Name: manganese oxide nanoparticle synthesis by thermal decomposition of manganese(ii) acetylacetonate
Uploaded: 2020-06-18T15:00:00
Description: Watch this Scientific Journal Video about Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of ManganeseII Acetylacetonate at JoVE.com

This work was supported by WVU Chemical and Biomedical Engineering Department startup funds (M.F.B.). The authors would like to thank Dr. Marcela Redigolo for guidance on grid preparation and image capture of nanoparticles with TEM, Dr. Qiang Wang for support on evaluating XRD and FTIR spectra, Dr. John Zondlo and Hunter Snoderly for programming and integrating the temperature controller into the nanoparticle synthesis protocol, James Hall for his assistance in assembly of the nanoparticle synthesis setup, Alexander Pueschel and Jenna Vito for aiding in quantification of MnO nanoparticle diameters from TEM images, and the WVU Shared Research Facility for use of the TEM, XRD, and FTIR.

1. Glassware and tubing assembly &#8211; to be performed only the first time
NOTE: Figure 1 shows the experimental setup for MnO nanoparticle synthesis with numbered tubing connections. Figure S1 shows the same setup with the main glassware components labeled. If there is a mismatch between the chemical resistant tubing and the glass connection size, cover the glass connection first with a short piece of smaller tubing before adding the...

The protocol herein describes a facile, one-pot synthesis of MnO nanoparticles using Mn(II) ACAC, DE, and OA. Mn(II) ACAC is utilized as the starting material to provide a source of Mn2+ for MnO nanoparticle formation. The starting material can be easily substituted to enable production of other metal oxide nanoparticles. For example, when iron(III) ACAC is applied, Fe3O4 nanoparticles can be generated using the same nanoparticle synthesis equipment and protocol described<sup class="xref"...

