CN103044492A - Ferroelectric organometallic compound, as well as preparation method and application thereof - Google Patents
Ferroelectric organometallic compound, as well as preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 150000002902 organometallic compounds Chemical class 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims description 31
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 10
- 125000002524 organometallic group Chemical group 0.000 claims description 9
- 229940011182 cobalt acetate Drugs 0.000 claims description 8
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
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- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 101100233056 Caenorhabditis elegans ima-2 gene Proteins 0.000 abstract description 2
- 238000003491 array Methods 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 1
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- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及一种铁电材料有机金属配合物及其制备方法与应用。 The invention relates to a ferroelectric material organometallic complex and a preparation method and application thereof.
背景技术 Background technique
铁电材料是一种同时具有铁电、压电、热释电、电光、非线性光学等性能的多功能材料。所谓铁电材料，是指晶体结构在不加外电场时就具有自发极化现象，其自发极化的方向能够被外加电场反转或重新定向的材料。材料的这种特性被称为“铁电现象”或“铁电效应”。近些年来，铁电材料发展极为迅速，已广泛应用于电子技术、激光技术、红外探测技术、超声（和微波声学）技术、固态记忆和显示技术以及其他工程技术方面，而研制和生产性能优良的铁电材料，又是发展各种铁电、压电、热电和电光等功能器件的基础。因此，目前国际上对铁电材料的研制和探索十分活跃。 Ferroelectric material is a kind of multifunctional material with properties of ferroelectricity, piezoelectricity, pyroelectricity, electro-optic and nonlinear optics at the same time. The so-called ferroelectric material refers to a material whose crystal structure has spontaneous polarization when no external electric field is applied, and the direction of its spontaneous polarization can be reversed or reoriented by an external electric field. This property of the material is known as "ferroelectricity" or "ferroelectric effect". In recent years, ferroelectric materials have developed extremely rapidly and have been widely used in electronic technology, laser technology, infrared detection technology, ultrasonic (and microwave acoustics) technology, solid-state memory and display technology, and other engineering technologies, and their development and production performance are excellent. Ferroelectric materials are the basis for the development of various functional devices such as ferroelectrics, piezoelectrics, pyroelectrics, and electro-optics. Therefore, the development and exploration of ferroelectric materials are very active in the world at present.
目前人们对铁电材料的研究和应用主要集中在无机材料上。无机铁电材料由于具有高强度、高硬度、耐高温、性能长期稳定、使用寿命长等优点而被广泛应用，但是由于无机铁电薄膜的制作需要高真空较高温度的条件，使制作成本较为昂贵，不易制作大面积薄膜且需要采用硬质材料作基片，较大地限制了其应用。近年来，有机铁电体薄膜也倍受青睐，主要是由于与无机铁电材料相比，其具有易制成大面积薄膜、制作成本低、低温制作条件、相对大的分子超极化率、大的电致伸缩应变能力、与空气的抗声阻匹配性有独特的优越性等优点，同时由于其低温制作条件而可以用柔软的塑料作基片。但是由于有机铁电材料的铁电耦合系数较低，相对介电常数较小，性能、功能的长期稳定性相对差一些，从而使其应用受到较大限制。因此，研究新型铁电材料以克服无机或有机铁电材料的固有缺陷已成为当前铁电材料的研究重点。 At present, the research and application of ferroelectric materials are mainly concentrated on inorganic materials. Inorganic ferroelectric materials are widely used due to their advantages of high strength, high hardness, high temperature resistance, long-term stable performance, and long service life. However, since the production of inorganic ferroelectric thin films requires high vacuum and high temperature conditions, the production cost is relatively Expensive, difficult to make large-area thin films and requires hard materials as substrates, which greatly limits its application. In recent years, organic ferroelectric thin films are also favored, mainly because compared with inorganic ferroelectric materials, they are easy to make large-area thin films, low manufacturing cost, low temperature manufacturing conditions, relatively large molecular hyperpolarizability, It has the advantages of large electrostrictive strain capacity and unique superiority in anti-acoustic resistance matching with air. At the same time, it can use soft plastic as the substrate due to its low-temperature manufacturing conditions. However, due to the low ferroelectric coupling coefficient and small relative permittivity of organic ferroelectric materials, the long-term stability of performance and function is relatively poor, which greatly limits their application. Therefore, the study of new ferroelectric materials to overcome the inherent defects of inorganic or organic ferroelectric materials has become the current research focus of ferroelectric materials.
