Methods of making metal oxide nanoparticles

A technology of nanoparticles and oxides, applied in ferrous oxides, iron compounds, chemical instruments and methods, etc.

Inactive Publication Date: 2010-03-24
3M INNOVATIVE PROPERTIES CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have proven problematic when large quantities (e.g., 100 grams or more) of nanoparticles are required

Method used

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  • Methods of making metal oxide nanoparticles
  • Methods of making metal oxide nanoparticles
  • Methods of making metal oxide nanoparticles

Examples

Experimental program
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example

[0089] These examples are for illustrative purposes only and are not intended to limit the scope of the appended claims. All parts, percentages, ratios, etc. in the examples are by weight unless otherwise specified.

[0090] Ethanol (95%), hexane, acetone, isopropanol and toluene were obtained from EMD (San Diego, CA). All other reagents were obtained from Sigma-Aldrich Chemical Company (Milwaukee, WI) unless otherwise noted.

[0091] Test Methods

[0092] Transmission Electron Microscopy (TEM)

[0093] Samples for TEM imaging were prepared by placing a drop of undiluted sample or by placing a drop of diluted sample (1 part sample mixed with 2 parts hexane) on a 400-mesh copper TEM grid on an irregular carbon ( Ted Pella Company, Redding, CA) with an ultrathin carbon substrate on top of the grid. A portion of the sample drop was removed by touching the sides or bottom of the grid with filter paper. Allow remaining sample to dry. This allows the particles to remain on...

example 1

[0128] The feed composition was prepared by adding ferric oleate precursor (161.2 grams), prepared as described in Preliminary Example 1, to a plastic container. Octadecene (750 mL) was added followed by oleic acid (25.3 g).

[0129] The feed composition was pumped through the tubular reactor as described in Table 1 at a rate of 2 ml / min. The tubular reactor was immersed in a DURATHERM S oil bath heated at 300°C. The residence time (ie, the time the reacting stream is within the portion of the tube submerged in oil) was 38 minutes. Reactor conditions are summarized in Table 2. The product was a black solution.

[0130] Particles in the reactor product were washed according to Separation Method 1. Two drops of the resulting dispersion were diluted in 2 ml of hexane. The sample was evaluated using TEM and XRD. Representative TEM images are shown in image 3 middle. The magnification is 300,000X. The characterization results are summarized in Table 3.

example 2

[0132] The feed composition was prepared by adding iron oleate precursor (92.4 grams), which was prepared as described in Preliminary Example 1, to a plastic container. Octadecene (412 g) was added followed by oleic acid (14.2 g).

[0133] The feed composition was pumped through the tubular reactor as described in Table 1 at a rate of 2 ml / min. The tubular reactor was immersed in a DURATHERM S oil bath heated at 300°C. The residence time was 38 minutes. Reactor conditions are summarized in Table 2. The product was a black solution.

[0134] The drops of reactor effluent were diluted in hexane at a concentration of 1-10 drops / ml. The samples were evaluated using TEM. The characterization results are summarized in Table 3.

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Abstract

Methods of preparing metal oxide nanoparticles are described. The methods involve the thermal decomposition of a metal-carboxylate complex within a continuous, flow-through, tubular reactor. The resulting metal oxide nanoparticles contain iron and can be magnetic, non-agglomerated, crystalline or a combination thereof.

Description

technical field [0001] The present invention describes methods for preparing metal oxide nanoparticles. Background technique [0002] Various methods have been proposed for the preparation of iron-containing metal oxide nanoparticles. Some of these methods involve the formation of iron-containing complexes followed by thermal decomposition of the iron-containing complexes. However, these methods have proven problematic when large quantities (eg, 100 grams or more) of nanoparticles are required. More specifically, preparing large quantities of iron-containing metal oxide nanoparticles having a relatively uniform particle size distribution (eg, particles having an average particle size no greater than about 100 nanometers) is difficult. Contents of the invention [0003] The present invention describes methods for preparing iron-containing metal oxide nanoparticles. The process involves the thermal decomposition of iron-carboxylate complexes in a continuous, flow-through,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/00C01G49/08
CPCC01G49/08C01P2004/64C01P2004/04C01G49/0018B82Y30/00
Inventor 萨拉·M·马林斯格兰特·F·蒂芬布鲁克丹尼·B·安德森
Owner 3M INNOVATIVE PROPERTIES CO
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