阅读说明：本技术 一种纳米氢氧化铟的制备方法 (Preparation method of nano indium hydroxide ) 是由 邵学亮 王继民 朱刘 于 2020-05-21 设计创作，主要内容包括：本发明揭示了一种纳米氢氧化铟的制备方法,包括以下步骤：以金属铟为阳极、惰性电极为阴极、铵盐水溶液为电解液进行电解,即可得到氢氧化铟。本发明提供的一种纳米氢氧化铟的制备方法,阳极、阴极同时安装在一个电解室内,阳极、阴极通过与电解室内的电解液接触相连通,电解过程中,不需要配制阴极液、阳极液,只需要配制一种电解液,使电解液在电解室内保持循环流动,就能完成整个电解过程,极大的降低了设备成本,且不需添加辅料,工艺简单。(The invention discloses a preparation method of nano indium hydroxide, which comprises the following steps: and electrolyzing by taking the metal indium as an anode, an inert electrode as a cathode and an ammonium salt aqueous solution as electrolyte to obtain the indium hydroxide. According to the preparation method of the nanometer indium hydroxide, the anode and the cathode are simultaneously arranged in the electrolytic chamber, the anode and the cathode are communicated with the electrolyte in the electrolytic chamber in a contact manner, and during the electrolytic process, the catholyte and the anolyte do not need to be prepared, only one electrolyte needs to be prepared, and the electrolyte keeps circulating flow in the electrolytic chamber, so that the whole electrolytic process can be completed, the equipment cost is greatly reduced, auxiliary materials do not need to be added, and the process is simple.)

1. A preparation method of nano indium hydroxide is characterized by comprising the following steps: and electrolyzing by taking the metal indium as an anode, an inert electrode as a cathode and an ammonium salt aqueous solution as electrolyte to obtain the indium hydroxide.

2. The method for preparing nano indium hydroxide according to claim 1, wherein the anode and the cathode are simultaneously installed in an electrolytic chamber, and the anode and the cathode are in contact communication with an electrolyte in the electrolytic chamber.

3. The method for preparing nano indium hydroxide according to claim 2, wherein the electrolyte is maintained in a circulating state in the electrolytic chamber during the electrolysis.

4. The method for preparing nano indium hydroxide according to claim 2, wherein the inert electrode is at least one of a titanium plate, a graphite plate, a platinum plate and a gold-plated plate; the ammonium salt in the ammonium salt aqueous solution is at least one of ammonium nitrate and ammonium sulfate.

5. The method for preparing nano indium hydroxide according to claim 2, wherein the ammonium salt aqueous solution is an ammonium nitrate aqueous solution having an ammonium nitrate concentration of 0.1 to 3 mol/L.

6. The method for preparing nano indium hydroxide according to claim 2, wherein the pH of the aqueous ammonium salt solution is 3.0 to 7.0.

7. The method for preparing nano indium hydroxide according to claim 2, wherein an electrode distance between the anode and the cathode is 30 to 200 mm.

8. The method as claimed in claim 2, wherein the current density of the electrolysis is 500-2000A/m²The temperature is 20-70 ℃.

9. The method for preparing nano indium hydroxide according to claim 1, further comprising the steps of: and performing solid-liquid separation on the indium hydroxide in the electrolyte to obtain the nano indium hydroxide powder.

10. The method for preparing nano indium hydroxide according to claim 9, wherein the obtained nano indium hydroxide powder has a particle size of 2 to 20nm and a specific surface area of more than 90m²/g。

Technical Field

The invention relates to the technical field of material preparation, in particular to a preparation method of nano indium hydroxide.

Background

Indium hydroxide (in (OH)₃) Indium hydroxide is a precursor for producing indium oxide or a compound powder containing indium oxide, and is used for producing an ITO target for sputtering for forming an ITO film (a composite oxide containing indium-tin as a main component), which is a transparent electrode film widely used in display devices such as solar cells and liquid crystal displays. With the rapid development of global digital technology, the current photoelectric equipment gradually develops towards personalization, ultra-large-scale and irregular-shaped display, the demand of transparent conductive films such as sputtering target materials and the like is remarkably increased, and the demand of indium hydroxide as a precursor of a main raw material for forming the transparent conductive film is also remarkably increased.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a preparation method of nano indium hydroxide.

