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Mn element and Zn element-doped super-paramagnetic ferrite nanoparticles and preparation method thereof

A superparamagnetic, elemental technology, applied in nanotechnology, nanotechnology, nanotechnology and other directions for materials and surface science, can solve the problems of large particle size, difficult to precisely control, high equipment and operation requirements, and achieve crystallinity. The effect of high, uniform size and high saturation magnetization

Active Publication Date: 2012-11-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This preparation method is carried out under high temperature and high pressure, which requires high equipment and operation, and the process of adjusting pH with ammonia water is not easy to accurately control
[0004] The Chinese patent application with the application number 20081003866.2 discloses a method for preparing manganese zinc ferrite magnetic nano-microspheres. The preparation method is to use soluble iron salts, manganese salts and zinc salts as raw materials by alcohol thermal method, and ethylene glycol As a solvent, anhydrous sodium acetate as a basic additive, polyethylene glycol and polyvinylpyrrolidone as a dispersant, the nano-magnetic spheres with relatively pure crystal phase and high magnetic saturation strength were prepared, but the particle size distribution was wide and the particle size also bigger

Method used

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  • Mn element and Zn element-doped super-paramagnetic ferrite nanoparticles and preparation method thereof
  • Mn element and Zn element-doped super-paramagnetic ferrite nanoparticles and preparation method thereof
  • Mn element and Zn element-doped super-paramagnetic ferrite nanoparticles and preparation method thereof

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Embodiment 1

[0031] The processing steps of the present embodiment are as follows:

[0032] (1) Synthesis of magnetic nanoparticles

[0033] Two precursors of iron acetylacetonate (1 mmol) and manganese acetylacetonate (0.4 mmol) were mixed with 5 mmol of 1,2-hexadecanol, and 3 mmol of oleic acid and 3 mmol of oleylamine were added as surfactants to 25 ml of benzyl ether was used as a solvent, heated to 200°C at a speed of 3°C / min and kept for 2h, and then heated to reflux temperature at the same heating rate, and kept at about 280°C for 1h.

[0034] (2) Post-processing of magnetic nanoparticles

[0035]Cool to room temperature, precipitate in 250 ml ethanol, decant the supernatant, and centrifuge at low speed (3500 rpm, 5 min). Add the obtained black precipitate to oleic acid (0.15 mmol) and oleylamine (0.15 mmol) to disperse in n-hexane and centrifuge at high speed (8000 rpm, 10 min), then precipitate the solution in ethanol again, then centrifuge at low speed to remove excess solvent,...

Embodiment 2

[0038] The processing steps of the present embodiment are as follows:

[0039] (1) Synthesis of magnetic nanoparticles

[0040] Two precursors of iron acetylacetonate (1 mmol) and manganese acetylacetonate (1.25 mmol) were mixed with 5 mmol of 1,2-hexadecanol, and 3 mmol of oleic acid and 3 mmol of oleylamine were added as surfactants to 25 ml of benzyl ether was used as a solvent, heated to 200°C at a speed of 3°C / min and kept for 2h, and then heated to reflux temperature at the same heating rate, and kept at about 280°C for 1h.

[0041] (2) Post-processing of magnetic nanoparticles

[0042] Cool to room temperature, precipitate in 250 ml ethanol, decant the supernatant, and centrifuge at low speed (3500 rpm, 5 min). Add the obtained black precipitate to oleic acid (0.15 mmol) and oleylamine (0.15 mmol) to disperse in n-hexane and centrifuge at high speed (8000 rpm, 10 min), then precipitate the solution in ethanol again, then centrifuge at low speed to remove excess solven...

Embodiment 3

[0045] The processing steps of the present embodiment are as follows:

[0046] (1) Synthesis of magnetic nanoparticles

[0047] Three precursors of iron acetylacetonate (0.75 mmol), manganese acetylacetonate (0.35 mmol) and zinc acetylacetonate (0.15 mmol) were mixed with 5 mmol 1,2-hexadecanol, 3 mmol oleic acid, 3 mmol Oleylamine was used as a surfactant, and 25 ml benzyl ether was used as a solvent, heated to 200°C at a rate of 3°C / min and kept for 2 hours, and then heated to reflux temperature at the same heating rate, and kept at about 280°C for 1 hour.

[0048] (2) Post-processing of magnetic nanoparticles

[0049] Cool to room temperature, precipitate in 250 ml ethanol, decant the supernatant, and centrifuge at low speed (3500 rpm, 5 min). Add the obtained black precipitate to oleic acid (0.15 mmol) and oleylamine (0.15 mmol) to disperse in n-hexane and centrifuge at high speed (8000 rpm, 10 min), then precipitate the solution in ethanol again, then centrifuge at low ...

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Abstract

The invention discloses Mn element and Zn element-doped super-paramagnetic ferrite nanoparticles and a preparation method thereof. Manganese element is added or manganese element and zinc element are simultaneously added into a face-centered cubic crystal structure of ferriferrous oxide nanoparticles by using a method of decomposing metal precursor compound at a high temperature; the magnetic performance of the prepared super-paramagnetic nanoparticles is improved by changing the doping amount and the distribution of the metal element; and primarily, the saturation magnetization is improved. The preparation method specifically comprises the following steps of: mixing acetylacetones of Fe and Mn as well as Zn with 1,2-hexadecanol; performing high-temperature decomposition in high-boiling-point solvent by taking oleic acid and oleylamine as surfactants; or performing high-temperature decomposition on composite oleate of Fe, Mn and Zn by taking the oleic acid as the surfactant; heating and preserving heat in stages in argon or nitrogen protective atmosphere to guarantee growth of nanoparticle nuclear; and cooling to room temperature after reaction is finished and settling and centrifuging to finally obtain the super-paramagnetic ferrite nanoparticles which are uniformly dispersed in normal hexane solution.

Description

Technical field [0001] The present invention is a preparation field of ultra -magnetic nanoparticles, involving an iron oxide supercipsychomy nanoparticles doped metal element MN and Zn. Background technique [0002] Nano -grade magnetic particles, especially oxidized iron magnetic nanoparticles, have attracted great research interests in the biomedical field due to their special magnetic orientation, ultra smooth magnetism, and surfaces that can connect multiple biochemical activity function groups.Biological separation, clinical testing, targeted administration, magnetic resonance imaging, and magnetic heat treatment have wide application prospects.However, because magnetic nanoparticles often need to be covered with surface coverage or branches, which will inevitably reduce its saturated magnetization intensity and affect its magnetic response.Preparation of magnetic nanoparticles with high saturation magnetization strength is one of the key links of its application. Some stud...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/26C04B35/622B82Y30/00
Inventor 吴尧顾忠伟刘克霞蓝芳曾晓波
Owner SICHUAN UNIV
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