Metal oxide nanoparticles possess magnetic, electric, and catalytic properties, which have been applied in bioimaging1,2,3, sensor technologies4,5, catalysis6,7,8, energy storage9, and water purification10. Within the biomedical field, iron oxide nanoparticles and manganese oxide (MnO) nanoparticles have proven utility as contrast agents in magnetic resonance imaging (MRI)1,2. Iron oxide nanoparticles produce robust negative contrast on T2* MRI and are powerful enough to visualize single labeled cells in vivo11,12,13; however, the negative MRI signal cannot be modulated and remains &#8220;ON&#8221; throughout the duration of typical experiments. Due to endogenous iron present in the liver, bone marrow, blood and spleen, the negative contrast generated from iron oxide nanoparticles may be difficult to interpret. MnO nanoparticles, on the other hand, are responsive to a drop in pH. MRI signal for MnO nanoparticles can transition from &#8220;OFF&#8221; to &#8220;ON&#8221; once the nanoparticles are internalized inside the low pH endosomes and lysosomes of the target cell such as a cancer cell14,15,16,17,18,19. The positive contrast on T1 MRI produced from the dissolution of MnO to Mn2+ at low pH is unmistakable and can improve cancer detection specificity by only lighting up at the target site within a malignant tumor. Control over nanoparticle size, morphology and composition is crucial to achieve maximum MRI signal from MnO nanoparticles. Herein, we describe how to synthesize and characterize MnO nanoparticles using the thermal decomposition method and note different strategies for fine-tuning nanoparticle properties by altering variables in the synthesis process. This protocol can be easily modified to produce other magnetic nanoparticles such as iron oxide nanoparticles.
MnO nanoparticles have been produced by a variety of techniques including thermal decomposition20,21,22,23,24,25, hydro/solvothermal26,27,28,29, exfoliation30,31,32,33,34, permanganates reduction35,36,37,38, and adsorption-oxidation39,40,41,42. Thermal decomposition is the most commonly used technique which involves dissolving manganese precursors, organic solvents, and stabilizing agents at high temperatures (180 &#8211; 360 &#176;C) under the presence of an inert gaseous atmosphere to form MnO nanoparticles43. Out of all of these techniques, thermal decomposition is the superior method to generate a variety of MnO nanocrystals of pure phase (MnO, Mn3O4 and Mn2O3) with a narrow size distribution. Its versatility is highlighted through the ability to tightly control nanoparticle size, morphology and composition by altering reaction time44,45,46, temperature44,47,48,49, types/ratios of reactants20,45,47,48,50 and inert gas47,48,50 used. The main limitations of this method are the requirement for high temperatures, the oxygen-free atmosphere, and the hydrophobic coating of the synthesized nanoparticles, which requires further modification with polymers, lipids or other ligands to increase solubility for biological applications14,51,52,53.
Besides thermal decomposition, the hydro/solvothermal method is the only other technique that can produce a variety of MnO phases including MnO, Mn3O4, and MnO2; all other strategies only form MnO2 products. During hydro/solvothermal synthesis, precursors such as Mn(II) stearate54,55 and Mn(II) acetate27 are heated to between 120-200 &#176;C over several hours to achieve nanoparticles with a narrow size distribution; however, specialized reaction vessels are required and reactions are performed at high pressures. In contrast, the exfoliation strategy involves treatment of a layered or bulk material to promote dissociation into 2D single layers. Its main advantage is in producing MnO2 nanosheets, but the synthesis process is long requiring several days and the resulting size of the sheets is difficult to control. Alternatively, permanganates such as KMnO4 can react with reducing agents such as oleic acid56,57, graphene oxide58 or poly(allylamine hydrochloride)59 to create MnO2 nanoparticles. Use of KMnO4 facilitates nanoparticle formation at room temperature over a few minutes to hours within aqueous conditions43. Unfortunately, the rapid synthesis and nanoparticle growth makes it challenging to finely control resulting nanoparticle size. MnO2 nanoparticles can also be synthesized using adsorption-oxidation whereby Mn2+ ions are adsorbed and oxidized to MnO2 by oxygen under basic conditions. This method will produce small MnO2 nanoparticles with a narrow size distribution at room temperature over several hours in aqueous media; however the requirement for adsorption of Mn2+ ions and alkali conditions limits its widespread application43.
Of the MnO nanoparticle synthesis methods discussed, thermal decomposition is the most versatile to generate different monodisperse pure phase nanocrystals with control over nanoparticle size, shape and composition without requiring specialized synthesis vessels. In this manuscript, we describe how to synthesize MnO nanoparticles by thermal decomposition at 280 &#176;C using manganese(II) acetylacetonate (Mn(II) ACAC) as the source of Mn2+ ions, oleylamine (OA) as the reducing agent and stabilizer, and dibenzyl ether (DE) as the solvent under a nitrogen atmosphere. The glassware and tubing setup for nanoparticle synthesis is explained in detail. One advantage of the technique is the inclusion of a temperature controller, thermocouple probe, and heating mantle to enable precise control over the heating rate, peak temperature, and reaction times at each temperature to fine-tune nanoparticle size and composition. Herein, we show how nanoparticle size can also be manipulated by changing the ratio of OA to DE. Additionally, we demonstrate how to prepare nanoparticle samples and measure nanoparticle size, bulk composition and surface composition using transmission electron microscopy (TEM), x-ray diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR), respectively. Further guidance is included on how to analyze the collected images and spectra from each instrument. To generate uniformly shaped MnO nanoparticles, a stabilizer and adequate nitrogen flow must be present; XRD and TEM results are shown for undesired products formed in the absence of OA and under low nitrogen flow. In the Discussion section, we highlight crucial steps in the protocol, metrics to determine successful nanoparticle synthesis, further variation of the decomposition protocol to modify nanoparticle properties (size, morphology and composition), troubleshooting and limitations of the method, and applications of MnO nanoparticles as contrast agents for biomedical imaging.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Chemicals and Gases</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Benzyl ether (DE)</td>
