阅读说明：本技术 一种羟基氯化锌超薄纳米片及其制备方法 (Zinc hydroxychloride ultrathin nanosheet and preparation method thereof ) 是由 张剑 魏子钦 罗亚肖 王美玲 赵悦 田辉 崔啟良 于 2019-09-02 设计创作，主要内容包括：本发明的一种羟基氯化锌超薄纳米片及其制备方法,属于IIB族羟基氯化物纳米材料制备的技术领域。所述的羟基氯化锌超薄纳米片,是以化学计量数为5:8:2的比例构成的化合物Zn<Sub>5</Sub>(OH)<Sub>8</Sub>Cl<Sub>2</Sub>,是正交系晶体,空间群为Pcab；具有层状纳米片结构,纳米片边长为200～3000nm,厚度约为4.0～7.9nm。其制备方法为,首先将氯化锌固体颗粒加入异丙醇或丙醇中,搅拌60分钟、超声30分钟,重复2～3次,将得到的悬浊液离心后用无水乙醇再离心清洗3次后烘干、研磨。本发明操作简单、重复性好、成本低廉、反应物毒性小；制备出的Zn<Sub>5</Sub>(OH)<Sub>8</Sub>Cl<Sub>2</Sub>纳米片的产量高、纯度高,室温环境下能够长时间稳定存放不变性。(The invention discloses a zinc hydroxychloride ultrathin nanosheet and a preparation method thereof, and belongs to the technical field of preparation of IIB family hydroxychloride nanomaterials. The hydroxyl zinc chloride ultrathin nano-sheet is a compound Zn formed by a stoichiometric number of 5:8:2 5 (OH) 8 Cl 2 Is an orthorhombic crystal, and has a space group of Pcap; the nano-sheet has a layered nano-sheet structure, wherein the side length of the nano-sheet is 200-3000 nm, and the thickness of the nano-sheet is about 4.0-7.9 nm. The preparation method comprises the steps of firstly adding zinc chloride solid particles into isopropanol or propanol, stirring for 60 minutes, carrying out ultrasonic treatment for 30 minutes, repeating for 2-3 times, centrifuging the obtained suspension, then carrying out centrifugal cleaning for 3 times by using absolute ethyl alcohol, drying and grinding. The method has the advantages of simple operation, good repeatability, low cost and low toxicity of reactants; prepared Zn 5 (OH) 8 Cl 2 The nano-sheet has high yield and high purity, and can be stably stored for a long time without denaturation in a room temperature environment.)

1. An ultrathin zinc hydroxychloride nanosheet, which is a compound Zn consisting of a stoichiometric number of 5:8:2₅(OH)₈Cl₂Is an orthorhombic crystal, and has a space group of Pcap; utensil for cleaning buttockThe nano-sheet has a layered nano-sheet structure, wherein the side length of the nano-sheet is 200-3000 nm, and the thickness of the nano-sheet is about 4.0-7.9 nm.

2. A preparation method of zinc hydroxychloride ultrathin nanosheets as claimed in claim 1, comprising the steps of taking zinc chloride solid particles and isopropanol or propanol as raw materials, firstly adding the zinc chloride solid particles into the isopropanol or propanol, wherein the mass-to-volume ratio of the zinc chloride to the isopropanol or propanol is 0.5-2 g:15 mL; stirring in a magnetic stirrer for 60 minutes, then putting the mixed solution into an ultrasonic machine for ultrasonic treatment for 30 minutes, and repeating the whole stirring and ultrasonic treatment process for 2-3 times to obtain a suspension; centrifuging the suspension to obtain white precipitate, centrifuging and cleaning the white precipitate with anhydrous ethanol for 3 times, drying, and grinding to obtain zinc hydroxychloride Zn₅(OH)₈Cl₂An ultrathin nanosheet.

3. The method for preparing ultrathin zinc hydroxychloride nanosheets as in claim 2, wherein the starting materials are solid particles of zinc chloride and isopropanol.

4. The preparation method of ultrathin zinc hydroxychloride nanosheets as recited in claim 3, wherein the mass to volume ratio of the solid particles of zinc chloride to isopropanol is 1g:15 mL.

5. The method for preparing ultrathin zinc hydroxychloride nanosheets as in claim 2, wherein the drying is at 80 ℃ for 8 hours.

Technical Field

The invention belongs to the technical field of IIB family hydroxychloride nano material preparation, and particularly relates to a simple, novel and efficient method for preparing a zinc hydroxychloride nanosheet.

Background

The research of two-dimensional materials has been rapidly developed in recent years. The novel two-dimensional nano material represented by graphene has a unique structure and excellent electronic characteristics, and has great application potential in various electrochemical fields. In addition, the two-dimensional material has been widely applied in the fields of optics, magnetics, high-density materials and the like. Therefore, the preparation of the novel two-dimensional nano material and the exploration of the novel preparation method of the two-dimensional nano flaky structure material have important research significance for the exploration in the nano field.