近几年来，具有铁电效应的有机模板金属硼磷酸盐引起了人们的极大研究兴趣，这是由于这类杂化材料经过精心设计和调控，可以达到扬无机材料和有机材料各自优点之长和避其缺点之短的“杂交优势”的效果，而且无机硼氧金属骨架和有机模板组份之间的相互作用，可以使此类材料呈现出新颖的性质。 In recent years, organic template metal borophosphates with ferroelectric effect have attracted great research interest, because this kind of hybrid materials can achieve the advantages of inorganic materials and organic materials through careful design and regulation. The effect of "hybrid vigor" and the shortcoming of avoiding its shortcoming, and the interaction between the inorganic boron metal oxide framework and the organic template component can make this kind of material exhibit novel properties.
发明内容 Contents of the invention
本发明的目的就在于提供一种铁电材料有机金属配合物及其制备方法与应用，其技术方案如下： The object of the present invention is just to provide a kind of ferroelectric material organometallic complex and its preparation method and application, and its technical scheme is as follows:
本发明提供的一种铁电材料有机金属配合物，该配合物分子式为C4H13N2B2P3CoO13，空间群为Ima2 (No.46)，单胞参数为a = 12.4820 (8) ?, b = 9.4146 (3) ?, c = 11.4646 (2) ?,α= β=γ = 90.00 o, Z = 4, 单胞体积V =1347.2(1) ?3。 The present invention provides a ferroelectric material organometallic complex, the molecular formula of which is C 4 H 13 N 2 B 2 P 3 CoO 13 , the space group is Im a2 (No.46), and the unit cell parameter is a = 12.4820 (8) ?, b = 9.4146 (3) ?, c = 11.4646 (2) ?, α = β = γ = 90.00 o, Z = 4, unit cell volume V =1347.2(1) 3 .
本发明还提供一种铁电材料有机金属配合物的制备方法，在水热条件下，反应物乙酸钴（Co(CH3COO)2）、硼酸（H3BO3）、哌嗪(C4H10N2)、磷酸(H3PO4)作为原料，其摩尔比为0.5～5：1～3：0.5～3：1.5～6，采用水作为溶剂，水热反应升温至140～220℃，室温下自然冷却，得到C4H13N2B2P3CoO13。 The present invention also provides a method for preparing a ferroelectric material organometallic complex. Under hydrothermal conditions, the reactants cobalt acetate (Co(CH 3 COO) 2 ), boric acid (H 3 BO 3 ), piperazine (C 4 H 10 N 2 ), phosphoric acid (H 3 PO 4 ) as raw materials, the molar ratio is 0.5~5:1~3:0.5~3:1.5~6, water is used as solvent, and the temperature of hydrothermal reaction is raised to 140~220℃ , and naturally cooled at room temperature to obtain C 4 H 13 N 2 B 2 P 3 CoO 13 .
上述乙酸钴被同物质量的六水合硝酸钴、硝酸钴、硫酸钴或氯化钴取代。 The above-mentioned cobalt acetate is replaced by cobalt nitrate hexahydrate, cobalt nitrate, cobalt sulfate or cobalt chloride of the same substance amount.
本发明还提供一种铁电材料有机金属配合物的用途，该材料应用于存储和恢复信息、传输光信息、图像显示或全息照像中的编页器、铁电光阀阵列作全息照像的存储。 The present invention also provides the use of a ferroelectric material organometallic complex, which is used in storage and recovery of information, transmission of optical information, image display or holographic pagers, ferroelectric light valve arrays for holographic imaging storage.
我们选择乙酸钴（Co(CH3COO)2）、硼酸（H3BO3）、哌嗪(C4H10N2)、磷酸(H3PO4)作为原料，其摩尔比为0.5～2.5：1.5～2.5：0.5～1.5：1.5～4.5，采用水作为溶剂，在水热反应条件下，硼酸、乙酸钴、哌嗪和磷酸发生化学反应，生长了有机模板金属钴硼磷酸盐的单晶。 We choose cobalt acetate (Co(CH 3 COO) 2 ), boric acid (H 3 BO 3 ), piperazine (C 4 H 10 N 2 ), phosphoric acid (H 3 PO 4 ) as raw materials, and the molar ratio is 0.5-2.5 : 1.5 ~ 2.5: 0.5 ~ 1.5: 1.5 ~ 4.5, using water as a solvent, under hydrothermal reaction conditions, boric acid, cobalt acetate, piperazine and phosphoric acid react chemically to grow a single crystal of organic template metal cobalt borophosphate .
我们测得该有机模板金属钴硼磷酸盐的晶体结构，结构参数如下： We measured the crystal structure of the organic template metal cobalt borophosphate, and the structural parameters are as follows:
分子式为C4H13N2B2P3CoO13，空间群为Ima2 (No.46)，单胞参数为a = 12.4820 (8) ?, b = 9.4146 (3) ?, c = 11.4646 (2) ?,α= β=γ = 90.00 o, Z = 4, 单胞体积V =1347.2(1) ?3。 The molecular formula is C 4 H 13 N 2 B 2 P 3 CoO 13 , the space group is Ima2 (No.46), and the unit cell parameters are a = 12.4820 (8) ?, b = 9.4146 (3) ?, c = 11.4646 (2 ) ?, α = β = γ = 90.00 o, Z = 4, unit cell volume V =1347.2(1) 3 .
