阅读说明：本技术 一种氧化铟钙纳米片材料及制备方法 (Indium calcium oxide nanosheet material and preparation method thereof ) 是由 封伟 王宇 冯奕钰 赵付来 张鑫 梁雪静 于 2019-10-18 设计创作，主要内容包括：本发明公开一种氧化铟钙纳米片材料及制备方法,将Ca、In、P按化学计量比封装在在管式炉中进行程序控温得到前驱体,将得到的前驱体与水在低于室温下进行反应,即可得到氧化铟钙纳米片。本发明的方法步骤简单,材料产量大,具有纳米片结构,且组成不同于已知结构,在光电器件、光催化、储能等方面具有较大的潜在应用。(The invention discloses an indium calcium oxide nanosheet material and a preparation method thereof. The method has the advantages of simple steps, high material yield, nanosheet structure, composition different from the known structure, and great potential application in the aspects of photoelectric devices, photocatalysis, energy storage and the like.)

1. An indium calcium oxide nanosheet material, characterized by being prepared according to the following steps: mixing Ca, In and P according to the proportion of 1: 2: 2, weighing the materials according to the molar ratio, sequentially adding the materials into a quartz tube, carrying out vacuum packaging, heating and sintering in a tube furnace under an inert protective atmosphere, carrying out melting and cooling to obtain a precursor, and reacting the obtained precursor with water to obtain the indium oxide calcium nanosheet material, wherein: raising the temperature to 950-; the mass ratio of the precursor to the water is 1: (100-200).

2. The indium calcium oxide nanosheet material of claim 1, wherein the inert protective atmosphere is nitrogen, helium or argon.

3. The ITO nanosheet material of claim 1, wherein the temperature is raised from 20-25 ℃ to 980-1030 ℃ within 300 ± 10min, the temperature is maintained for 1200-1400 min, and then the temperature is lowered to 20-25 ℃ at 5-10 ℃/min.

4. An ito nanoplatelet according to claim 1 wherein the reaction of the precursor with water is performed at a temperature of 20-25 degrees c below room temperature, such as 0-10 degrees c.

5. The indium calcium oxide nanosheet material as claimed in claim 1, wherein the mass ratio of the precursor to the water is 1: (100-150).

6. The preparation method of the indium calcium oxide nanosheet material is characterized by comprising the following steps of: mixing Ca, In and P according to the proportion of 1: 2: 2, weighing the materials according to the molar ratio, sequentially adding the materials into a quartz tube, carrying out vacuum packaging, heating and sintering in a tube furnace under an inert protective atmosphere, carrying out melting and cooling to obtain a precursor, and reacting the obtained precursor with water to obtain the indium oxide calcium nanosheet material, wherein: raising the temperature to 950-; the mass ratio of the precursor to the water is 1: (100-200).

7. The method for preparing an indium calcium oxide nanosheet material as recited in claim 6, wherein the inert protective atmosphere is nitrogen, helium, or argon.

8. The method as claimed in claim 6, wherein the temperature is raised to 980-1030 ℃ within 300 ± 10min from room temperature 20-25 ℃, the temperature is maintained for 1200-1400 min, and then the temperature is lowered to room temperature 20-25 ℃ at 5-10 ℃/min.

9. The method of claim 6, wherein the reaction of the precursor with water is performed at a temperature of 20-25 ℃ lower than room temperature, such as 0-10 ℃.

10. The method for preparing an indium calcium oxide nanosheet material according to claim 6, wherein the mass ratio of the precursor to the water is 1: (100-150).

Technical Field

The invention relates to preparation of an indium calcium oxide nanosheet, belongs to the technical field of preparation of nano materials, and particularly relates to an indium calcium oxide nanosheet and a preparation method thereof.

