CN103435060A - A strontium boron compound - Google Patents
A strontium boron compound Download PDFInfo
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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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- ZQYZLRKRUCDMQI-UHFFFAOYSA-N boron strontium Chemical compound [Sr].[B] ZQYZLRKRUCDMQI-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 49
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 6
- 150000007513 acids Chemical class 0.000 claims description 3
- 150000001642 boronic acid derivatives Chemical class 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000547 structure data Methods 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- YISOXLVRWFDIKD-UHFFFAOYSA-N bismuth;borate Chemical class [Bi+3].[O-]B([O-])[O-] YISOXLVRWFDIKD-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical group OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000004467 single crystal X-ray diffraction Methods 0.000 description 1
- 238000000373 single-crystal X-ray diffraction data Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
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Abstract
本发明公开了一种硼锶化合物，涉及人工晶体和晶体生长领域。该化合物的化学式为Sr2B16O26，分子量为764.22，该化合物的制备包括如下步骤：S1：称取Bi2O3，SrCO3和H3BO3，所述Bi2O3∶SrCO3∶H3BO3的摩尔比为3∶3∶26；S2：将步骤S1中称取的Bi2O3，SrCO3和H3BO3混合后装入小坩埚，加热至735℃，反应2周，然后5℃/h的速率冷却至500℃，最后再以20℃/h冷却至室温，即可得到硼锶化合物，并且制得了该硼锶化合物的晶体。
The invention discloses a boron-strontium compound and relates to the field of artificial crystal and crystal growth. The chemical formula of this compound is Sr 2 B 16 O 26 , and its molecular weight is 764.22. The preparation of this compound includes the following steps: S1: Weigh Bi 2 O 3 , SrCO 3 and H 3 BO 3 , and the Bi 2 O 3 : SrCO 3 The molar ratio of : H 3 BO 3 is 3: 3: 26; S2: Mix the Bi 2 O 3 , SrCO 3 and H 3 BO 3 weighed in step S1, put them into a small crucible, heat to 735°C, and react 2 week, then cooled at a rate of 5°C/h to 500°C, and finally cooled to room temperature at 20°C/h to obtain the boron strontium compound, and the crystal of the boron strontium compound was obtained.
Description
技术领域technical field
本发明涉及人工晶体和晶体生长领域，尤其是涉及一种硼锶化合物，并且培养出其晶体。The invention relates to the fields of artificial crystals and crystal growth, in particular to a boron-strontium compound and its crystals.
背景技术Background technique
随着激光科学和技术的不断发展，在频率转换方面，无机非线性光学晶体材料起着越来越重要的作用，特别是在紫外和深紫外光谱区域。这对功能晶体提出了各种各样的新要求，对现有晶体的质量要求也越来越高。With the continuous development of laser science and technology, inorganic nonlinear optical crystal materials play an increasingly important role in frequency conversion, especially in the ultraviolet and deep ultraviolet spectral regions. This puts forward various new requirements for functional crystals, and the quality requirements for existing crystals are also getting higher and higher.
硼酸盐晶体具有丰富的结构种类，具有宽的透过波段、高的损伤阀值、稳定的物理和化学性质、适中的双折射率等特点，所以广泛用作非线性的光学材料和激光、发光基质材料。它们在激光倍频、电光调制、参量振荡、实时全息存储等诸多领域有着广阔的应用前景。Borate crystals have rich structure types, wide transmission band, high damage threshold, stable physical and chemical properties, moderate birefringence, etc., so they are widely used as nonlinear optical materials and lasers, Luminescent matrix material. They have broad application prospects in many fields such as laser frequency doubling, electro-optic modulation, parametric oscillation, and real-time holographic storage.
根据当前无机非线性光学晶体材料发展情况，对新型无机非线性光学晶体不仅要求具有大的倍频系数，而且还要求它的综合性能参数好，同时易于生成优质大尺寸体块晶体，这就需要进行大量系统而深入的研究工作。对硼酸盐体系的深入研究有着重要的实际应用价值，除了对现有的功能晶体设法继续提高质量或掺杂改性外，探索寻找各种新型功能晶体始终是一个热门课题。According to the current development of inorganic nonlinear optical crystal materials, the new inorganic nonlinear optical crystal not only requires a large frequency multiplication coefficient, but also requires its comprehensive performance parameters to be good, and at the same time, it is easy to produce high-quality large-size bulk crystals, which requires Carry out a lot of systematic and in-depth research work. In-depth research on the borate system has important practical application value. In addition to trying to continue to improve the quality or doping modification of the existing functional crystals, it is always a hot topic to explore and find various new functional crystals.
发明内容Contents of the invention
本发明所要解决的技术问题是：提供一种硼锶化合物及其晶体，涉及硼锶化合物晶体合成方法和晶体结构表征。The technical problem to be solved by the present invention is to provide a boron-strontium compound and its crystal, which relate to a crystal synthesis method and crystal structure characterization of the boron-strontium compound.
