：The hydrofluoric acid aqueous solution is 40% by mass fraction
HF solution and water by volume 1：1~2 mixes.
4. the method according to claims 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, belonging to monoclinic system, it is brilliant
Body space group is P21, its cell parameter isα=90 °, β=
100.509 (6) °, γ=90 °.
6. a kind of CsBi prepared described in claim 52(IO3)2F5The method of crystal, it is characterised in that comprise the following steps：Will
Mol ratio is 4：4：1：4 CsIO4：CsF、Bi2O3And H5IO6Add in hydrothermal reaction kettle, add hydrofluoric acid aqueous solution, stir
Uniformly, wherein the molal quantity of HF is more than five times of CsF；By hydrothermal reaction kettle it is closed after be heated to 210 DEG C -230 DEG C, constant temperature is anti-
Answer more than 4 days, room temperature is slowly dropped to afterwards；After reaction terminates, then product suction filtration is washed with deionized water and ethanol successively
Wash, that is, obtain CsBi2(IO3)2F5Crystal.
7. the method according to claims 6, it is characterised in that：The hydrofluoric acid aqueous solution is 40% by mass fraction
HF solution and water by volume 1：1~2 mixes.
8. the method according to claims 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 inorganic fluoriodate crystal described in claims 1 or 5 as non-linear optical crystal material in optical field
Using.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016112466961 | 2016-12-29 | ||
| CN201611246696 | 2016-12-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106757344A true CN106757344A (en) | 2017-05-31 |
| CN106757344B CN106757344B (en) | 2018-11-23 |
Family
ID=58941450
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710047966.4A Active CN106757344B (en) | 2016-12-29 | 2017-01-20 | Two kinds of inorganic fluoriodate crystal and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106757344B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108363259A (en) * | 2018-02-08 | 2018-08-03 | 中国科学院福建物质结构研究所 | A kind of inorganic crystal material, its prepare and as nonlinear optical crystal application |
| CN109023502A (en) * | 2018-09-06 | 2018-12-18 | 中国科学院新疆理化技术研究所 | Compound fluorine cerous iodate and fluorine cerous iodate nonlinear optical crystal and preparation method and purposes |
| CN111321455A (en) * | 2018-12-17 | 2020-06-23 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal niobium oxysulfate iodate as well as preparation method and application thereof |
| CN113337890A (en) * | 2020-03-03 | 2021-09-03 | 中国科学院福建物质结构研究所 | Preparation method and application of yttrium fluoiodate compound and crystal thereof |
| CN115404548A (en) * | 2021-05-28 | 2022-11-29 | 深圳市启扬光学科技有限公司 | Compound fluorine-containing titanium iodate and fluorine-containing titanium iodate nonlinear optical crystal, and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831698A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Non-linear optical crystal of iodic acid zinc potassium |
| CN102808220A (en) * | 2011-05-31 | 2012-12-05 | 中国科学院理化技术研究所 | Nonlinear optical crystal Bi2I4O13And preparation method and application thereof |
| CN103757701A (en) * | 2014-02-20 | 2014-04-30 | 武汉大学 | Nonlinear optical crystal bismuth potassium iodide, and preparation method and application thereof |
| CN103789831A (en) * | 2014-02-20 | 2014-05-14 | 武汉大学 | Nonlinear optical crystal bismuth rubidium iodate as well as preparation method and application thereof |
-
2017
- 2017-01-20 CN CN201710047966.4A patent/CN106757344B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831698A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Non-linear optical crystal of iodic acid zinc potassium |
| CN102808220A (en) * | 2011-05-31 | 2012-12-05 | 中国科学院理化技术研究所 | Nonlinear optical crystal Bi2I4O13And preparation method and application thereof |
| CN103757701A (en) * | 2014-02-20 | 2014-04-30 | 武汉大学 | Nonlinear optical crystal bismuth potassium iodide, and preparation method and application thereof |
| CN103789831A (en) * | 2014-02-20 | 2014-05-14 | 武汉大学 | Nonlinear optical crystal bismuth rubidium iodate as well as preparation method and application thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108363259A (en) * | 2018-02-08 | 2018-08-03 | 中国科学院福建物质结构研究所 | A kind of inorganic crystal material, its prepare and as nonlinear optical crystal application |
| CN108363259B (en) * | 2018-02-08 | 2020-08-28 | 中国科学院福建物质结构研究所 | Inorganic crystal material, preparation thereof and application of inorganic crystal material as nonlinear optical crystal |
| CN109023502A (en) * | 2018-09-06 | 2018-12-18 | 中国科学院新疆理化技术研究所 | Compound fluorine cerous iodate and fluorine cerous iodate nonlinear optical crystal and preparation method and purposes |
