WO2008136855A2 - Metal oxide nanocrystal composition and methods - Google Patents
Metal oxide nanocrystal composition and methods Download PDFInfo
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- WO2008136855A2 WO2008136855A2 PCT/US2007/083804 US2007083804W WO2008136855A2 WO 2008136855 A2 WO2008136855 A2 WO 2008136855A2 US 2007083804 W US2007083804 W US 2007083804W WO 2008136855 A2 WO2008136855 A2 WO 2008136855A2
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Definitions
- the present disclosure relates generally to synthesis of nanocrystals. More specifically, the present disclosure relates to improved methods of making magnetic nanocrystals.
- Magnetic nanocrystals including magnetite (Fe 3 O 4 ) and maghemite ( ⁇ Fe 2 O 3 ), have been intensively studied because of their unique and tunable magnetic properties. Their magnetic features have found wide spread use in applications including, but not limited to, environmental remediation, magnetic recording and magnetic resonance imaging. For all applications, synthetic techniques which provide, among other things, precise control over nanocrystal grain size may be useful in that they permit engineering of the magnetic properties (e.g. superparamagnetic versus paramagnetic). Additionally, in many cases large quantities of highly monodisperse materials may ultimately be required in order to enable large scale testing and development. Production of nanocrystals with large and permanent magnetic dipole moments may be required for magnetic separations, and such particles may have diameters from about 10 to about 25 nm.
- the present disclosure relates generally to synthesis of nanocrystals. More specifically, the present disclosure relates to improved methods of making magnetic nanocrystals.
- the present disclosure relates to a method of making magnetic nanocrystals, the method comprising: providing a metal component comprising at least one metal component selected from the group consisting of: a metal oxide; a metal hydroxide; a metal hydrate; and any combination thereof; providing an oil comprising a free acid; and reacting the metal component and the oil having a free acid at a temperature sufficient to form metal oxide nanocrystals.
- Figure 1 shows a transmission electron microscopy (TEM) image of metal oxide nanocrystals.
- Figure 2 shows magnetite nanocrystal synthesis from FeOOH and (a) oleic acid, 10.84 ⁇
- Figure 3 shows magnetite synthesis with FeOOH and oleic acid (a) in ODE, 12.04 ⁇ 1.23 nm, (b) with no ODE, 66.80 ⁇ 13.56 nm. While the present disclosure is susceptible to various modifications and alternative forms, specific example embodiments have been shown in the figures and are herein described in more detail. It should be understood, however, that the description of specific example embodiments is not intended to limit the invention to the particular forms disclosed, but on the contrary, this disclosure is to cover all modifications and equivalents as illustrated, in part, by the appended claims.
- the present disclosure relates generally to synthesis of nanocrystals. More specifically, the present disclosure relates to improved methods of making magnetic nanocrystals.
- the present disclosure provides, according to certain embodiments, a method of making magnetic nanocrystals, the method comprising: providing a metal component comprising at least
- HOU02:1120468 one metal component selected from the group consisting of: a metal oxide; a metal hydroxide; a metal hydrate; and any combination thereof; providing an oil comprising a free acid; and reacting the metal component and the oil having a free acid at a temperature sufficient to form metal oxide nanocrystals.
- the methods of the present disclosure may benefit from, among other things, the use of environmentally friendly and relatively inexpensive starting materials.
- the metal oxide nanocrystals formed, although relatively inexpensive to produce, may be of a high quality and monodisperse.
- Such metal oxide nanocrystals may be used in applications including, but not limited to, water treatment (e.g., arsenic removal), magnetic resonance imaging (MRI), ferrofluids, data storage, sensors, medicinal and diagnostic imaging, drug delivery, catalysis, magnetic and optical devices, and protein separations.
- the metal component may comprise any metal component suitable for the production of metal oxide nanocrystals by reaction with an oil comprising a free acid.
- metal components include, but are not limited to, a metal oxide, a metal hydroxide or a metal hydrate.
- Such metal oxides, metal hydroxides, and metal hydrates may comprise titanium (Ti), zinc (Zn), nickel (Ni), manganese (Mn), cadmium (Cd), and any combination thereof.
- the metal component comprises iron oxide-hydrates, commonly referred to as "rust.”
- rust iron oxide-hydrates
- the metal component may be ground into a fine powder before reaction with the oil.
- One of ordinary skill in the art with the benefit of the present disclosure, may recognize additional metal components that may be suitable for use in the methods of the present disclosure. Such metal components are still considered within the spirit of the present disclosure.
- the oil comprising a free acid may be any oil comprising a free acid and suitable for use in the production of metal oxide nanocrystals by reaction with a metal component.