为解决上述技术问题，本发明的技术方案是：In order to solve the problems of the technologies described above, the technical solution of the present invention is:
一种硼锶化合物，其特征是，该化合物的化学式为Sr2B16O26，分子量为764.22，该化合物的制备包括如下步骤：A strontium boron compound is characterized in that the chemical formula of the compound is Sr 2 B 16 O 26 and the molecular weight is 764.22. The preparation of the compound comprises the following steps:
S1：称取Bi2O3，SrCO3和H3BO3，所述Bi2O3∶SrCO3∶H3BO3的摩尔比为3∶3∶26；S1: Weigh Bi 2 O 3 , SrCO 3 and H 3 BO 3 , the molar ratio of Bi 2 O 3 : SrCO 3 : H 3 BO 3 is 3:3:26;
S2：将步骤S1中称取的Bi2O3，SrCO3和H3BO3混合后装入小坩埚，加热至735℃，反应2周，然后5℃/h的速率冷却至500℃，最后再以20℃/h冷却至室温，即可得到硼锶化合物。S2: Mix the Bi 2 O 3 , SrCO 3 and H 3 BO 3 weighed in step S1, put them into a small crucible, heat to 735°C, react for 2 weeks, then cool to 500°C at a rate of 5°C/h, and finally Then cool down to room temperature at 20°C/h to obtain boron strontium compound.
上述硼锶化合物的晶体，其特征是，该晶体的化学式为Sr2B16O26，分子量为764.22，该单晶属于单斜晶系，P21/c空间群，晶胞参数，，β＝106.330(10)°，Z＝4，其晶体为3维网状结构的[B16O32]16-，由12个三角锥型BO3和4个正四面体型BO4构成，是一个五硼酸上连接了三个三硼酸[B3O7]5-和两个硼酸根[BO3]3-。The above-mentioned crystal of strontium boron compound is characterized in that the chemical formula of the crystal is Sr 2 B 16 O 26 , the molecular weight is 764.22, the single crystal belongs to the monoclinic system, the space group P2 1 /c, and the unit cell parameters , , β=106.330(10)°, Z=4, its crystal is [B 16 O 32 ] 16- with 3-dimensional network structure, composed of 12 triangular pyramid BO 3 and 4 regular tetrahedral BO 4 , is Three triboronic acids [B 3 O 7 ] 5- and two borates [BO 3 ] 3- are connected to one pentaboronic acid.
采用了上述技术方案，本发明的有益效果为：制备了一种新的硼锶化合物及其晶体，本发明的生产工艺比较简单，生产成本较低，生产的安全性较高。By adopting the above technical scheme, the beneficial effects of the present invention are: a new boron-strontium compound and its crystal are prepared, the production process of the present invention is relatively simple, the production cost is low, and the production safety is high.
附图说明Description of drawings
附图1是本发明化合物的粉末X-射线衍射图谱(a)和本发明的的x射线衍射模式单晶数据(b)；Accompanying drawing 1 is the powder X-ray diffraction pattern (a) of the compound of the present invention and the single crystal data (b) of the x-ray diffraction mode of the present invention;
附图2是本发明化合物的单晶结构图；Accompanying drawing 2 is the single crystal structure diagram of the compound of the present invention;
附图3是本发明化合物沿a轴的晶体结构图；Accompanying drawing 3 is the crystal structure diagram of the compound of the present invention along the a axis;
附图4是本发明化合物沿c轴的晶体结构图；Accompanying drawing 4 is the crystal structure diagram of the compound of the present invention along the c-axis;
附图5是本发明化合物的红外光谱图；Accompanying drawing 5 is the infrared spectrogram of compound of the present invention;
其中：附图3中，Sr1原子：十字架圆圈；Sr2原子：圆圈；BO3基团：平行线填充的三角形；BO4基团：内有十字架的四面体状。Wherein: in accompanying drawing 3, Sr 1 atom: cross circle; Sr 2 atom: circle; BO 3 group: triangle filled with parallel lines; BO 4 group: tetrahedral shape with cross inside.
具体实施方式Detailed ways
下面结合附图和实施例对本发明进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and embodiments.
一种硼锶化合物，该化合物的化学式为Sr2B16O26，分子量为764.22，该化合物的制备包括如下步骤：A strontium boron compound, the compound has a chemical formula of Sr 2 B 16 O 26 and a molecular weight of 764.22. The preparation of the compound comprises the following steps:
S1：称取Bi2O3，SrCO3和H3BO3，所述Bi2O3∶SrCO3∶H3BO3的摩尔比为3∶3∶26；S1: Weigh Bi 2 O 3 , SrCO 3 and H 3 BO 3 , the molar ratio of Bi 2 O3:SrCO 3 : H 3 BO 3 is 3:3:26;
S2：将步骤S1中称取的Bi2O3，SrCO3和H3BO3混合后装入小坩埚，加热至735℃，反应2周，然后5℃/h的速率冷却至500℃，最后再以20℃/h冷却至室温，即可得到硼锶化合物。S2: Mix the Bi 2 O 3 , SrCO 3 and H 3 BO 3 weighed in step S1, put them into a small crucible, heat to 735°C, react for 2 weeks, then cool to 500°C at a rate of 5°C/h, and finally Then cool down to room temperature at 20°C/h to obtain boron strontium compound.