In order to achieve the purpose, the invention adopts the following technical scheme.

The invention provides a preparation method of nano indium hydroxide, which is characterized by comprising the following steps: and electrolyzing by taking the metal indium as an anode, an inert electrode as a cathode and an ammonium salt aqueous solution as electrolyte to obtain the indium hydroxide.

As a further improvement of the invention, the anode and the cathode are simultaneously arranged in an electrolytic chamber, and the anode and the cathode are communicated by being in contact with the electrolyte in the electrolytic chamber.

As a further improvement of the invention, during the electrolysis process, the electrolyte is kept in a circulating flow state in the electrolytic chamber.

As a further improvement of the invention, the inert electrode is at least one of a titanium plate, a graphite plate, a platinum plate and a gold-plated plate; the ammonium salt in the ammonium salt aqueous solution is at least one of ammonium nitrate and ammonium sulfate.

As a further improvement of the invention, the ammonium salt aqueous solution is an ammonium nitrate aqueous solution with the ammonium nitrate concentration of 0.1-3 mol/L.

As a further improvement of the invention, the pH value of the ammonium salt aqueous solution is 3.0-7.0.

As a further improvement of the invention, the electrode distance between the anode and the cathode is 30-200 mm.

As a further improvement of the invention, the current density of the electrolysis is 500-2000A/m²The temperature is 20-70 ℃.

As a further improvement of the present invention, the method further comprises the steps of: and performing solid-liquid separation on the indium hydroxide in the electrolyte to obtain the nano indium hydroxide powder.

As a further improvement of the invention, the obtained nano indium hydroxide powder has the particle size of 2-20nm and the specific surface area of more than 90m²/g。

According to the preparation method of the nanometer indium hydroxide, the anode and the cathode are simultaneously arranged in the electrolytic chamber, the anode and the cathode are communicated with the electrolyte in the electrolytic chamber in a contact manner, and during the electrolytic process, the catholyte and the anolyte do not need to be prepared, only one electrolyte needs to be prepared, and the electrolyte keeps circulating flow in the electrolytic chamber, so that the whole electrolytic process can be completed, the equipment cost is greatly reduced, auxiliary materials do not need to be added, and the process is simple.

Drawings

FIG. 1 is a scanning electron microscope image of indium hydroxide powder prepared in example 1 of the present invention.

FIG. 2 is a graph of the particle size distribution and BET data of indium hydroxide powder prepared in example 1 of the present invention.

FIG. 3 is a scanning electron microscope image of indium hydroxide powder prepared in example 2 of the present invention.

FIG. 4 is a graph of the particle size distribution and BET data of indium hydroxide powder prepared in example 2 of the present invention.

FIG. 5 is a scanning electron microscope image of indium hydroxide powder prepared in example 3 of the present invention.

FIG. 6 is a graph of the particle size distribution and BET data of indium hydroxide powder prepared in example 3 of the present invention.

Detailed Description

The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a preparation method of nano indium hydroxide, which comprises the following steps:

and electrolyzing by taking the metal indium as an anode, an inert electrode as a cathode and an ammonium salt aqueous solution as electrolyte to obtain the indium hydroxide. Wherein, the electrode distance between the anode and the cathode is 30-200mm, when the electrode distance is more than 200mm, the resistance between the anode and the cathode is increased, and the power consumption is increased; when the electrode pitch is less than 30mm, contact or short circuit between electrodes is likely to occur.

The inert electrode is at least one of a titanium plate, a graphite plate, a platinum plate and a gold-plated plate, and as a further preferable embodiment of the method for preparing nano indium hydroxide of the present invention, the inert electrode is preferably a titanium plate.

The ammonium salt in the ammonium salt aqueous solution is at least one of ammonium nitrate and ammonium sulfate, and as a further preferable embodiment of the method for preparing nano indium hydroxide of the present invention, the ammonium salt in the ammonium salt aqueous solution is preferably ammonium nitrate.

