Method for preparing ferric oxide nanoparticles with different morphologies

Abstract

The invention discloses a method for preparing ferric oxide nanoparticles with different morphologies, which comprises the following steps: 1) respectively adding ferric salt and sodium hydroxide into water, and uniformly mixing under magnetic stirring to obtain 0.015 mol of ferric chloride solution and 0.03 mol of sodium hydroxide solution; (2) dropwise adding the sodium hydroxide solution into the ferric chloride solution by using an injector, gradually generating precipitates, and gradually changing the color of the solution from light green to grey green; dropwise adding an acetic acid aqueous solution with the volume ratio of 1: 1 into the precipitate, quickly dissolving the precipitate until the color of the solution becomes yellowish-brown, and reacting for three days under magnetic stirring by using a co-precipitation strategy; 3) centrifuging the reactant to obtain a precipitate (hereinafter referred to as a precursor); and 4) weighing 0.1 g of the precursor as a reactant, dissolving the reactant in 15 mL of water, reacting at different temperatures for different times by using a one-step hydrothermal method strategy, naturally cooling to room temperature, collecting a product, and collecting a dried substance in a 60 DEG C oven. According to the invention, the temperature and time are regulated and controlled to regulate and synthesize the ferric oxide nano-materials with nano-sheet-shaped and multi-scale-shaped structures, and the method for preparing the ferric oxide nano-materials with different morphologies is simple to operate.

Description

Technical Field

[0001] The invention belongs to the field of nano materials, and more specifically, relates to a method for preparing ferric oxide nanoparticles with different morphologies. Background Art

[0002] Nanomaterials are metastable substances with unique characteristics such as large specific surface area, small particle size, high surface atomic ratio, electronic motion state and surface effect. They have great application potential in photocatalysis, optoelectronics, batteries, sensors and microelectronics industries. The characteristics of nanomaterials include electrical conductivity, magnetic susceptibility and high specific heat, and they have broad application prospects in the electronics industry, military aerospace ceramic coatings, biomedicine and other industries. As an important chemical raw material, ferric oxide is widely used in industrial products such as supercapacitors, catalysts and functional ceramics. From the perspective of consumption, 70% of ferric oxide comes from industrial synthesis.

[0003] At present, there is no report of nano-thin sheet and multi-scale structure of iron oxide nanomaterials. It is common to use ball milling to prepare sheet-like iron oxide nanomaterials. The morphology of the nanomaterials prepared by this method is mostly uneven and the size is uncontrollable. There are also a small number of patents that use high temperature and high pressure methods to prepare sheet-like iron oxide under the conditions of using complex organic matter. The above methods are not conducive to the large-scale and cheap preparation of nano-sheet materials. Therefore, according to the application requirements, the control of the morphology of nano-iron oxide materials is achieved, and new methods of iron-based oxides suitable for the requirements of the times and production scale are explored, especially pollution-free, low-energy consumption, and high-yield preparation methods. Summary of the invention

[0004] The purpose of the present invention is to solve the above problems in the prior art and provide a method for preparing ferric oxide nanoparticles with different morphologies. The purpose of the present invention is achieved through the following technical solutions:

[0005] A method for preparing ferric oxide nanoparticles with different morphologies comprises the following steps:

[0006] S1: Prepare 0.015mol / 15mL ferric chloride solution and 0.03mol / 15mL sodium hydroxide solution on a magnetic stirrer. The solvent is double distilled water.

[0007] S2: Add 15 mL of sodium hydroxide solution dropwise into the prepared ferric chloride solution and react for 0.5 to 1 hour;

[0008] S3: adding an acetic acid aqueous solution with a volume ratio of 1:1 dropwise to the reactant prepared in S2 to dissolve the precipitate;

[0009] S4: The S3 reaction solution is reacted for 3 days, and the precipitate is obtained by centrifugation to obtain a precursor;

[0010] S5: Weigh 0.1 g of the precursor and dissolve it in 10 mL of double distilled water. Put the reactants into a reactor equipped with an inner liner, place it in an oven, set the temperature and perform a hydrothermal reaction for a certain period of time;

[0011] S6: Finally, the product is obtained by centrifugation, separation and drying in ethanol.

[0012] Furthermore, the temperature in S5 is 180-230° C., and the reaction time is 5 h-40 h.

[0013] Compared with the prior art, this application has the following effects:

[0014] 1. The method for preparing different morphologies of ferric oxide provided by the present application does not require a complicated preparation method, toxic substances, pre-treatment of reactants, or expensive drugs and instruments. The instruments used are also common magnetic stirrers and reaction ovens, and the reaction environment does not require a clean room.