| CN109023502B (en) * | 2018-09-06 | 2020-07-28 | 中国科学院新疆理化技术研究所 | Compound cerium fluoroiodate, cerium fluoroiodate nonlinear optical crystal, preparation method and application |
| CN111321455A (en) * | 2018-12-17 | 2020-06-23 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal niobium oxysulfate iodate as well as preparation method and application thereof |
| CN111321455B (en) * | 2018-12-17 | 2021-05-11 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal niobium oxysulfate iodate as well as preparation method and application thereof |
| CN113337890A (en) * | 2020-03-03 | 2021-09-03 | 中国科学院福建物质结构研究所 | Preparation method and application of yttrium fluoiodate compound and crystal thereof |
| CN115404548A (en) * | 2021-05-28 | 2022-11-29 | 深圳市启扬光学科技有限公司 | Compound fluorine-containing titanium iodate and fluorine-containing titanium iodate nonlinear optical crystal, and preparation method and application thereof |
| CN115404548B (en) * | 2021-05-28 | 2023-11-03 | 深圳市启扬光学科技有限公司 | Compound fluorine-containing titanodinate and fluorine-containing titanodinate nonlinear optical crystal, and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106757344B (en) | 2018-11-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mutailipu et al. | Toward the enhancement of critical performance for deep-ultraviolet frequency-doubling crystals utilizing covalent tetrahedra | |
| Li et al. | Mixed-anion inorganic compounds: a favorable candidate for infrared nonlinear optical materials | |
| Yang et al. | AZn2BO3X2 (A= K, Rb, NH4; X= Cl, Br): New members of KBBF family exhibiting large SHG response and the enhancement of layer interaction by modified structures | |
| CN106757344B (en) | Two kinds of inorganic fluoriodate crystal and its preparation method and application | |
| Ran et al. | Enhanced second-harmonic-generation efficiency and birefringence in melillite oxychalcogenides Sr2MGe2OS6 (M= Mn, Zn, and Cd) | |
| Han et al. | Experimental and theoretical studies on the linear and nonlinear optical properties of lead phosphate crystals LiPbPO 4 | |
| Guo et al. | BaBe2BO3F3: A KBBF-type deep-ultraviolet nonlinear optical material with reinforced [Be2BO3F2]∞ layers and short phase-matching wavelength | |
| Shi et al. | A2Bi2 (SeO3) 3F2 (A= K and Rb): excellent mid-infrared nonlinear optical materials with both strong SHG responses and large band gaps | |
| Luo et al. | Na4La2 (CO3) 5 and CsNa5Ca5 (CO3) 8: two new carbonates as UV nonlinear optical materials | |
| Li et al. | Exploring short-wavelength phase-matching nonlinear optical crystals by employing KBe2BO3F2 as the template | |
| Zhou et al. | Rational Design of Novel Promising Infrared Nonlinear Optical Materials: Structural Chemistry and Balanced Performances | |
| CN103031607B (en) | Infrared nonlinear optical crystal AB4C5Se12 | |
| CN105002558B (en) | Second-order non-linear optical crystal K2SbF2Cl3And its preparation method and application | |
| Shi et al. | Phase matching achieved by isomorphous substitution in IR nonlinear optical material Ba 2 SnSSi 2 O 7 with an undiscovered [SnO 4 S] functional motif | |
| Wang et al. | Exploring potential beryllium-free, deep-ultraviolet optical crystals in the rare earth fluoride carbonate–water system | |
| CN107021462A (en) | Selenium gallium zinc barium compound, selenium gallium zinc barium infrared nonlinear optical crystal and its production and use | |
| CN106435737A (en) | Infrared nonlinear optical crystal and preparation method thereof | |
| He et al. | Hydrogen bonding assisted construction of graphite-like deep-UV optical materials with two types of parallel π-conjugated units | |
| CN106757362A (en) | Selenium germanium cadmium strontium compound and preparation method thereof, selenium germanium cadmium strontium crystal and its preparation method and application | |
| Aibibula et al. | Rb3Na (H2C3N3O3) 4· 3H2O with large birefringence | |
| CN103789831B (en) | Non-linear optical crystal of iodic acid bismuth rubidium and its preparation method and application | |
| CN108070906A (en) | Non-linear optical crystal of iodic acid germanium lithium and its preparation method and application | |
| CN105755542A (en) | Crystal material, preparation method of crystal material, and application of crystal material as non-linear optical crystal | |
| CN105624780B (en) | Nonlinear optical crystal fluoboric acid beryllium and its preparation method and application | |
| CN104562196A (en) | Compound lead borate hydrate nonlinear optical crystal and preparation method and use thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |