CN103435060A - Boron-strontium compound - Google Patents

Boron-strontium compound Download PDF

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CN103435060A
CN103435060A CN201310344834XA CN201310344834A CN103435060A CN 103435060 A CN103435060 A CN 103435060A CN 201310344834X A CN201310344834X A CN 201310344834XA CN 201310344834 A CN201310344834 A CN 201310344834A CN 103435060 A CN103435060 A CN 103435060A
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compound
crystal
boron
strontium compound
srco
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唐志华
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Shaanxi University of Technology
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Shaanxi University of Technology
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Abstract

The invention discloses a boron-strontium compound and relates to the field of intraocular crystals and crystal growth. The chemical formula of the compound is Sr2B16O26, and the molecular weight of the compound is 764.22. The compound is prepared through the following steps: S1, weighing Bi2O3, SrCO3 and H3BO3, wherein the molar ratio of the Bi2O3 to the SrCO3 to the H3BO3 is 3 to 3 to 26; S2, mixing the Bi2O3, the SrCO3 and the H3BO3 weighed in the S1, placing the mixture in a small crucible, heating to 735 DEG C, performing reaction for two weeks, then cooling to 500 DEG C at the speed of 5 DEG C/h, and finally cooling to indoor temperature at the speed of 20 DEG C/h to obtain the boron-strontium compound and prepare crystals of the boron-strontium compound.

Description

A kind of boron strontium compound
Technical field
The present invention relates to artificial lens and field of crystal growth, especially relate to a kind of boron strontium compound, and turn out its crystal.
Background technology
Along with the development of laser science and technology, aspect frequency inverted, the inorganic nonlinear optical crystal material plays a part more and more important, particularly in ultraviolet and deep ultraviolet spectrum zone.This has proposed various new demands to functional crystal, also more and more higher to the specification of quality of existing crystal.
Borate crystal has abundant structure species, has wide to see through wave band, high damage threshold, stable physics and chemistry character, the moderate characteristics such as degree of birefringence, so be widely used as nonlinear optical material and laser, luminous host material.They have broad application prospects at numerous areas such as laser freuqency doubling, Electro-optical Modulation, parametric oscillation, holographic real-time storages.
According to current inorganic nonlinear optical crystal Materials situation, the novel inorganic non-linear optic crystal is not only required to have large Clock Multiplier Factor, but also require its over-all properties parameter good, be easy to generate high quality and large size body piece crystal, this carries out a large amount of systems and deep research work with regard to needs simultaneously.Further investigation to borate salt system has important actual application value, and except existing functional crystal being managed to continue to improve quality or doping vario-property, exploring and finding various new function crystal is a heat subject all the time.
Summary of the invention
Technical problem to be solved by this invention is: a kind of boron strontium compound and crystal thereof are provided, relate to boron strontium compound crystal synthetic method and Crystal Structure.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of boron strontium compound, is characterized in that, the chemical formula of this compound is Sr 2b 16o 26, molecular weight is 764.22, the preparation of this compound comprises the steps:
S1: take Bi 2o 3, SrCO 3and H 3bO 3, described Bi 2o 3: SrCO 3: H 3bO 3mol ratio be 3: 3: 26;
S2: by the Bi taken in step S1 2o 3, SrCO 3and H 3bO 3the monkey of packing into after mixing, be heated to 735 ℃, reacts 2 weeks, and then the speed of 5 ℃/h is cooled to 500 ℃, finally is cooled to room temperature with 20 ℃/h again, can obtain the boron strontium compound.
The crystal of above-mentioned boron strontium compound, is characterized in that, the chemical formula of this crystal is Sr 2b 16o 26, molecular weight is 764.22, this monocrystalline belongs to oblique system, P2 1/ c spacer, unit cell parameters , , β=106.330 (10) °, Z=4, its crystal is the cancellated [B of 3 dimension 16o 32] 16-, by 12 triangular pyramid type BO 3with 4 positive tetrahedron type BO 4forming, is to have connected three three boric acid [B on five boric acid 3o 7] 5-with two borate [BO 3] 3-.
Adopted technique scheme, beneficial effect of the present invention is: prepared a kind of new boron strontium compound and crystal thereof, production technique of the present invention is fairly simple, and production cost is lower, and the security of production is higher.
The accompanying drawing explanation
Accompanying drawing 1 is the powder x-ray diffraction collection of illustrative plates (a) of the compounds of this invention and x ray diffraction pattern monocrystalline data (b) of the present invention;
Accompanying drawing 2 is single crystal structure figure of the compounds of this invention;
Accompanying drawing 3 is the compounds of this invention crystalline structure figure along a axle;
Accompanying drawing 4 is the compounds of this invention crystalline structure figure along c-axis;
Accompanying drawing 5 is infrared spectrograms of the compounds of this invention;
Wherein: in accompanying drawing 3, Sr 1atom: cross bar circle; Sr 2atom: circle; BO 3group: the trilateral that parallel lines are filled; BO 4group: the tetrahedral that cross bar is inside arranged.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
A kind of boron strontium compound, the chemical formula of this compound is Sr 2b 16o 26, molecular weight is 764.22, the preparation of this compound comprises the steps:
S1: take Bi 2o 3, SrCO 3and H 3bO 3, described Bi 2o3: SrCO 3: H 3bO 3mol ratio be 3: 3: 26;
S2: by the Bi taken in step S1 2o 3, SrCO 3and H 3bO 3the monkey of packing into after mixing, be heated to 735 ℃, reacts 2 weeks, and then the speed of 5 ℃/h is cooled to 500 ℃, finally is cooled to room temperature with 20 ℃/h again, can obtain the boron strontium compound.
The crystal of above-mentioned boron strontium compound, the chemical formula of this crystal is Sr 2b 16o 26, molecular weight is 764.22, this monocrystalline belongs to oblique system, P2 1/ c spacer, unit cell parameters
Figure BSA0000093720840000031
Figure BSA0000093720840000032
, β=106.330 (10) °, Z=4, its crystal is the cancellated [B of 3 dimension 16o 32] 16-, by 12 triangular pyramid type BO 3with 4 positive tetrahedron type BO 4forming, is to have connected three three boric acid [B on five boric acid 3o 7] 5-with two borate [BO 3] 3-; This tridimensional network provides cross one another open channel, and a axle at the Sr place in the allomeric is parallel with c-axis.Infrared spectra has further proved in structure and has had BO 3and BO 4group.
Crystal prepared by the present invention carries out x ray single crystal diffraction.Crystal also can carry out the scanning of x X-ray analysis X by electron microscope, and it is unique heavy element that result is presented at strontium in compound.Although do not detect Bi in final structure, the borate of bismuth may serve as the fusing assistant of crystal growth.
Turned out Sr under 735 ℃ 2b 16o 26monocrystalline.For preparation Sr 2b 16o 26polycrystalline, we are in proportion by SrCO 3and H 3bO 3after mixing, at 600 ℃, heat 2 weeks, and by the x ray powder diffraction, intermediate and the finished product are wherein analyzed, result shows, x ray diffraction experimental patterns and monocrystalline data calculating collection of illustrative plates are compared, clearly experimental observation to collection of illustrative plates and Theoretical Calculation gained collection of illustrative plates reach well and coincide, as shown in Figure 1.
The crystal of preparing has been carried out to the Single Crystal X-ray diffraction, the Single Crystal X-ray diffraction data is to adopt the Mo Ka ray scanning of monochromatization under 298K on AFC7R Rigaku four-circle diffractometer, the least-squares refinement of structure cell the data, 2 36.64 ° of θ sweep limits~44.28 °, every 150 point diffractions remeasure three standard point diffractions one time, except crossing in ± 1.43% scope, fluctuation, do not observe obvious decay.
Crystalline structure is directly provided by the SHELXS97 routine package, and whole atomic coordinate and anisotropy thermal parameter thereof are carried out to the complete matrix least-squares refinement.After refine, R is respectively 0.0395 and 0.0751,3724 of observable point diffractions [I >=2 σ (I)].Electron density difference is not obvious, and high electron density is less than 0.615eA °-3, and the crystalline structure data see the following form 1.Bond distance in crystalline structure sees the following form 2, the bond angle in crystalline structure and following table 3.
Table 1Sr 2b 16o 26the crystalline structure data
Figure BSA0000093720840000051
Table 2.Sr 2b 16o 26bond distance in crystal (A °)
Figure BSA0000093720840000061
Table 3Sr 2b 16o 26bond angle in crystal (°)
Figure BSA0000093720840000071
Whether it is emphasized that compound has shown some interfere informations, be our target compound in order to judge product, to Sr 2b 16o 26in atomic parameter carry out refine, B 2and O 26all with theoretical value, well coincide, determined compound S r 2b 16o 26.
The present invention is not limited to above-mentioned concrete embodiment, and those of ordinary skill in the art is from above-mentioned design, and without performing creative labour, all conversion of having done, within all dropping on protection scope of the present invention.