			<td>Acros Organics</td>
			<td>AC14840-0010</td>
			<td>Concentration: 99%, 1 L</td>
		</tr>
		<tr>
			<td>Drierite</td>
			<td>W. A. Hammond Drierite Co. LTD</td>
			<td>23001</td>
			<td>Drierite 8 mesh, 1 lb</td>
		</tr>
		<tr>
			<td>Ethanol</td>
			<td>Decon Laboratories&#160;</td>
			<td>2701</td>
			<td>200 proof, 4 x 3.7 L</td>
		</tr>
		<tr>
			<td>Hexane</td>
			<td>Macron Fine Chemicals</td>
			<td>5189-08</td>
			<td>Concentration:&#160; &#8805;98.5%, 4 L</td>
		</tr>
		<tr>
			<td>Hydrochloric acid</td>
			<td>VWR</td>
			<td>BDH3030-2.5LPC</td>
			<td>Concentration: 36.5 - 38.0 % ACS, 2.5 L</td>
		</tr>
		<tr>
			<td>Manganese (II) acetyl acetonate (Mn(II)ACAC)</td>
			<td>Sigma Aldrich</td>
			<td>245763-100G</td>
			<td>100 g</td>
		</tr>
		<tr>
			<td>Nitrogen gas tank</td>
			<td>Airgas</td>
			<td>NI R300</td>
			<td>Research 5.7 grade nitrogen, size 300 cylinder</td>
		</tr>
		<tr>
			<td>Nitrogen regulator</td>
			<td>Airgas</td>
			<td>Y11244D580-AG</td>
			<td>Single stage brass 0-100 psi analytical cylinder regulator CGA-580 with needle outlet</td>
		</tr>
		<tr>
			<td>Oleylamine (OA)</td>
			<td>Sigma Aldrich</td>
			<td>O7805-500G</td>
			<td>Concentration: 70%, technical grade, 500 g</td>
		</tr>
		<tr>
			<td>Silicone oil</td>
			<td>Beantown Chemical</td>
			<td>221590-100G</td>
			<td>100 g</td>
		</tr>
		<tr>
			<td>Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge</td>
			<td>Beckman-Coulter</td>
			<td>Avanti J-E</td>
			<td>JA-20 fixed-angle aluminum rotor, 8 x 50 mL, 48,400 x g</td>
		</tr>
		<tr>
			<td>Hemisphere mantle</td>
			<td>Ace Glass Inc.</td>
			<td>12035-17</td>
			<td>115 V, 270 W, 500 mL, temperature up to 450 &#176;C</td>
		</tr>
		<tr>
			<td>Hot plate stirrer</td>
			<td>VWR</td>
			<td>97042-642</td>
			<td>120 V, 1000 W, 8.3 A, ceramic top</td>
		</tr>
		<tr>
			<td>Temperature controller</td>
			<td>Yokogawa Electric Corporation</td>
			<td>UP351</td>
			<td></td>
		</tr>
		<tr>
			<td>Temperature probe</td>
			<td>Omega</td>
			<td>KMQXL-040G-12</td>
			<td>Immersion probe, temperature up to 1335 &#176;C</td>
		</tr>
		<tr>
			<td>Vacuum oven</td>
			<td>Fisher Scientific</td>
			<td>282A</td>
			<td>120 V, 1800 W, temperature up to 280 &#176;C</td>
		</tr>
		<tr>
			<td>Vortex mixer</td>
			<td>Fisher Scientific</td>
			<td>02-215-365</td>
			<td>120 V, 50/60 Hz, 150 W</td>
		</tr>
		<tr>
			<td>Water bath sonicator</td>
			<td>Fisher Scientific</td>
			<td>FS30H</td>
			<td>Ultrasonic power 130 W, 3.7 L tank</td>
		</tr>
		<tr>
			<td>Tools and Materials</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Dumont tweezer</td>
			<td>Electron Microscopy Sciences</td>
			<td>72703D</td>
			<td>Style 5/45, Dumoxel, 109 mm, for picking up TEM grids</td>
		</tr>
		<tr>
			<td>Dumont reverse tweezer</td>
			<td>Ted Pella</td>
			<td>5748</td>
			<td>Style N2a, 118 mm, NM-SS, self-closing, holding TEM grids in place for sample preparation</td>
		</tr>
		<tr>
			<td>Mortar and pestle</td>
			<td>Amazon</td>
			<td>BS0007</td>
			<td>BIPEE agate mortar and pestle, 70 X 60 X 15 mm labware</td>
		</tr>
		<tr>
			<td>Nalgene&#8482; Oak Ridge tubes</td>
			<td>ThermoFisher Scientific</td>
			<td>3139-0050</td>
			<td>Polypropylene copolymer, 50,000 x g, 50 mL, pack of 10</td>
		</tr>
		<tr>
			<td>Scintillation vials</td>
			<td>Fisher Scientific</td>
			<td>03-337-4</td>
			<td>20 mL vials with white caps, case of 500</td>
		</tr>
		<tr>
			<td>TEM grids</td>
			<td>Ted Pella</td>
			<td>01813-F</td>
			<td>Carbon Type-B, 300 mesh, copper, pack of 50</td>
		</tr>
		<tr>
			<td>Glassware Setup</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>4-neck round bottom flask</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-1534-01</td>
			<td>24/40 joint, 500 mL, #7 chem thread for thermometers</td>
		</tr>
		<tr>
			<td>6-port vacuum manifold</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-4430-02</td>
			<td>480 nm, 6 ports, 4 mm PTFE stopcocks</td>
		</tr>
		<tr>
			<td>Adapter</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-1014-01</td>
			<td>24/40 inner joint, 90&#176;</td>
		</tr>
		<tr>
			<td>Condenser</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-1216-03</td>
			<td>24/40 joint, 365 mm, 250 mm jacket length</td>
		</tr>
		<tr>
			<td>Drierite 26800 drying column</td>
			<td>Cole-Parmer&#160;</td>
			<td>EW-07193-00</td>
			<td>200 L/hr, 90 psi</td>
		</tr>
		<tr>
			<td>Funnel</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-1720-L-02</td>
			<td>24/40 joint, 100 powder funnel, 195 mm OAL</td>
		</tr>
		<tr>
			<td>Interlocked worm gear hose clamp</td>
			<td>Grainger</td>
			<td>16P292</td>
			<td>1/2&#34; wide stainless steel clamp, 3/8&#34; to 7/8&#34; diameter, to secure condenser tubing, 10 pack&#160;</td>
		</tr>
		<tr>
			<td>Keck clips</td>
			<td>Kemtech America Inc</td>
			<td>CS002440</td>
			<td>24/40 joint</td>
		</tr>
		<tr>
			<td>Metal claw clamp</td>
			<td>Fisher Scientific</td>
			<td>05-769-7Q</td>
			<td>22cm, three-prong extension clamps</td>
		</tr>
		<tr>
			<td>Metal claw clamp holder</td>
			<td>Fisher Scientific</td>
			<td>05-754Q</td>
			<td>Clamp regular holder</td>
		</tr>
		<tr>
			<td>Mineral oil bubbler</td>
			<td>Kemtech America Inc</td>
			<td>B257040</td>
			<td>185 mm</td>
		</tr>
		<tr>
			<td>Rotovap trap</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-1319-02</td>
			<td>24/40 joints, 100 mL, self washing rotary evaporator</td>
		</tr>
		<tr>
			<td>Rubber stopper</td>
			<td>Chemglass Life Sciences</td>
			<td>CG-3022-98</td>
			<td>24/40 joints, red rubber</td>
		</tr>
		<tr>
			<td>Tubing for air/water&#160;</td>
			<td>McMaster-Carr</td>
			<td>6516T21</td>
			<td>Clear Tygon PVC for air/water, B-44-3, 1/4&#34; ID, 1/16&#34; wall, 25 ft</td>
		</tr>
		<tr>
			<td>Tubing for air/water&#160;</td>
			<td>McMaster-Carr</td>
			<td>6516T26</td>
			<td>Clear Tygon PVC for air/water, B-44-3, 3/8&#34; ID, 1/16&#34; wall, 25 ft</td>
		</tr>
		<tr>
			<td>Tubing for chemicals</td>
			<td>McMaster-Carr</td>
			<td>5155T34</td>
			<td>Clear Tygon PVC for chemicals, E-3603, 3/8&#34; ID, 1/16&#34; wall, 50 ft</td>
		</tr>
		<tr>
			<td>Analysis Programs</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>XRD analysis program</td>
			<td>Malvern Panalytical</td>
			<td>N/A</td>
			<td>X&#39;Pert HighScore Plus</td>
		</tr>
		<tr>
			<td>FTIR analysis program</td>
			<td>Varian, Inc.</td>
			<td>N/A</td>
			<td>Varian Resolutions Pro</td>
		</tr>
	</tbody>
</table>