- the oil comprising a free acid may be a naturally occurring oil.
- suitable oils include, but are not limited to, olive oil (glyceryl trioleate and/or oleic acid), coconut oil, corn oil, vegetable oil, oleic acid ((9Z)-octadec-9-enoic acid), linoleic acid ((9Z, 12Z)- octadeca-9, 12-dienoic acid), stearic acid (octadecanoic acid), palmitic acid (hexadecanoic acid), and any combination thereof.
- the metal component may be mixed with the oil having a free acid, such as olive oil, to form a 0.1M solution.
- HOU02:11 2 0468 skill in the art may recognize additional oils that may be suitable for use in the methods of the present disclosure. Such oils are still considered within the spirit of the present disclosure.
- a solvent may be used in the synthesis of metal oxide nanocrystals.
- a solvent may be used, among other things, to tailor the size of the metal oxide nanocrystals.
- ODE 1-octadecene
- heat may be applied in an amount sufficient to produce a crystalline structure.
- a temperature sufficient to produce a crystalline structure may be about 35O°C.
- the metal oxide nanocrystals formed by the methods of the present disclosure may be purified following their synthesis.
- the resulting metal oxide nanocrystals may be separated from the solution using any technique suitable for such a separation.
- An example of such a suitable separation technique comprises the use of a polar solvent followed by centrifugation and extraction with a hydrocarbon based solvent, such as hexane.
- a hydrocarbon based solvent such as hexane.
- Table 1 shows the reactants and reaction temperature for a number of test samples.
- Table 2 shows the reaction time, as well as any observations pertaining to magnetism and TEM images.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
Improved methods of making magnetic nanocrystals are provided. According to certain embodiments, a method of making magnetic nanocrystals is provided, the method comprising: providing a metal component comprising at least one metal component selected from the group consisting of: a metal oxide; a metal hydroxide; a metal hydrate; and any combination thereof; providing an oil comprising a free acid; and reacting the metal component and the oil comprising a free acid at a temperature sufficient to form metal oxide nanocrystals.
Description
METAL OXIDE NANOCRYSTAL COMPOSITIONS AND METHODS
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application Serial No. 60/864,780 filed November 7, 2006, which is incorporated by reference herein.
STATEMENT OF GOVERNMENT INTEREST
This disclosure was made with support under grant numbers EEC-0118007 and EEC- 0647452 awarded by the National Science Foundation. The U.S. government has certain rights in the invention.
BACKGROUND The present disclosure relates generally to synthesis of nanocrystals. More specifically, the present disclosure relates to improved methods of making magnetic nanocrystals.
Magnetic nanocrystals, including magnetite (Fe3O4) and maghemite (γ Fe2O3), have been intensively studied because of their unique and tunable magnetic properties. Their magnetic features have found wide spread use in applications including, but not limited to, environmental remediation, magnetic recording and magnetic resonance imaging. For all applications, synthetic techniques which provide, among other things, precise control over nanocrystal grain size may be useful in that they permit engineering of the magnetic properties (e.g. superparamagnetic versus paramagnetic). Additionally, in many cases large quantities of highly monodisperse materials may ultimately be required in order to enable large scale testing and development. Production of nanocrystals with large and permanent magnetic dipole moments may be required for magnetic separations, and such particles may have diameters from about 10 to about 25 nm.
There has been much interest in the development of synthetic methods to produce high quality iron oxide systems. Many traditional approaches to iron oxide colloids have relied on the aqueous precipitation or hydrolysis of Fe2+ and/or Fe3+ salt(s); these materials, however, can be poorly crystalline and polydisperse in many cases. Recently, high quality iron oxide nanomaterials have been generated using high temperature solution phase methods similar to those used for semiconductor quantum dots.
HOU02: 1120468
SUMMARY
The present disclosure relates generally to synthesis of nanocrystals. More specifically, the present disclosure relates to improved methods of making magnetic nanocrystals.
In certain embodiments, the present disclosure relates to a method of making magnetic nanocrystals, the method comprising: providing a metal component comprising at least one metal component selected from the group consisting of: a metal oxide; a metal hydroxide; a metal hydrate; and any combination thereof; providing an oil comprising a free acid; and reacting the metal component and the oil having a free acid at a temperature sufficient to form metal oxide nanocrystals. DRAWINGS
Some specific example embodiments of the disclosure may be understood by referring, in part, to the following description and the accompanying drawings.