Claims (2)

1. a boron strontium compound, is characterized in that, the chemical formula of this compound is Sr 2b 16o 26, molecular weight is 764.22, the preparation of this compound comprises the steps:
S1: take Bi 2o 3, SrCO 3and H 3bO 3, described Bi 2o 3: SrCO 3: H 3bO 3mol ratio be 3: 3: 26;
S2: by the Bi taken in step S1 2o 3, SrCO 3and H 3bO 3the monkey of packing into after mixing, be heated to 735 ℃, reacts 2 weeks, and then the speed of 5 ℃/h is cooled to 500 ℃, finally is cooled to room temperature with 20 ℃/h again, can obtain the boron strontium compound.
2. the crystal of a kind of boron strontium compound according to claim 1, is characterized in that, the chemical formula of this crystal is Sr 2b 16o 26, molecular weight is 764.22, this monocrystalline belongs to oblique system, P2 1/ c spacer, unit cell parameters
Figure FSA0000093720830000011
, β=106.330 (10) °, Z=4, its crystal is the cancellated [B of 3 dimension 16o 32] 16-, by 12 triangular pyramid type BO 3with 4 positive tetrahedron type BO 4forming, is to have connected three three boric acid [B on five boric acid 3o 7] 5-with two borate [BO 3] 3-.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0648818A1 (en) * 1993-10-06 1995-04-19 Sakai Chemical Industry Co., Ltd., Strontium borate pigment composition, method of making same, and processes for imparting anti-corrosive, anti-bacterial and/or anti-fungal, and non-flammable properties to materials by using same
US5858079A (en) * 1996-11-18 1999-01-12 Sakai Chemical Industry Co., Ltd. Strontium borate pigment composition, method of making same, and processes of imparting anti-corrosive, anti-bacterial/anti-fungal and non-flammable properties to materials by using same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0648818A1 (en) * 1993-10-06 1995-04-19 Sakai Chemical Industry Co., Ltd., Strontium borate pigment composition, method of making same, and processes for imparting anti-corrosive, anti-bacterial and/or anti-fungal, and non-flammable properties to materials by using same
US5858079A (en) * 1996-11-18 1999-01-12 Sakai Chemical Industry Co., Ltd. Strontium borate pigment composition, method of making same, and processes of imparting anti-corrosive, anti-bacterial/anti-fungal and non-flammable properties to materials by using same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ALI HUSSAIN RESHAK,ET AL.: "X-ray Diffraction, X-ray Photoelectron Spectra, Crystal Structure, and Optical Properties", 《J. PHYS. CHEM. B》 *
ZHI-HUA TANG,ET.AL.: "Synthesis and crystal structure of a new strontium borate, Sr2B16O26", 《SOLID STATE SCIENCES》 *

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Application publication date: 20131211