[0015] 2. The thickness of the nanosheets prepared using this technology can be as low as a few nanometers. At the same time, scaly nano-iron oxide materials can be prepared by simply changing the temperature and reaction time. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a scanned image of the nano-thin sheet ferric oxide material prepared by the present invention.

[0017] Figure 2 This is the XRD diagram of the nano-thin sheet ferric oxide material prepared by the present invention.

[0018] Figure 3 This is a scanned image of the flaky ferric oxide material prepared by the present invention.

[0019] Figure 4 This is the XRD diagram of the flaky ferric oxide material prepared in the present invention. DETAILED DESCRIPTION

[0020] The reagents, methods and equipment used in the present invention are all conventional reagents, methods and equipment in the art. Unless otherwise specified, the reagents and materials used in the following examples are all commercially available.

[0021] Example 1

[0022] A method for preparing nano-flaky ferric oxide nanoparticles comprises the following steps:

[0023] S1: Prepare 0.015mol / 15mL ferric chloride solution (light green) and 0.03mol / 15mL sodium hydroxide solution on a magnetic stirrer. The solvent is double distilled water.

[0024] S2: Add 15 mL of sodium hydroxide solution dropwise into the prepared ferric chloride solution, react for 0.5 to 1 hour, and obtain a gray-green precipitate;

[0025] S3: Add acetic acid aqueous solution with a volume ratio of 1:1 dropwise to the reactant prepared in S2 to dissolve the precipitate. The solution is yellow-brown; wherein, the acetic acid aqueous solution has a total of 30 ml, 15 ml of acetic acid, and 15 ml of water;

[0026] S4: The S3 reaction solution is reacted for 3 days, and then the precipitate is obtained by centrifugation to obtain a precursor;

[0027] S5: Weigh 0.1 g of the precursor and dissolve it in 10 mL of double distilled water. Put the reactants into a reactor equipped with an inner liner, place it in an oven, set the temperature to 230 ° C, and the reaction time to 5 h for hydrothermal reaction;

[0028] S6: Finally, the product is centrifuged and separated in ethanol and dried to obtain a flake product.

[0029] like Figure 1 As shown, the material morphology is nano-thin flakes, and the thickness of the flakes is several nanometers.

[0030] like Figure 2 As shown, by analyzing the physical structure of the material, it was found that the material was ferric oxide nanomaterial.

[0031] Example 2

[0032] A method for preparing flaky ferric oxide nanoparticles comprises the following steps:

[0033] S1: Prepare 0.015mol / 15mL ferric chloride solution (light green) and 0.03mol / 15mL sodium hydroxide solution on a magnetic stirrer. The solvent is double distilled water.

[0034] S2: Then, 15 mL of sodium hydroxide solution is added dropwise into the prepared ferric chloride solution, and the reaction is carried out for 0.5 to 1 hour to obtain a gray-green precipitate;

[0035] S3: Next, add acetic acid aqueous solution with a volume ratio of 1:1 dropwise to the reactant prepared in S2 to dissolve the precipitate. The solution is yellow-brown. The acetic acid aqueous solution contains 30 ml of acetic acid, 15 ml of acetic acid, and 15 ml of water.

[0036] S4: The S3 reaction solution is reacted for 3 days, and the precipitate is obtained by centrifugation to obtain a precursor;

[0037] S5: Weigh 0.1 g of the precursor and dissolve it in 10 mL of double distilled water. Put the reactants into a reactor equipped with an inner liner, place it in an oven, set the temperature to 200 ° C, and the reaction time to 20 h for hydrothermal reaction;

[0038] S6: Finally, the product is centrifuged and separated in ethanol and dried to obtain a flake product.

[0039] like Figure 3 As shown, the material morphology is a flake-like structure.

[0040] like Figure 4 As shown, by analyzing the physical structure of the material, it was found that the material was ferric oxide nanomaterial.

Claims

1. A method for preparing ferric oxide nanoparticles with different morphologies, characterized in that: The steps include: S1: Prepare 0.015mol / 15mL ferric chloride solution and 0.03mol / 15mL sodium hydroxide solution on a magnetic stirrer. The solvent is double distilled water. S2: Then, 15 mL of sodium hydroxide solution is added dropwise into the prepared ferric chloride solution, and the reaction is carried out for 0.5 to 1 hour; S3: Next, an acetic acid aqueous solution with a volume ratio of 1:1 is added dropwise to the reactant prepared in S2 to dissolve the precipitate; S4: After the S3 reaction solution is reacted for 3 days, the precipitate is obtained by centrifugation to obtain the precursor; S5: Weigh 0.1 g of the precursor and dissolve it in 10 mL of double distilled water. Put the reactants into a reactor equipped with an inner liner, place it in an oven, and set the temperature and time for hydrothermal reaction; S6: Centrifuge, separate and dry to obtain the product.

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