Figure 1 shows a transmission electron microscopy (TEM) image of metal oxide nanocrystals. Figure 2 shows magnetite nanocrystal synthesis from FeOOH and (a) oleic acid, 10.84 ±
0.55 nm, (b) cone, oleic acid, 9.41 ± 0.92 nm, (c) stearic acid, 8.90 ± 0.60 nm, (d) linoleic acid, 7.68 ± 1.47 nm, and 1-octadecene.
Figure 3 shows magnetite synthesis with FeOOH and oleic acid (a) in ODE, 12.04 ± 1.23 nm, (b) with no ODE, 66.80 ± 13.56 nm. While the present disclosure is susceptible to various modifications and alternative forms, specific example embodiments have been shown in the figures and are herein described in more detail. It should be understood, however, that the description of specific example embodiments is not intended to limit the invention to the particular forms disclosed, but on the contrary, this disclosure is to cover all modifications and equivalents as illustrated, in part, by the appended claims.
DESCRIPTION
The present disclosure relates generally to synthesis of nanocrystals. More specifically, the present disclosure relates to improved methods of making magnetic nanocrystals.
The present disclosure provides, according to certain embodiments, a method of making magnetic nanocrystals, the method comprising: providing a metal component comprising at least
HOU02:1120468
one metal component selected from the group consisting of: a metal oxide; a metal hydroxide; a metal hydrate; and any combination thereof; providing an oil comprising a free acid; and reacting the metal component and the oil having a free acid at a temperature sufficient to form metal oxide nanocrystals. The methods of the present disclosure may benefit from, among other things, the use of environmentally friendly and relatively inexpensive starting materials. The metal oxide nanocrystals formed, although relatively inexpensive to produce, may be of a high quality and monodisperse. Such metal oxide nanocrystals may be used in applications including, but not limited to, water treatment (e.g., arsenic removal), magnetic resonance imaging (MRI), ferrofluids, data storage, sensors, medicinal and diagnostic imaging, drug delivery, catalysis, magnetic and optical devices, and protein separations.
The metal component may comprise any metal component suitable for the production of metal oxide nanocrystals by reaction with an oil comprising a free acid. Examples of such metal components include, but are not limited to, a metal oxide, a metal hydroxide or a metal hydrate. Such metal oxides, metal hydroxides, and metal hydrates may comprise titanium (Ti), zinc (Zn), nickel (Ni), manganese (Mn), cadmium (Cd), and any combination thereof. In a specific example, the metal component comprises iron oxide-hydrates, commonly referred to as "rust." For metal components such as rust, the metal component may be ground into a fine powder before reaction with the oil. One of ordinary skill in the art, with the benefit of the present disclosure, may recognize additional metal components that may be suitable for use in the methods of the present disclosure. Such metal components are still considered within the spirit of the present disclosure.
The oil comprising a free acid may be any oil comprising a free acid and suitable for use in the production of metal oxide nanocrystals by reaction with a metal component. In certain embodiments, the oil comprising a free acid may be a naturally occurring oil. Examples of suitable oils include, but are not limited to, olive oil (glyceryl trioleate and/or oleic acid), coconut oil, corn oil, vegetable oil, oleic acid ((9Z)-octadec-9-enoic acid), linoleic acid ((9Z, 12Z)- octadeca-9, 12-dienoic acid), stearic acid (octadecanoic acid), palmitic acid (hexadecanoic acid), and any combination thereof. For example, in the case of rust, the metal component may be mixed with the oil having a free acid, such as olive oil, to form a 0.1M solution. One of ordinary
HOU02:1120468
skill in the art, with the benefit of the present disclosure, may recognize additional oils that may be suitable for use in the methods of the present disclosure. Such oils are still considered within the spirit of the present disclosure.
In certain embodiments, a solvent may be used in the synthesis of metal oxide nanocrystals. A solvent may be used, among other things, to tailor the size of the metal oxide nanocrystals. For example, 1-octadecene (ODE) may be used to achieve smaller metal oxide nanocrystals.
In certain embodiments, once the metal oxide or metal hydroxide or metal hydrate and oil comprising a free acid are mixed, heat may be applied in an amount sufficient to produce a crystalline structure. For example, when rust and olive oil are reacted, a temperature sufficient to produce a crystalline structure may be about 35O°C. In certain embodiments, the metal oxide nanocrystals formed by the methods of the present disclosure may be purified following their synthesis.
After the metal component and oil having a free acid are at least partially reacted, the resulting metal oxide nanocrystals may be separated from the solution using any technique suitable for such a separation. An example of such a suitable separation technique comprises the use of a polar solvent followed by centrifugation and extraction with a hydrocarbon based solvent, such as hexane. One of ordinary skill in the art, with the benefit of the present disclosure, will recognize additional separation techniques that may be suitable. Such additional separation techniques are still considered within the spirit of the present disclosure.