The ammonium salt aqueous solution is ammonium nitrate aqueous solution with ammonium nitrate concentration of 0.1-3mol/L, when the ammonium nitrate concentration is lower than 0.1mol/L, voltage can be increased during electrolysis, heating of an electrified part is caused, and electric power cost is increased; when the concentration of ammonium nitrate is higher than 3mol/L, the salt content of the slurry obtained by electrolysis is high, so that the water consumption for removing impurity salt in indium hydroxide is increased, the economy and environmental protection are not sufficient, and the obtained indium hydroxide powder is thick and uneven in particle size distribution.

The pH value of the ammonium salt aqueous solution is 3.0-7.0, and when the pH value of the ammonium salt aqueous solution is less than 3.0, the settling property of the indium hydroxide generated by electrolysis is poor; when the pH value of the ammonium salt aqueous solution is more than 7.0, the precipitation speed of the indium hydroxide is too high, so that the concentration of the anolyte is not uniform on one hand, and the indium hydroxide is directly precipitated on the other hand, so that the indium hydroxide has a wide particle size range and is not suitable as a raw material of ITO powder.

In this example, the electrolytic reaction of the indium hydroxide production method was as follows:

an anode region: in → In³⁺+3e

In³⁺+3OH^-→In(OH)₃；

A cathode region: h⁺+2e→H₂。

The anode and the cathode are simultaneously arranged in an electrolytic chamber, the anode and the cathode are communicated by being in contact with electrolyte in the electrolytic chamber, and the reaction generated in the electrolytic process of the electrolytic chamber is as follows:

NH₄NO₃→NH₄ ⁺+NO₃ ^-；

NH₄ ⁺→NH₃+H⁺；

NH₃+H₂O→NH₄ ⁺+OH^-。

in the electrolytic process, the current density of electrolysis is 500-2000A/m². When the current density is less than 500A/m²In the process, the generation amount of indium hydroxide is reduced, and the productivity is lower; when the current density is more than 2000A/m²In the electrolysis, the cell voltage is significantly increased, the electrified part generates heat, and the energy consumption is increased.

During the electrolysis, the electrolysis temperature is 20-70 ℃. When the electrolysis temperature is lower than 20 ℃, the precipitation speed of the indium hydroxide becomes too slow; when the electrolysis temperature is higher than 70 ℃, the energy consumption is high, the electrolyte is seriously volatilized, the environment is not environment-friendly, and the precipitation speed of the indium hydroxide is too high, so that the particle size distribution is widened.

In the electrolytic process, the electrolyte keeps a circulating flow state in the electrolytic chamber, the whole electrolytic process does not need to prepare catholyte and anolyte, the whole electrolytic process can be completed only by preparing the electrolyte and keeping the circulating flow state between the anode and the cathode, and the anode and the cathode simultaneously carry out electrolytic reaction in one electrolytic chamber, so that the electrolytic reaction is more complete, and the nano indium hydroxide powder with high product purity, low impurity content, uniform particle size distribution and larger specific surface area is generated. The traditional electrolytic method for preparing indium hydroxide needs to prepare catholyte and anolyte, which not only increases the cost, but also causes incomplete reaction, thereby failing to prepare the nano indium hydroxide powder with high product purity, low impurity content, uniform particle size distribution and larger specific surface area.

After the electrolysis is finished, performing solid-liquid separation on the indium hydroxide in the electrolyte to obtain nano indium hydroxide powder, wherein the equipment for performing solid-liquid separation is a filter press, and the obtained indium hydroxide powder has the particle size of 2-20nm and the specific surface area of more than 90m²The larger the specific surface area of the obtained indium hydroxide powder is, the larger the adsorption area of the indium hydroxide powder is, the higher the activity is and the better the dispersibility is, in the application of the rear end, the battery prepared by utilizing the indium oxide powder can realize rapid charge and discharge, the conductive material or other luminescent materials prepared by utilizing the indium oxide powder can ensure that the conductivity of the material is more uniform, and the lower sintering temperature can be used for preparing the oxide target material by utilizing the indium oxide powder, so that the energy is saved.

For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.