Background

Since the emergence of graphene in 2004, various novel nano materials are continuously emerging, and have great application potential in the fields of photoelectric devices, photocatalysis, energy storage and the like. Therefore, the development of various nano materials has positive significance in various fields. Two-dimensional nanosheet materials known to date include single-element two-dimensional materials such as graphene, silylene, germylene, and black phosphene, transition metal dichalcogenides, transition metal carbo/nitrides, two-dimensional covalent organic framework materials, two-dimensional metal organic framework materials, two-dimensional perovskites, carbon nitride, boron nitride, and various oxide nanosheets. The oxide nanosheet has a wide variation range of the band gap value, can span from a conductive material to an insulator material, and is a material with extremely wide application. For example, indium tin oxide films can be conductive, as conductive glass coatings; titanium dioxide has a band gap of about 3eV, and is a good photocatalytic material; the hafnium oxide nano-sheet has an ultra-high band gap of 6eV, and has a very high dielectric constant, thus being an excellent dielectric material. Meanwhile, the nano-sheet structure has extremely high specific surface area and quantum effect, and has extremely wide application prospect in the fields of advanced science and application technology.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provides an indium oxide calcium nanosheet and a preparation method thereof, and the method has the advantages of simple steps and extremely high yield. The nano-sheet structure material has a 2.33eV band gap and has great potential application in photoelectric devices, photocatalysis, energy storage and other aspects.

The technical purpose of the invention is realized by the following technical scheme.

An indium calcium oxide nanosheet material and a preparation method thereof are carried out according to the following steps: mixing Ca, In and P according to the proportion of 1: 2: 2, weighing the materials according to the molar ratio, sequentially adding the materials into a quartz tube, carrying out vacuum packaging, heating and sintering in a tube furnace under an inert protective atmosphere, carrying out melting and cooling to obtain a precursor, and reacting the obtained precursor with water to obtain the indium oxide calcium nanosheet material, wherein: raising the temperature to 950-; the mass ratio of the precursor to the water is 1: (100-200).

And after the precursor reacts with water, the obtained product is washed by deionized water and ethanol for 3-5 times respectively, and is dried in vacuum at the room temperature of 20-25 ℃ for 20-24 h.

Moreover, the inert protective atmosphere is nitrogen, helium or argon.

And raising the temperature to 980-1030 ℃ within 300 +/-10 min from the room temperature of 20-25 ℃, keeping the temperature for 1200-1400 min, and then reducing the temperature to 20-25 ℃ at the speed of 5-10 ℃/min.

Furthermore, the reaction of the precursor with water is carried out at a temperature of 20 to 25 degrees celsius below room temperature, such as 0 to 10 degrees celsius.

And, the mass ratio of the precursor to water is 1: (100-150).

Compared with the prior art, the invention provides the indium oxide calcium nanosheet and the preparation method thereof, the temperature is controlled by a program to obtain a precursor, and the precursor reacts with water at the temperature lower than room temperature to obtain the indium oxide calcium nanosheet. The method has simple steps and great yield. The nano-sheet structure material has a novel structure and has great potential application in photoelectric devices, photocatalysis, energy storage and other aspects.

Drawings

FIG. 1 is an XRD spectrum diagram of the indium oxide calcium nanosheet obtained in the invention.

FIG. 2 is an infrared spectrum diagram of the indium oxide calcium nanosheet obtained in the present invention.

FIG. 3 is an energy spectrum element analysis diagram of the indium oxide calcium nanosheet obtained in the present invention.

FIG. 4 is a scanning electron micrograph of the indium oxide calcium nanosheet obtained in the present invention.

FIG. 5 is a transmission electron micrograph of the indium oxide calcium nanosheet obtained in the present invention.

FIG. 6 is an ultraviolet-visible light absorption diagram of the indium oxide calcium nanosheet obtained in the present invention.

Detailed Description

The invention will be further described with reference to specific embodiments in which argon is selected as the inert shielding gas. The following examples of the present invention are given to further illustrate the present invention, but not to limit the scope of the present invention.

Example 1

0.01mol Ca, 0.02mol in and 0.02mmol P are sequentially weighed in a glove box, sequentially added into a quartz tube, sealed by a vacuum tube sealing system, sintered in a tube furnace, and subjected to temperature control program of raising the temperature from normal temperature (namely room temperature of 20-25 ℃) to 950 ℃ for 300min, maintaining the temperature for 1200min, and then reducing the temperature to normal temperature (namely room temperature of 20-25 ℃) at the temperature of 5 ℃/min. 1g of the precursor was reacted with 150mL of water at 10 ℃. And washing the obtained product with deionized water and ethanol for three times respectively, and performing vacuum drying at room temperature for 24 hours to obtain the indium oxide calcium nanosheet.

