Ultrasound wave auxiliary hydrothermal synthesis technique for magnetic magnetic iron oxide nano ultra-tiny grain

A technology of ferroferric oxide and hydrothermal synthesis, which is applied in the direction of iron oxide/iron hydroxide, ferrous iron oxide, etc., can solve the problems of large particle size, application limitation, and difficult control of organic compounds, and achieve remanence The effect of very little, low preparation cost, and small grain size

Inactive Publication Date: 2008-05-07
CIVIL AVIATION UNIV OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are two defects in this new method of preparing nanometer ferroferric oxide by irradiation chemical technology. One, because of the large particle size, the product prepared by this new method is not suitable for magnetic immune cell separation, DNA separation, nucleic acid hybridization and magnetic The application of the preparation of targeted drug-loaded microspheres is limited; secondly, due to the use of the organic compound isopropanol as an oxidative free scavenger in aqueous solution, and the use of surfactant polyvinyl alcohol (PVA) to control crystallization The growth rate of the nucleus is used to control the particle size. In the preparation process of this method, the organic compounds are difficult to be completely controlled. Whether it conforms to the 12 principles of green chemistry needs further investigation and verification.

Method used

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  • Ultrasound wave auxiliary hydrothermal synthesis technique for magnetic magnetic iron oxide nano ultra-tiny grain
  • Ultrasound wave auxiliary hydrothermal synthesis technique for magnetic magnetic iron oxide nano ultra-tiny grain
  • Ultrasound wave auxiliary hydrothermal synthesis technique for magnetic magnetic iron oxide nano ultra-tiny grain

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Experimental program
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Effect test

Embodiment 1

[0015] as per figure 1 The process flow shown makes the product.

[0016] The first step: the FeCl 3 ·6H 2 O and FeCl 2 4H 2 O is dissolved in distilled water at a ratio of 1.75:1, and N 2 The air is passed into distilled water, the air in the water is removed, and the mixed solution is obtained under magnetic stirring;

[0017] The second step: the resulting mixed solution is transferred to a 250ml ground-mouthed three-neck flask, and N 2 The other mouth is equipped with a dropping funnel filled with concentrated ammonia water, and the remaining mouth is plugged with a ground plug. In a constant temperature magnetic stirring electric heating mantle, under constant temperature 60°C magnetic stirring, slowly add concentrated ammonia water to adjust the pH of the solution to 11, and then Put it in a digitally controlled ultrasonic oscillator (setting temperature 60°C, power setting 70KHz), and ultrasonically oscillate for 1 hour to obtain Fe 3 o 4 precursors of

[0018]...

Embodiment 2

[0022] Concentrated ammonia water was added to adjust the pH of the solution to 12; the reaction temperature of hydrothermal synthesis was 150° C. for 4 hours. All the other are the same as Example 1, finally obtain the black magnetic ferric oxide nano-powder product, the average grain size of the grain is 20.2nm, the specific saturation magnetization is 63emu / g, the coercive force is 27.8Oe, and the remanence is 2.8emu / g, it can be confirmed that the prepared black magnetic ferric oxide nanopowder is a better superparamagnetic material. Its TEM photo and hysteresis loop as Figure 2B , shown in b.

Embodiment 3

[0024] Concentrated ammonia water was added to adjust the pH of the solution to 13; the reaction temperature of hydrothermal synthesis was 140° C. for 4 hours. All the other are the same as in Example 1, finally obtain the black magnetic iron ferric oxide nano powder product, the average grain size of the grain is 12.4nm, the specific saturation magnetization is 64emu / g, the coercive force is 20.4Oe, and the remanence is 1.8emu / g, it can be confirmed that the prepared black magnetic ferric oxide nanopowder is a better superparamagnetic material. Its TEM photo and hysteresis loop as Figure 2C , as shown in c.

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Abstract

The invention discloses an ultrasonic assistant hydro-thermal synthesis process for magnetic Fe3O4 nanometer super fine grain. The invention solves the problems of impure products and large grain diameter. The invention has the technical proposal that the form of Fe3O4 crystal nucleus is promoted in the cavitation effect of ultrasonic; cavitation gas bubble is produced in mediums; the pH value of strong ammonia is adjusted to 11 to 13; and the nanometer grain diameter size and the magnetic characteristics are controlled by controlling the hydro-thermal synthesis temperature within range from 140 DEG C to 160 DEG C and within time of 3 to 5 hours, and by changing the micro environment of the air bubble chamber, so as to obtain the dry product which is black magnetic Fe3O4 nanometer powder after being milled. The invention comprises no organic solvent, belonging to full green environmental protection which is a break in the field, and the invention is also the first to use the ultrasonic technology for assistant hydro-thermal synthesis. The invention has the advantages of simple technology, low cost, small powder granularity and even grain diameter. The powder not only can be used as duplicate ink powder, but also can be board used in aspects such as medical, biological technology, magnetic immunocyte separation, DNA separation, nucleic acid hybridization, and preparation for magnetic butt directional medicine carrying micron ball.

Description

technical field [0001] The invention relates to a process for preparing magnetic material nanoparticles by using ultramicro technology, in particular to a process for preparing ferrous oxide ultrafine magnetic powder nanomaterials, which belongs to B82B3 / 00; B82B1 / 00; H01F1 / 10C01G49 / 08 technology field. technical background [0002] The nano-magnetic material Fe3O4 is an important inverse spinel ferrite, when the magnetic Fe 3 o 4 When the particle diameter is smaller than a certain critical size, superparamagnetism occurs. This material is very easy to magnetize under the external magnetic field, but when the external magnetic field is cancelled, it is very easy to demagnetize, there is no hysteresis phenomenon, and the coercive force is zero, so that the nanoparticles will not be permanently magnetized in the magnetic field. Due to its special magnetic and electrical properties, it has broad application prospects in the fields of magnetic fluid, magnetic recording, magn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 郭英李酽刘秀琳才华栗建钢吴瑶
Owner CIVIL AVIATION UNIV OF CHINA
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