该材料的优点是不易溶于一般的溶剂，热分解温度点高（空气氛中可以稳定到250 oC），晶体颗粒均匀。 The advantage of this material is that it is not easily soluble in common solvents, its thermal decomposition temperature is high (it can be stable to 250 o C in air atmosphere), and its crystal particles are uniform.
本发明的有益效果：Beneficial effects of the present invention:
本发明提供的有机模板金属钴硼磷酸盐是在溶剂热合成方法生长出的晶体。所采用的材料制备工艺简单、产率高及重复性好。 The organic template metal cobalt borophosphate provided by the invention is a crystal grown by a solvothermal synthesis method. The material preparation process adopted is simple, the yield is high and the repeatability is good.
该材料的优点是自发极化通过氢键产生，极化模式稳定，具有较好的应用价值。 The advantage of this material is that the spontaneous polarization is generated through hydrogen bonds, the polarization mode is stable, and it has good application value.
该材料具有的重要铁电特性为：在室温下其电致曲线的Pr＝0.029μC/cm2，Ps＝0.055μC/cm2，但是随着外界的温度逐渐的升高，其自发极化率Ps和残余极化率可以会相应的减弱，这种随温度变化导致的铁电性质变化，有可能被利用到一些新型的电子、激光或红外探测电子器件上。这种特性具有在已知的铁电体中并不常见。 The important ferroelectric properties of this material are: Pr=0.029μC/cm 2 and Ps=0.055μC/cm 2 of its electric curve at room temperature, but as the external temperature gradually increases, its spontaneous polarizability Ps and remnant polarizability can be correspondingly weakened. This ferroelectric property change with temperature change may be used in some new electronic, laser or infrared detection electronic devices. Such properties are unusual among known ferroelectrics.
具体实施方式 Detailed ways
1、 化合物的制备1. Preparation of compounds
称取乙酸钴（Co(CH3COO)2）0.088到0.880g，硼酸（H3BO3）0.062到0.186g，哌嗪(C4H10N2) 0.048到0.258，量取0.18到0.72ml磷酸水溶液(H3PO4，质量浓度85%)，水（H2O）3.0到9.0ml，其摩尔比为0.5～5：1～3：0.5～3：1.5～6：16～50，搅拌20min，装入密闭的28 mL的反应釜中，升温至140～220 ℃，恒温1到7天，取出后在室温条件下自然冷却，便可得到晶体。经X射线单晶衍射分析，确定该晶体为C4H13N2B2P3CoO13。乙酸钴被同物质量的六水合硝酸钴、硝酸钴、硫酸钴或氯化钴取代，可以得到相同的C4H13N2B2P3CoO13化合物。 Weigh 0.088 to 0.880g of cobalt acetate (Co(CH 3 COO) 2 ), 0.062 to 0.186g of boric acid (H 3 BO 3 ), 0.048 to 0.258 of piperazine (C 4 H 10 N 2 ), and weigh 0.18 to 0.72ml Phosphoric acid aqueous solution (H 3 PO 4 , mass concentration 85%), water (H 2 O) 3.0 to 9.0ml, the molar ratio is 0.5～5:1～3:0.5～3:1.5～6:16～50, stirring After 20 minutes, put it into a closed 28 mL reaction kettle, raise the temperature to 140-220 ℃, keep the temperature for 1-7 days, take it out and let it cool naturally at room temperature to obtain crystals. X-ray single crystal diffraction analysis confirmed that the crystal was C 4 H 13 N 2 B 2 P 3 CoO 13 . Cobalt acetate is replaced by the same amount of cobalt nitrate hexahydrate, cobalt nitrate, cobalt sulfate or cobalt chloride, and the same C 4 H 13 N 2 B 2 P 3 CoO 13 compound can be obtained.
