Synthesis method of tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal
阅读说明：本技术 四方平板状的(C6H5CH2CH2NH3)2MnCl4微纳单晶的合成方法 (Synthesis method of tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal ) 是由 马德伟 于 2019-09-25 设计创作，主要内容包括：一种四方平板状的(C_6H_5CH_2CH_2NH_3)_2MnCl_4微纳单晶的溶液化学合成方法,包括以下步骤：(1)称取设定量的PbAc_2粉末,溶于水溶液中,然后采用滴涂法在玻璃或硅片衬底上制成PbAc_2预沉积薄膜；(2)称取设定量的C_6H_5CH_2CH_2NH_3Cl粉末,溶于异丙醇中,得C_6H_5CH_2CH_2NH_3Cl有机先驱体溶液；(3)待PbAc_2预沉积薄膜干燥后,将薄膜浸于C_6H_5CH_2CH_2NH_3Cl/异丙醇溶液中1小时以上取出,最终在衬底片上生成四方平板状的(C_6H_5CH_2CH_2NH_3)_2MnCl_4微纳单晶。本发明不需要真空、高温以及复杂昂贵的设备,反应在空气中、室温条件下即可进行,工艺简单,成本低廉。(A chemical synthesis method of a tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3 ) 2 MnCl 4 micro-nano monocrystal solution comprises the following steps of (1) weighing a set amount of PbAc 2 powder, dissolving the PbAc 2 powder in an aqueous solution, preparing a PbAc 2 pre-deposited film on a glass or silicon wafer substrate by adopting a drop coating method, (2) weighing a set amount of C 6 H 5 CH 2 CH 2 NH 3 Cl powder, dissolving the C 6 H 5 CH 2 CH 2 NH 3 Cl organic precursor solution, soaking the film in a C 6 H 5 CH 2 CH 2 NH 3 Cl/isopropanol solution for more than 1 hour after the PbAc 2 pre-deposited film is dried, taking out, and finally generating the tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3 ) 2 MnCl 4 micro-nano monocrystal on a substrate sheet without needing vacuum, high temperature and complicated reaction equipment, and low reaction cost and simple process at room temperature.)
1. A solution chemical synthesis method of tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal is characterized in that PbAc 2 and C 6 H 5 CH 2 CH 2 NH 3 Cl are respectively used as precursors of Pb and Cl, and two-step solution chemical synthesis is adopted, and the method comprises the following steps:
(1) weighing PbAc 2 powder with a set amount, dissolving the PbAc 2 powder in an aqueous solution, and preparing a PbAc 2 pre-deposited film on a glass or silicon wafer substrate by adopting a dripping method;
(2) Weighing a set amount of C 6 H 5 CH 2 CH 2 NH 3 Cl powder, and dissolving the powder in isopropanol to obtain C 6 H 5 CH 2 CH 2 NH 3 Cl organic precursor solution;
(3) After the PbAc 2 pre-deposited film is dried, the film is soaked in a C 6 H 5 CH 2 CH 2 NH 3 Cl/isopropanol solution for more than 1 hour and taken out, and finally, tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal is generated on a substrate sheet.
2. The method for the chemical synthesis of a tetragonal flat plate (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro nano single crystal according to claim 1, wherein lead acetate is used as a Pb source, C 6 H 5 CH 2 CH 2 NH 3 Cl is used as an organic precursor, water is used as a solvent for the lead acetate, and isopropanol is used as a solvent for C 6 H 5 CH 2 CH 2 NH 3 Cl.
3. the solution chemical synthesis method of tetragonal flat plate-like (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro nano single crystal according to claim 1 or 2, characterized in that when preparing the lead acetate aqueous solution, the concentration of the lead acetate in the aqueous solution is 50-150 mg/mL.
4. The solution chemical synthesis method of tetragonal flat plate-like (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro nano single crystal according to claim 1 or 2, characterized in that when a C 6 H 5 CH 2 CH 2 NH 3 Cl solution is prepared, the concentration of C 6 H 5 CH 2 CH 2 NH 3 Cl/isopropanol is 10-80 mg/mL.
