阅读说明：本技术 一种FeMnSx纳米片簇及其制备方法 (FeMnSxNanosheet cluster and preparation method thereof ) 是由 钟晓聪 王瑞祥 徐志峰 林振聪 袁远亮 于 2021-02-03 设计创作，主要内容包括：本发明公开了一种FeMnS-x纳米片簇及其制备方法。该FeMnS-x纳米簇是一种由FeMnS-x纳米片堆积成簇状物。其制备方法包括以下步骤,首先,将摩尔比为1：2的氯化胆碱与乙二醇混匀获得低共熔溶剂,依次加入FeCl-3、MnCl-2、硫代乙酰胺、尿素；然后,将上述溶液倒入水热反应釜中,在170℃下反应20h；最后,待反应釜自然冷却到室温,离心分离、洗涤、冷冻干燥,获得FeMnS-x纳米片簇。该FeMnS-x纳米片簇具有比表面积大、析氧反应催化活性高的优点,具有良好的商业化应用前景。(The invention discloses FeMnS x Nanosheet clusters and a preparation method thereof. The FeMnS x The nanocluster is a cluster formed by FeMnS x The nanoplatelets are stacked into clusters. The preparation method comprises the following steps of firstly, mixing the raw materials in a molar ratio of 1:2, evenly mixing choline chloride and ethylene glycol to obtain a eutectic solvent, and sequentially adding FeCl 3 、MnCl 2 Thioacetamide, urea; then pouring the solution into a hydrothermal reaction kettle, and reacting for 20 hours at 170 ℃; finally, after the reaction kettle is naturally cooled to room temperature, carrying out centrifugal separation, washing and freeze drying to obtain FeMnS x Nanosheet clusters. The FeMnS x The nano-sheet cluster has the advantages of large specific surface area and high catalytic activity of oxygen evolution reaction, and has good commercial application prospect.)

1. FeMnS_xNanosheet cluster, characterized by consisting of FeMnS_xThe nanoplatelets are stacked into clusters.

2. A FeMnS alloy as set forth in claim 1_xThe preparation method of the nanosheet cluster is characterized by comprising the following steps:

mixing a mixture of 1:2, evenly mixing choline chloride and ethylene glycol at 70 ℃ to obtain eutectic solvent, and sequentially adding FeCl₃、MnCl₂Thioacetamide and urea, wherein FeCl₃、MnCl₂The concentration of the compound is 0.25M, and the concentration of thioacetamide and urea is 0.1M;

pouring the solution into a hydrothermal reaction kettle, and reacting for 20 hours at 170 ℃;

after the reaction kettle is naturally cooled to room temperature, centrifugally separating, washing, freezing and drying to obtain FeMnS_xNanosheet clusters.

Technical Field

The invention relates to the field of nano materials, in particular to FeMnS_xA method for preparing a nano-sheet cluster.

Background

The transition metal sulfide has the advantages of rich raw material reserves, low cost, greenness, no toxicity and oxygen evolution reaction catalysisHigh chemical activity, and is widely applied to the field of hydrogen production by water cracking. At present, the transition metal sulfides reported in the literature for oxygen evolution reaction are mainly CoS and NiFeS_x、NiCoS_xAnd CoNiS_xAnd the like. Transition metal sulfides have various types, and transition metal sulfides with different compositions and structures can be prepared by changing the types of metals and a synthesis method. At present, the common preparation methods of transition metal sulfides mainly include a hydrothermal method or a solvothermal method, such as reaction in aqueous solution, alcoholic solution and other systems at high temperature to obtain a nano material.

Disclosure of Invention

The invention mainly aims to provide FeMnS_xA nanosheet cluster and a preparation method thereof aim to develop an electrocatalyst with large specific surface area and high oxygen evolution activity and a preparation method thereof, improve the oxygen evolution activity of transition metal sulfides, and overcome the defect that nano products are easy to agglomerate in the traditional hydrothermal and solvothermal preparation process.