具体反应物实施实例如下： Concrete reactant implementation example is as follows:
（1）Co：H3BO3：C4H10N2：H3PO4：H2O＝0.5：1：0.5：1.5：16， (1) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=0.5:1:0.5:1.5:16,
（2）Co：H3BO3：C4H10N2：H3PO4：H2O＝2：2：1：4：35， (2) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=2:2:1:4:35,
（3）Co：H3BO3：C4H10N2：H3PO4：H2O＝0.5：3：3：6：50， (3) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=0.5:3:3:6:50,
（4）Co：H3BO3：C4H10N2：H3PO4：H2O＝1：3：2：3：40， (4) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=1:3:2:3:40,
（5）Co：H3BO3：C4H10N2：H3PO4：H2O＝0.5：3：3：6：16， (5) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=0.5:3:3:6:16,
（6）Co：H3BO3：C4H10N2：H3PO4：H2O＝5：1：3：6：16， (6) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=5:1:3:6:16,
（7）Co：H3BO3：C4H10N2：H3PO4：H2O＝0.5：1：0.5：6：16， (7) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=0.5:1:0.5:6:16,
（8）Co：H3BO3：C4H10N2：H3PO4：H2O＝0.5：3：0.5： 6：50， (8) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=0.5:3:0.5:6:50,
（9）Co：H3BO3：C4H10N2：H3PO4：H2O＝5：3：3：6：16， (9) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=5:3:3:6:16,
（10）Co：H3BO3：C4H10N2：H3PO4：H2O＝5：3：0.5：1.5：16， (10) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=5:3:0.5:1.5:16,
（11）Co：H3BO3：C4H10N2：H3PO4：H2O＝3：2：3：5：45， (11) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=3:2:3:5:45,
（12）Co：H3BO3：C4H10N2：H3PO4：H2O＝5：1：3：6：50， (12) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O=5:1:3:6:50,
（13）Co：H3BO3：C4H10N2：H3PO4：H2O＝5：1：0.5：1.5：50。 (13) Co: H 3 BO 3 : C 4 H 10 N 2 : H 3 PO 4 : H 2 O = 5:1:0.5:1.5:50.
2、结构解析2. Structure analysis
选取合适尺寸的无色颗粒状单晶，用Siemens Smart CCD衍射仪在293（±2）K下使用经石墨单色化的Mo Kα射线(λ=0.071073 nm)收集衍射强度数据。原始数据用ABSOR程序进行吸收校正，采用直接法确定晶体的初始结构模型。最后，用差值傅立叶分析和最小二乘法来扩充初始模型，并对所有非氢原子的位置及各向异性温度因子进行精修（SHELXTL-97）。结果表明，分子式为C4H13N2B2P3CoO13，空间群为Ima2 (No.46)，单胞参数为a = 12.4820 (8) ?, b = 9.4146 (3) ?, c = 11.4646 (2) ?,α= β=γ = 90.00 o, Z = 4, V =1347.2(1) ?3。 Select a colorless granular single crystal with a suitable size, and use a Siemens Smart CCD diffractometer at 293 (±2) K to collect diffraction intensity data using Mo Kα rays (λ=0.071073 nm) monochromated by graphite. The raw data were corrected for absorption with the program ABSOR, and the initial structure model of the crystal was determined by the direct method. Finally, the initial model was augmented with difference Fourier analysis and least squares and refined for all non-hydrogen atom positions and anisotropy temperature factors (SHELXTL-97). The results show that the molecular formula is C 4 H 13 N 2 B 2 P 3 CoO 13 , the space group is Im a2 (No.46), and the unit cell parameters are a = 12.4820 (8) ?, b = 9.4146 (3) ?, c = 11.4646(2) ?, α = β = γ = 90.00o, Z = 4, V =1347.2(1) 3 .
3、性能测试 3. Performance test
选取适量的样品，在压片机下加工为厚度0.6mm圆形待测样品，在压片的上下两侧，涂上导电银胶。然后在aix-ACCT TF2000铁电测试仪上进行测试。我们对得到的有机模板金属钴硼磷酸盐进行研究发现：该配合物的极化强度P与外施电场强度E的关系曲线表明具有明显的铁电效应，Pr＝0.029μC/cm2，Ps＝0.055μC/cm2。变温极化曲线按照每升高10K，记录一次电致曲线。可观察到明显的Pr与Ps值，随温度变化而逐渐的降低。 Select an appropriate amount of sample, and process it into a circular sample with a thickness of 0.6mm under the tablet press, and coat the upper and lower sides of the tablet with conductive silver glue. Then test on aix-ACCT TF2000 ferroelectric tester. We researched the obtained organic template metal cobalt boron phosphate and found that: the relationship curve between the polarization intensity P and the applied electric field intensity E of the complex shows obvious ferroelectric effect, Pr=0.029μC/cm 2 , Ps= 0.055 μC/cm 2 . The temperature-changing polarization curve was recorded according to every 10K increase, and the electric induction curve was recorded once. Obvious Pr and Ps values can be observed, which gradually decrease with temperature changes.
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| CN109659570A (en) * | 2019-01-09 | 2019-04-19 | 长江大学 | The application of the metal organic framework compound hollow microsphere of load iron cobalt sulfide |
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