manganese oxide nanoparticle synthesis by thermal decomposition of manganese(ii) acetylacetonate

For biomedical applications, metal oxide nanoparticles such as iron oxide and manganese oxide (MnO), have been used as biosensors and contrast agents in magnetic resonance imaging (MRI). While iron oxide nanoparticles provide constant negative contrast on MRI over typical experimental timeframes, MnO generates switchable positive contrast on MRI through dissolution of MnO to Mn2+ at low pH within cell endosomes to &#8216;turn ON&#8217; MRI contrast. This protocol describes a one-pot synthesis of MnO nanoparticles formed by thermal decomposition of manganese(II) acetylacetonate in oleylamine and dibenzyl ether. Although running the synthesis of MnO nanoparticles is simple, the initial experimental setup can be difficult to reproduce if detailed instructions are not provided. Thus, the glassware and tubing assembly is first thoroughly described to allow other investigators to easily reproduce the setup. The synthesis method incorporates a temperature controller to achieve automated and precise manipulation of the desired temperature profile, which will impact resulting nanoparticle size and chemistry. The thermal decomposition protocol can be readily adapted to generate other metal oxide nanoparticles (e.g., iron oxide) and to include alternative organic solvents and stabilizers (e.g., oleic acid). In addition, the ratio of organic solvent to stabilizer can be changed to further impact nanoparticle properties, which is shown herein. Synthesized MnO nanoparticles are characterized for morphology, size, bulk composition, and surface composition through transmission electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy, respectively. The MnO nanoparticles synthesized by this method will be hydrophobic and must be further manipulated through ligand exchange, polymeric encapsulation, or lipid capping to incorporate hydrophilic groups for interaction with biological fluids and tissues.