上述硼锶化合物的晶体，该晶体的化学式为Sr2B16O26，分子量为764.22，该单晶属于单斜晶系，P21/c空间群，晶胞参数
对本发明制备的晶体进行x射线单晶衍射。晶体也可以通过电子显微镜进行x射线分析扫描，结果显示在化合物中锶是唯一的重元素。虽然最终的结构中没有检测出Bi，但铋的硼酸盐可能充当了晶体生长的助熔剂。X-ray single crystal diffraction is carried out on the crystal prepared by the present invention. The crystals were also scanned by an electron microscope for x-ray analysis, which revealed that strontium was the only heavy element in the compound. Although no Bi was detected in the final structure, bismuth borates may have acted as a flux for crystal growth.
在735℃下培养出了Sr2B16O26单晶。为制备Sr2B16O26多晶，我们按比例将SrCO3和H3BO3混合后在600℃加热2周，并通过x射线粉末衍射对其中的中间体和最终产品进行分析，结果表明，将x射线衍射实验图谱与单晶数据计算图谱进行比较，很明显实验观察到的图谱与理论计算所得图谱达到很好的吻合，如附图1所示。Sr 2 B 16 O 26 single crystals were grown at 735°C. To prepare polycrystalline Sr 2 B 16 O 26 , we mixed SrCO 3 and H 3 BO 3 in proportion and heated them at 600°C for 2 weeks, and analyzed the intermediates and final products by X-ray powder diffraction. The results showed that , Comparing the X-ray diffraction experimental spectrum with the calculated spectrum of single crystal data, it is obvious that the experimentally observed spectrum is in good agreement with the theoretically calculated spectrum, as shown in Figure 1.
对制备出的晶体进行了单晶X射线衍射，单晶X射线衍射数据是298K下在AFC7R Rigaku四圆衍射仪上采用单色化的Mo Ka射线扫描，晶胞数据采用最小二乘法修正，2θ扫描范围36.64°～44.28°，每150个衍射点重新测量一次三个标准衍射点，除过在±1.43％范围内波动外没有观察到明显衰减。The prepared crystals were subjected to single crystal X-ray diffraction. The single crystal X-ray diffraction data was scanned by monochromatic Mo Ka rays on the AFC7R Rigaku four-circle diffractometer at 298K. The unit cell data was corrected by the least square method, and the 2θ The scanning range is 36.64°～44.28°, and the three standard diffraction points are re-measured every 150 diffraction points. No obvious attenuation is observed except for fluctuations in the range of ±1.43%.
晶体结构由SHELXS97程序包直接给出，对全部原子坐标及其各向异性热参数进行全矩阵最小二乘法修正。精修后R分别为0.0395和0.0751，可观察衍射点3724个[I≥2σ(I)]。电子密度差异不明显，最高电子密度小于0.615eA°-3，晶体结构数据见下表1。晶体结构中的键长见下表2，晶体结构中的键角和下表3。The crystal structure is directly given by the SHELXS97 program package, and the full-matrix least-squares correction is performed on all atomic coordinates and their anisotropic thermal parameters. After refinement, R is 0.0395 and 0.0751 respectively, and 3724 diffraction points [I≥2σ(I)] can be observed. The difference in electron density is not obvious, and the highest electron density is less than 0.615eA°-3. The crystal structure data are shown in Table 1 below. The bond lengths in the crystal structure are shown in Table 2 below, the bond angles in the crystal structure and Table 3 below.
表1Sr2B16O26的晶体结构数据Table 1 Crystal structure data of Sr 2 B 16 O 26
表2.Sr2B16O26晶体中的键长(A°)Table 2. Bond lengths in Sr 2 B 16 O 26 crystals (A°)
表3Sr2B16O26晶体中的键角(°)Table 3 Bond angles in Sr 2 B 16 O 26 crystals (°)
需要强调的是化合物表现出了一些干扰信息，为了判断产物是否为我们的目标化合物，对Sr2B16O26中的原子参数进行精修，B2和O26都与理论值很好的吻合，确定了化合物Sr2B16O26。It should be emphasized that the compound shows some interference information. In order to judge whether the product is our target compound, the atomic parameters in Sr 2 B 16 O 26 are refined, and both B 2 and O 26 are in good agreement with the theoretical values. , and identified the compound Sr 2 B 16 O 26 .
本发明不局限于上述具体的实施方式，本领域的普通技术人员从上述构思出发，不经过创造性的劳动，所作出的种种变换，均落在本发明的保护范围之内。The present invention is not limited to the above-mentioned specific implementation manners, and various transformations made by those skilled in the art starting from the above-mentioned concept without creative work all fall within the protection scope of the present invention.
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Citations (2)
| 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 |
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| 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)
| 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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