EXAMPLES Example 1
Table 1 shows the reactants and reaction temperature for a number of test samples. Table 2 shows the reaction time, as well as any observations pertaining to magnetism and TEM images.
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TABLE 1
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TABLE 2
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* These averages are estimates from about 40 particles.
HOU02: 1120468
Example 2
In an example synthesis, oil, vinegar, a pan, CRYSTAL DRAIN OPENER (sodium hydroxide; ROEBIC Laboratories, Orange, Connecticut) and rust were used. First, the oil, CRYSTAL DRAIN OPENER and water were mixed to form a soap. After curing for about 24 hours the soap solidified. For efficient dissolution in subsequent steps, the soap was ground into a fine powder and mixed with vinegar while heating on a conventional stove. Once the soap was dissolved, the solution forms two layers: a yellow (fatty acid) top layer and a cloudy white/yellow bottom layer. The solution was then heated at 110 0C to remove excess water and vinegar by-products. The clear yellow fatty acid components was then collected and mixed with rust. The resulting mixture was heated for 2 hours at below and near boiling temperatures. A TEM micrograph of the nanocrystals formed was obtained after magnetic separation in chloroform and is shown in Figure 2.
Therefore, the present invention is well adapted to attain the ends and advantages mentioned as well as those that are inherent therein. While numerous changes may be made by those skilled in the art, such changes are encompassed within the spirit of this invention as illustrated, in part, by the appended claims.
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Claims
1. A method for making metal oxide nanocrystals comprising: providing a metal component comprising at least one metal component selected from the group consisting of: a metal oxide; a metal hydroxide; a metal hydrate; and any combination thereof; providing an oil comprising a free acid; and reacting the metal component and the oil comprising a free acid at a temperature sufficient to form metal oxide nanocrystals.
2. The method of claim 1 wherein the metal component comprises an iron-oxide hydrate.
3. The method of claim 1 wherein the oil comprising a free acid is chosen from olive oil, coconut oil, corn oil, vegetable oil, oleic acid, linoleic acid, stearic acid, palmitic acid, and any combination thereof.
4. The method of claim 1 wherein the oil comprising a free acid comprises glycerol trioleate.
5. The method of claim 1 wherein the temperature sufficient to form metal oxide nanocrystals is about 3500C.
6. The method of claim 1 wherein reacting the metal component and the oil comprising a free acid at a temperature sufficient to form metal oxide nanocrystals further comprises reacting 1-octadecene with the metal component and the oil comprising a free acid.
7. The method of claim 1 further comprising purifying the metal oxide nanocrystals.
8. The method of claim 1, wherein the metal oxide or the metal hydroxide or the metal hydrate is rust, the oil having a free acid is olive oil, and the temperature sufficient to form metal oxide nanocrystals is about 35O0C.
HOU02: 1 120468
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US86478006P | 2006-11-07 | 2006-11-07 | |
| US60/864,780 | 2006-11-07 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| WO2008136855A2 true WO2008136855A2 (en) | 2008-11-13 |
| WO2008136855A3 WO2008136855A3 (en) | 2008-12-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US2007/083804 Ceased WO2008136855A2 (en) | 2006-11-07 | 2007-11-06 | Metal oxide nanocrystal composition and methods |
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| Country | Link |
|---|---|
| WO (1) | WO2008136855A2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9771275B2 (en) | 2013-12-06 | 2017-09-26 | Hanwha Chemical Corporation | Method for preparing uniform metal oxide nanoparticles with high reproducibility |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5746837A (en) * | 1992-05-27 | 1998-05-05 | Ppg Industries, Inc. | Process for treating an aluminum can using a mobility enhancer |
| US6262129B1 (en) * | 1998-07-31 | 2001-07-17 | International Business Machines Corporation | Method for producing nanoparticles of transition metals |
| US7531149B2 (en) * | 2003-10-14 | 2009-05-12 | The Board Of Trustees Of The University Of Arkansas | Synthetic control of metal oxide nanocrystal sizes and shapes |
-
2007
- 2007-11-06 WO PCT/US2007/083804 patent/WO2008136855A2/en not_active Ceased
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9771275B2 (en) | 2013-12-06 | 2017-09-26 | Hanwha Chemical Corporation | Method for preparing uniform metal oxide nanoparticles with high reproducibility |
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| Publication number | Publication date |
|---|---|
| WO2008136855A3 (en) | 2008-12-24 |
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