With the continuous progress and development of scientific research, research on the properties of metal hydroxyhalides and synthesis methods is receiving attention, and at present, the synthesis methods of these compounds generally adopt an electrodeposition method and a hydrothermal method. According to the related report, the zinc hydroxychloride forms a compound Zn according to the perfect proportion that zinc, hydroxyl and chlorine are respectively 5:8:2 stoichiometric numbers₅(OH)₈Cl₂Belongs to an orthorhombic system, is hexagonal and flaky, and has a nanosheet side length of 0.1-100 μm. Penhongxing and the like research the synthesis process conditions of basic zinc chloride by using liquid zinc chloride and liquid sodium hydroxide as raw materials; the yellow intelligence source and the subject group members thereof explore a method capable of recovering Zn from brass slag to prepare basic zinc chloride; the preparation and electrical property conditions of the composite material of the zinc hydroxychloride and the graphene are introduced in the reports of the excellent semiconductor property of the zinc hydroxychloride and the outstanding conductivity and mechanical property of the graphene.

The existing published method for preparing zinc hydroxychloride has the limitations of long reaction time, complex and fussy process, strict requirements on reaction conditions, unstable chemical properties, complex and expensive synthetic reactants, difficult storage of products and the like, and the prepared zinc hydroxychloride nanosheet is thick and about 20nm-20 mu m in thickness. Thinner zinc hydroxychloride nanosheets and methods of making the same have been reported.

Disclosure of Invention

The invention aims to solve the technical problem of providing zinc hydroxychloride (Zn) for overcoming the defects in the prior art₅(OH)₈Cl₂) Ultrathin nanosheets and a preparation method thereof.

The specific technical scheme is as follows:

An ultrathin zinc hydroxychloride nanosheet, which is a compound Zn consisting of a stoichiometric number of 5:8:2₅(OH)₈Cl₂Is an orthorhombic crystal, and has a space group of Pcap; the nano-sheet has a layered nano-sheet structure, wherein the side length of the nano-sheet is 200-3000 nm, and the thickness of the nano-sheet is about 4.0-7.9 nm.

A preparation method of a zinc hydroxychloride ultrathin nanosheet comprises the steps of taking zinc chloride solid particles and isopropanol or propanol as raw materials, firstly adding the zinc chloride solid particles into the isopropanol or propanol, wherein the mass-volume ratio of zinc chloride to the isopropanol or propanol is 0.5-2 g:15 mL; stirring in a magnetic stirrer for 60 minutes, then putting the mixed solution into an ultrasonic machine for ultrasonic treatment for 30 minutes, and repeating the whole stirring and ultrasonic treatment process for 2-3 times to obtain a suspension; centrifuging the suspension to obtain white precipitate, centrifuging and cleaning the white precipitate with anhydrous ethanol for 3 times, oven drying, and grinding to obtain zinc hydroxychloride (Zn)₅(OH)₈Cl₂) An ultrathin nanosheet.

In the preparation method of the zinc hydroxychloride ultrathin nanosheet, the raw materials are preferably zinc chloride solid particles and isopropanol, the mass-to-volume ratio is preferably 1g:15mL, and the drying condition is preferably drying for 8 hours at 80 ℃.

Has the advantages that:

The invention synthesizes hydroxyl zinc chloride (Zn) for the first time₅(OH)₈Cl₂) An ultrathin nanosheet structure; the side length of the nanosheet is 200-3000 nm, the thickness of the nanosheet is about 4.0-7.9nm, and the nanosheet is regular in shape and smooth in surfaceNo defect and uniform size. The method overcomes many limitations, breaks through the condition that the sample must be prepared at high temperature and high pressure in the past, can be prepared by reaction at room temperature, and has the advantages of simple operation, good repeatability, low cost and little toxicity of reactants; prepared Zn₅(OH)₈Cl₂The nanosheet has high yield and high purity, can be stably stored for a long time without denaturation in a room temperature environment, and lays a foundation for further research on application of hydroxyhalide.

Drawings

FIG. 1 shows Zn obtained in example 1₅(OH)₈Cl₂EDX picture of nanoplates.

FIG. 2 shows Zn obtained in example 1₅(OH)₈Cl₂XRD spectrogram of the nanosheet.

FIG. 3 shows Zn obtained in example 1₅(OH)₈Cl₂SEM image of nanoplatelets.

FIG. 4 shows Zn obtained in example 1₅(OH)₈Cl₂SEM image of nanoplatelets.

FIG. 5 shows Zn obtained in example 1₅(OH)₈Cl₂TEM images of the nanoplates.

FIG. 6 shows Zn obtained in example 1₅(OH)₈Cl₂TEM images of the nanoplates.

FIG. 7 shows Zn obtained in example 1₅(OH)₈Cl₂TEM images of the nanoplates.

FIG. 8 shows Zn obtained in example 1₅(OH)₈Cl₂TEM images of the nanoplates.

FIG. 9 shows Zn obtained in example 1₅(OH)₈Cl₂Electron diffraction pattern of nanoplatelets.

FIG. 10 shows Zn obtained in example 2₅(OH)₈Cl₂XRD spectrogram of the nanosheet.

FIG. 11 shows Zn obtained in example 3₅(OH)₈Cl₂SEM image of nanoplatelets.

FIG. 12 shows Zn obtained in example 4₅(OH)₈Cl₂SEM image of nanoplatelets.

Figure 13 is an XRD spectrum of the sample prepared in example 5.

Figure 14 is an XRD spectrum of the sample prepared in example 6.

Figure 15 is the XRD spectrum of the sample prepared in example 7.

Figure 16 is the XRD spectrum of the sample prepared in example 8.

figure 17 is the XRD spectrum of the sample prepared in example 9.

Detailed Description