Method for preparing Nano cube of hematite

A nano-cube and hematite technology, applied in the direction of iron oxide, iron oxide/iron hydroxide, etc., can solve the problem of poor shape and size uniformity of nanoparticles, agglomeration of hematite nanoparticles, complex process, etc. problems, to achieve the effects of easy control of the reaction process, uniform shape and particle size, and simple preparation process

Inactive Publication Date: 2007-07-25
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
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Problems solved by technology

This method involves two processes, the process is complicated and time-consuming, and at the same time, the obtained hematite nanoparticles are seriously agglomerated
[0006] Germany "Advanced Functional Materials" (Advanced Functional Materials, 2006, volume 16, pages 1805-1813) reported adding ferric salt solution to the system of oleic acid, ethanol and sodium hydroxide, followed by hydrothermal treatment to synthesize hematite ore nanocubes, obtained hematite nanoparticles with relatively good monodispersity, but the uniformity of the shape and particle size of the nanoparticles was not very good

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  • Method for preparing Nano cube of hematite

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] According to the molar ratio of sodium oleate and iron ion number 3:1, 1.6g (5.1mmol) sodium oleate, 0.48g (1.7mmol) ferric chloride hexahydrate, 1mL oleic acid and 10mL ethanol were added to the The volume of 16mL aqueous solution is 30mL polytetrafluoroethylene reactor, stir magnetically at 400rpm for one hour, the solution is divided into two uniform phases: the upper layer is reddish brown, and the lower layer is colorless; after sealing the reactor, place it in an oven at 180°C Stand at constant temperature for 8 hours. The obtained synthetic solution was cooled to room temperature, and 0.12 g of solid was obtained after centrifugation. After the solid was washed with ethanol, it was dispersed in 10 mL of cyclohexane. 10 mL of ethanol was added to precipitate a solid product.

[0022] During the synthesis process, the prepared reaction solution is stirred and divided into two uniform phases. After detection, the reddish brown on the upper layer is the oleic acid s...

Embodiment 2

[0029] According to the molar ratio of potassium oleate and iron ion number 2:1, 1.5g (4.8mmol) potassium oleate, 0.48g (2.4mmol) ferric dichloride tetrahydrate, 2mL oleic acid and 8mL ethanol were added to the The volume of 16mL aqueous solution is 30mL polytetrafluoroethylene reaction kettle, magnetically stirred at 500rpm for two hours, the solution is divided into reddish-brown upper layer and colorless uniform two-phase lower layer; the reaction kettle is sealed and placed in an oven at 220°C to keep the temperature static Placed for 8 hours; the resulting synthetic solution was cooled to room temperature, centrifuged to obtain 0.14g solid, washed with ethanol, dispersed in 20mL of hexane, centrifuged again to separate the solid precipitate, and obtained red hexane Add 20 mL of ethanol to the alkane colloidal solution, and the solid product is precipitated.

[0030] The characterization method is the same as in Example 1.

[0031] Figure 5 shows the transmission electron...

Embodiment 3

[0033]According to the molar ratio of sodium oleate and iron ion number 4:1, sequentially add the mixed solution of 0.97g (3.2mmol) sodium oleate, 0.32g (0.8mmol) ferric nitrate nonahydrate, 5mL oleic acid and 4mL ethanol to the container. There is 16mL of aqueous solution in a 30mL polytetrafluoroethylene reactor, magnetically stirred at 200rpm for two hours, until the solution is divided into two uniform phases, the reactor is sealed, and placed in an oven at 180°C for 8 hours at a constant temperature. The resulting synthetic solution was cooled to room temperature, and 0.09 g of solid was obtained after centrifugation. After the solid was washed with ethanol, it was dispersed in 2 mL of chloroform, and after the solid precipitate was separated by centrifugation, 2 mL of the obtained red chloroform colloidal solution was added. ethanol, the solid product precipitated out. The representation method is the same as above.

[0034] Figure 6 shows the transmission electron micr...

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Abstract

This invention discloses a method for preparing hematite nanocubes. The method comprises: (1) adding soluble inorganic ferric salt 0.8-2.4 mmol, potassium oleate or sodium oleate 2-4 mol times of ferric ions, ethanol 4-10 mL and oleic acid 1-5 mL into water 16 mL, stirring to uniformly demix, and placing in a sealed container; (2) standing at 160-220 deg.C for more than 8 h; (3) centrifuging to separate the solid precipitate, washing with ethanol, drying, and dispersing in alkane solvent; (4) centrifuging to separate the solid precipitate, adding ethanol into the obtained red alkane colloidal solution to precipitate aggregates of hematite nanocubes with average side length of 14-17 nm. The method has such advantages as easy operation, easy control, mild conditions and no pollution. The obtained hematite nanocubes have good monodispersity, uniform particle sizes, and regular and uniform morphology. The hematite nanocubes exhibit superparamagnetism at normal temperature, and can be used in magnetic storage and medical fields.

Description

Technical field: [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for synthesizing hematite nanocubes by a hydrothermal method. Background technique: [0002] British "Journal of Materials Chemistry" (Journal of Materials Chemistry, 2002, volume 12, pages 1676-1683) reported that a mixture of ethylene oxide and ethanol was added dropwise in an aqueous solution of ferric chloride, and treated at a high temperature above 300 ° C, passed Sol-gel method to prepare hematite nanoparticles. The particle size obtained by this method is relatively small (20-60 nanometers), and due to the lack of surfactant in the preparation system, the nucleation and growth of crystal grains cannot reach equilibrium, so the obtained product particle size distribution is wide, and the particle agglomeration is serious and difficult. There is no regular geometric shape; at the same time, high temperature treatment is required in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/02C01G49/06
Inventor 俞书宏汪尚兵
Owner UNIV OF SCI & TECH OF CHINA
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