5. The solution chemical synthesis method of tetragonal flat plate-like (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro nano single crystals according to claim 1 or 2, wherein the generated tetragonal flat plate-like micro nano single crystals have the advantages of large quantity, controllable appearance, smooth surface and 1-30 μm size.
Technical Field
The invention relates to the field of nano material preparation, in particular to a liquid phase synthesis method of a nano crystal for a micro-nano magnetoelectric and magneto-optical device.
background
Organic/inorganic perovskite materials have been the focus of research worldwide due to their broad application prospects in photovoltaic devices such as solar cells, Light Emitting Diodes (LEDs) and the like, in addition, perovskite structures have attracted considerable attention as multiferroic materials, for example, two-dimensional layered perovskite structures (RNH 3) 2 MX 4 (RNH 3 ═ organic chain amine or aromatic amine; M ═ Cu 2+, Cr 2+, Fe 2+, Mn 2+; X ═ Cl - , Br - ) are a class of important quasi-two-dimensional hesenberg ferromagnetic materials, which induce a series of ferroelectric, ferroelectric and ferromagnetic phase transitions under the drive of temperature, light, electromagnetic field, mechanical force and the like, such phenomena as reorientation of organic amine groups and tilt of [ MX ] 6 octahedrons, on the one hand, such structures enrich the electronic properties of two-dimensional materials, and provide a basis for the research of novel quantum phenomena.
The (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 belongs to an orthorhombic system, the space group is P bca, the unit cell parameters a 7.2075, b 7.3012, C39.413 a °, it is a two-dimensional antiferromagnetic material, and has weak ferromagnetism below the critical temperature T C K44.3K, the change of the magnetic susceptibility depends on different crystal orientations, external magnetic fields and magnetization processes, etc. the document reports that (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 bulk crystals are synthesized by a common slow evaporation method and a supersaturated solution cooling method.
disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a solution chemical synthesis method of a tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal, which does not need vacuum, high temperature, complex and expensive equipment, can be carried out in the air at room temperature, and has simple process and low cost.
The technical scheme adopted by the invention for solving the problems is as follows:
A solution chemical synthesis method of tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal takes PbAc 2 and C 6 H 5 CH 2 CH 2 NH 3 Cl as precursors of Pb and Cl respectively and adopts two-step solution chemical synthesis, and the method comprises the following steps:
(1) weighing PbAc 2 powder with a set amount, dissolving the PbAc 2 powder in an aqueous solution, and preparing a PbAc 2 pre-deposited film on a glass or silicon wafer substrate by adopting a dripping method;
(2) Weighing a set amount of C 6 H 5 CH 2 CH 2 NH 3 Cl powder, and dissolving the powder in isopropanol to obtain C 6 H 5 CH 2 CH 2 NH 3 Cl organic precursor solution;
(3) After the PbAc 2 pre-deposited film is dried, the film is soaked in a C 6 H 5 CH 2 CH 2 NH 3 Cl/isopropanol solution for more than 1 hour and taken out, and finally, tetragonal flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal is generated on a substrate sheet.
Further, lead acetate was used as a Pb source, C 6 H 5 CH 2 CH 2 NH 3 Cl was used as an organic precursor, water was used as a solvent for lead acetate, and isopropyl alcohol was used as a solvent for C 6 H 5 CH 2 CH 2 NH 3 Cl.
And further, when preparing the lead acetate aqueous solution, the concentration of the lead acetate in the aqueous solution is 50-150 mg/mL.
Furthermore, when a solution of C 6 H 5 CH 2 CH 2 NH 3 Cl is prepared, the concentration of C 6 H 5 CH 2 CH 2 NH 3 Cl/isopropanol is 10-80 mg/mL.
The generated square flat micro-nano single crystals are large in quantity, controllable in appearance, smooth in surface and 1-30 mu m in size.
The method has the beneficial effects that the synthesis process can be carried out in the air at room temperature, and the preparation process is simple, convenient to operate and low in cost, so that the method provides an important method for synthesizing the square flat plate-shaped (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 micro-nano single crystal.
Drawings
FIG. 1 is a typical XRD pattern of (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 synthesized by the present invention.
FIG. 2 is a typical SEM image of (C 6 H 5 CH 2 CH 2 NH 3) 2 MnCl 4 synthesized by the present invention.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
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