Example 2

0.01mol of Ca, 0.02mol of in and 0.02mmol of P are sequentially weighed in a glove box, sequentially added into a quartz tube, sealed by a vacuum tube sealing system, sintered in a tube furnace, and subjected to temperature control program of raising the temperature from normal temperature to 1000 ℃ for 330min, maintaining the temperature for 1500min and then reducing the temperature to normal temperature at 10 ℃/min. 1g of the precursor was reacted with 200mL of water at 5 ℃. And washing the obtained product with deionized water and ethanol for three times respectively, and performing vacuum drying at room temperature for 24 hours to obtain the indium oxide calcium nanosheet.

Example 3

0.01mol of Ca, 0.02mol of in and 0.02mmol of P are sequentially weighed in a glove box, sequentially added into a quartz tube, sealed by a vacuum tube sealing system, sintered in a tube furnace, and subjected to temperature control program of raising the temperature from normal temperature to 1030 ℃ for 280min, maintaining the temperature for 1000min and then reducing the temperature to normal temperature at 5 ℃/min. 1g of the precursor was reacted with 100mL of water at 8 ℃. And washing the obtained product with deionized water and ethanol for three times respectively, and performing vacuum drying at room temperature for 24 hours to obtain the indium oxide calcium nanosheet.

Example 4

0.01mol of Ca, 0.02mol of in and 0.02mmol of P are sequentially weighed in a glove box, sequentially added into a quartz tube, sealed by a vacuum tube sealing system, sintered in a tube furnace, and subjected to temperature control procedures of rising from normal temperature to 980 ℃ for 310min, maintaining for 1400min and then cooling to normal temperature at the speed of 5 ℃/min. 1g of the precursor was reacted with 120mL of water at 5 ℃. And washing the obtained product with deionized water and ethanol for three times respectively, and performing vacuum drying at room temperature for 24 hours to obtain the indium oxide calcium nanosheet.

Example 5

0.01mol of Ca, 0.02mol of in and 0.02mmol of P are sequentially weighed in a glove box, sequentially added into a quartz tube, sealed by a vacuum tube sealing system, sintered in a tube furnace, and subjected to temperature control procedures of raising the temperature from normal temperature to 1020 ℃ in 280min, maintaining the temperature for 1200min and then reducing the temperature to normal temperature at 5 ℃/min. 1g of the precursor was reacted with 150mL of water at 0 ℃. And washing the obtained product with deionized water and ethanol for three times respectively, and performing vacuum drying at room temperature for 24 hours to obtain the indium oxide calcium nanosheet.

Example 6

0.01mol of Ca, 0.02mol of in and 0.02mmol of P are sequentially weighed in a glove box, sequentially added into a quartz tube, sealed by a vacuum tube sealing system, sintered in a tube furnace, and cooled to the normal temperature at the speed of 10 ℃/min after the temperature is increased from the normal temperature to 1000 ℃ for 300min and maintained for 1500 min. 1g of the precursor was reacted with 120mL of water at 0 ℃. And washing the obtained product with deionized water and ethanol for three times respectively, and performing vacuum drying at room temperature for 24 hours to obtain the indium oxide calcium nanosheet.

The indium oxide calcium nanosheets prepared by the method are characterized as shown in the attached figures 1-6. The product obtained after the reaction has no obvious hydroxyl peak, and the XRD spectrogram does not match with the known structure, so that the product is a new structure. Tests have shown that the elements Ca, In and O are detected, indicating that P is etched away during the reaction with water, and that the atomic ratio of Ca to In is 3: 2. the product is shown as an oxide in conjunction with the infrared diagram. The product is of a very obvious nanosheet structure, the indium calcium oxide nanosheet layer structure is intact, and the transverse dimension is about 5 nm. The absorption edge of the nano-sheet product is 533nm, and the corresponding band gap value is 2.33 eV.

The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.