CN-117945465-B - Synthesis method of nano curved surface bicrystal hematite

Abstract

The invention discloses a method for synthesizing nano curved surface bicrystal hematite. And (3) taking the nanorod beta-FeOOH as a reaction precursor material, regulating the pH value of the solution to 1-3 by using hydrochloric acid, performing hydrothermal reaction at the temperature of 180-230 ℃, cooling the reaction kettle to room temperature, and washing and drying a solid precipitate obtained by centrifugation to obtain the nano curved surface bicrystal hematite. The hematite curved surface bicrystal obtained by the invention is artificial synthesis in a laboratory for the first time, and provides a new method for preparing and researching hematite materials with special morphology. The method has the advantages of no addition of other active agents in the reaction system, environmental protection, simple process and convenient operation, and can realize large-scale preparation.

Inventors

• LIANG WEI
• ZHU PINGHUA
• ZONG MEIRONG
• LIU HAONAN
• QIAN DUODUO
• JIANG HONGWEI
• LV QIFENG
• LIU HUI

Assignees

• 常州大学

Dates

Publication Date

20260505

Application Date

20240115

Claims (7)

1. 1. The synthesis method of the nano curved surface bicrystal hematite is characterized by comprising the following steps of: Under continuous stirring, feCl 3 ·6H 2 O is dissolved in deionized water to obtain ferric chloride solution, the ferric chloride solution is added into a reaction bottle for sealing, the reaction is carried out for 5-9 days at the temperature of 65-85 ℃, and the obtained precipitate is washed by deionized water and dried to obtain nano rod-shaped beta-FeOOH; And (2) fully dispersing the beta-FeOOH obtained in the step (1) in deionized water to obtain a beta-FeOOH aqueous solution, regulating the pH value of the solution to 1-3 by using hydrochloric acid, then carrying out hydrothermal reaction at 180-230 ℃ for 18-32 hours, and washing and drying the generated solid substance by using deionized water after cooling to room temperature to obtain the hematite nano curved surface bicrystal.
2. 2. The method for synthesizing nano curved surface bicrystal hematite according to claim 1, wherein the concentration of FeCl 3 ·6H 2 O in the step (1) is 0.03-0.08 mol/L.
3. 3. The method for synthesizing nano curved surface bicrystal hematite according to claim 1, wherein the reaction of the step (1) is a standing reaction.
4. 4. The method for synthesizing the nano curved surface bicrystal hematite according to claim 1, wherein the length of the nano rod-shaped beta-FeOOH is 400 nm-1.5 mu m, the width and the height are the same, and the size is 20 nm-60 nm.
5. 5. The method for synthesizing nano curved surface bicrystal hematite according to claim 1, wherein the concentration of the beta-FeOOH aqueous solution in the step (2) is 0.03-0.08 mol/L.
6. 6. The method for synthesizing nano curved surface bicrystal hematite according to claim 1, wherein the hydrothermal reaction in the step (2) is performed in a rotary oven of a reaction kettle.
7. 7. The nano curved surface double-crystal hematite synthesized by the method of any one of claims 1-6, wherein the nano curved surface double-crystal hematite has a shape of a symmetrical flying saucer-shaped double-crystal structure containing 12 curved surfaces.

Description

Synthesis method of nano curved surface bicrystal hematite Technical Field The invention belongs to the technical field of mineral material synthesis, in particular to a method for synthesizing hematite without adding green, and particularly relates to a method for synthesizing nano curved surface bicrystal hematite. Background Hematite is a natural semiconductor mineral, and has stable chemical properties on the surface of the earth and wide distribution. The nano-structure hematite has stable physicochemical properties, is an environment-friendly photoactive material with higher catalytic activity, and has wide application prospects in the aspects of photovoltaics, catalysis, solar energy, sensors, environmental adsorbents and the like. It is well known that particle shape, size, specific surface area and microstructure determine the chemical and physical properties of nanomaterials. The type of hematite crystal face has great influence on the physicochemical properties, and the synthesis method for flattening specific crystal faces is common at present, such as the synthesis of a (104) crystal face exposure nanocube (application number: 200610156050.4) and the synthesis method of a three-sided crystal bicrystal with two crystal faces exposed (application number: 202011471573.4). The mutual cooperation of different crystal faces of the hematite can improve the catalytic activity of the hematite, so that certain attention is paid to the synthesis of various crystal faces of exposed hematite, such as the synthesis of nano-porous hematite with high-efficiency catalytic performance (application number: 202111050200.4), the synthesis of porous hematite nano-arrays (application number: 201810488271.4), the production of hematite pellets (application number: 200410035715.7) and the like. Thus, knowing the synthesis conditions controlling particle size, morphology and crystal planes can lead to a new synthesis method, and nano hematite can be tailored to obtain optimal performance. No report exists at present on the synthesis of nano curved surface bicrystal hematite without any surfactant addition and with various active surfaces. Disclosure of Invention Aiming at the technical defects of the existing synthesis method, the invention aims to provide a green synthesis method without adding redundant surfactant for nano curved surface bicrystal hematite so as to solve the problem that the prior art does not synthesize nano curved surface bicrystal hematite. In order to achieve the above purpose, the invention adopts the following technical scheme: A method for synthesizing nano curved surface bicrystal hematite comprises the following steps: And step 1, under continuous stirring, feCl 3·6H2 O is dissolved in deionized water to obtain ferric chloride solution, the ferric chloride solution is placed in a reaction bottle, an oven is placed for reaction, and the obtained precipitate is washed and dried by using deionized water to obtain the nano rod-shaped beta-FeOOH. And 2, fully dispersing the nano rod-shaped beta-FeOOH in the step 1 in deionized water, regulating the pH value of the solution by utilizing hydrochloric acid, then adding the solution into a reaction kettle, placing the reaction kettle in an oven for hydrothermal reaction, and after the reaction kettle is cooled to room temperature, cleaning and drying the generated solid substance by using the deionized water to obtain the hematite nano curved surface bicrystal. Further, the ferric chloride solution in the step 1 is obtained by dissolving FeCl 3·6H2 O in deionized water, and the concentration of the ferric chloride solution is 0.03-0.8 mol/L. Further, the reaction bottle in the step1 is a sealable glass bottle. Further, the reaction temperature of the oven reaction in the step 1 is 65-85 ℃ and the reaction time is 5-9 days. If the temperature is lower than 65 ℃, beta-FeOOH cannot be completely produced, and if the temperature is higher than 85 ℃, hematite phase appears. If the standing reaction time is less than 5 days, the FeCl 3 is not completely hydrolyzed, and if the standing reaction time exceeds 9 days, beta-FeOOH can further react to generate hematite. Further, the deionized water cleaning in the step 1 is to ultrasonically disperse the obtained solid precipitate into deionized water, the solid-liquid ratio is 1:10, ultrasonically clean the solution for 10 min, and after cleaning, centrifugate the solution to remove the supernatant, and the step is repeated for 3-10 times. Until the supernatant was clear and transparent. Further, the dimension length of the nanorod-shaped beta-FeOOH in the step 1 is 400 nm-1.5 μm, the width and the height of the beta-FeOOH nanorod are the same, and the dimension range is 20 nm-60 nm. Further, the nanorod-shaped beta-FeOOH obtained in the step2 is fully dispersed in deionized water, and the concentration of the nanorod-shaped beta-FeOOH is 0.03-0.08 mol/L. Further, the fully dispersing of the nanorod-shaped beta-