In order to achieve the above object, the present invention provides a FeMnS_xNanosheet cluster consisting of FeMnS_xThe nanoplatelets are stacked into clusters.

In order to achieve the aim, the invention provides FeMnS_xThe preparation method of the nanosheet cluster comprises the following steps:

mixing a mixture of 1:2, evenly mixing choline chloride and ethylene glycol at 70 ℃ to obtain a eutectic solvent, and sequentially adding FeCl₃、MnCl₂Thioacetamide and urea, wherein FeCl₃、MnCl₂The concentration of the compound is 0.25M, and the concentration of thioacetamide and urea is 0.1M;

pouring the solution into a hydrothermal reaction kettle, and reacting for 20 hours at 170 ℃;

after the reaction kettle is naturally cooled to room temperature, centrifugally separating, washing, freezing and drying to obtain FeMnS_xNanosheet clusters.

The basic idea and technical principle of the invention are as follows:

CoS、NiFeS_x、NiCoS_xand CoNiS_xThe transition metal sulfide has good oxygen evolution catalytic activity. Mn as a majorityThe valence state metal, the compound of which is an ideal oxygen evolution reaction catalyst. Therefore, the invention tries to introduce manganese into transition metal sulfide, and invents FeMnS for catalyzing oxygen evolution reaction_x。

The common preparation method of the transition metal sulfide mainly comprises a hydrothermal method or a solvothermal method, and the nano material is obtained by adopting an aqueous solution and an alcohol solution and reacting at a high temperature. The solvent adopted in the synthesis process has obvious influence on the composition, crystallinity and morphological structure of the product, so the invention provides the eutectic solvent prepared by choline chloride-ethylene glycol, and FeMnS is obtained by reaction in a reaction kettle_xNanosheet clusters.

The FeMnS is prepared by taking ferric chloride and manganese chloride as metal sources, taking thioacetamide as a sulfur source and taking a low-eutectic solvent prepared from choline chloride and ethylene glycol as a reaction solvent through reaction at a high temperature_xNanosheet clusters. FeMnS_xLarge specific surface area, high oxygen evolution reaction activity and good application prospect.

Compared with the prior art, the invention has the following beneficial effects:

1) provides a FeMnS_xThe nano-sheet cluster has large specific surface area and high oxygen evolution activity;

2) the FeMnS with a unique shape and structure is prepared by adopting a eutectic solvent prepared from choline chloride-ethylene glycol_x。

3) FeMnS prepared by eutectic solvent_xThe nano-cluster has good dispersibility and is not easy to agglomerate.

Drawings

FIG. 1 shows FeMnS in the example_xAnd (3) a topography of the nanosheet cluster.

Detailed Description

The present invention will be described in detail with reference to the following examples.

The choline chloride and the ethylene glycol are uniformly stirred at 70 ℃ according to the molar ratio of 1:2 to prepare the eutectic solvent. Adding 10mmol of FeCl₃And 10mmol of MnCl₂Dissolved in 40mL of the eutectic solvent. 4mmol of thioacetamide and 4mmol of urea are added in sequence and mixed with the eutectic solvent uniformly. Mixing the aboveThe prepared solution was put into a 100mL hydrothermal reaction kettle and reacted at 170 ℃ for 20 hours. After the reaction kettle is naturally cooled, the solution in the reaction kettle is centrifugally washed by deionized water and ethanol. Putting the washed sample into a freeze drying box for drying to obtain FeMnS_xThe morphology of the nanosheet cluster is shown in figure 1. FeMnS is added_xDispersing in ethanol containing Nafion, making into ink, and dripping on foamed nickel (10 mm × 10 mm), FeMnS_xThe loading capacity is 1mg/cm². In a 1M KOH solution, the current density was 10mA/cm^-2At 25 deg.C, the overpotential for oxygen evolution is about 280 mV.