To confirm successful synthesis, MnO nanoparticles should be assayed for size and morphology (TEM), bulk composition (XRD), and surface composition (FTIR). Figure 2 shows representative TEM images of MnO nanoparticles synthesized using decreasing ratios of oleylamine (OA, the stabilizer) to dibenzyl ether (DE, the organic solvent): 60:0, 50:10, 40:20, 30:30, 20:40, 10:50. Ideal TEM images consist of individual nanoparticles (shown as dark rounded octagons in Figure 2</st...

Watch this Scientific Journal Video about Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of ManganeseII Acetylacetonate at JoVE.com

Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of ManganeseII Acetylacetonate

This protocol details a facile, one-pot synthesis of manganese oxide (MnO) nanoparticles by thermal decomposition of manganese(II) acetylacetonate in the presence of oleylamine and dibenzyl ether. MnO nanoparticles have been utilized in diverse applications including magnetic resonance imaging, biosensing, catalysis, batteries, and waste water treatment.

Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of Manganese(II) Acetylacetonate

For biomedical applications, metal oxide nanoparticles such as iron oxide and manganese oxide (MnO), have been used as biosensors and contrast agents in ...

Compared to other synthesis methods, thermal decomposition generates uniform metal oxide nano-particles with tight control over particle size, shape, and chemical composition. This technique is an easy one pot synthesis that uses three reagents, a metal precursor, an organic solvent and a stabilizer. It can produce different types of nano-particles including manganese oxide and iron oxide.Demonstrating the procedure will be Celia Martinez De La Torre, a graduate research assistant in my laboratory. Before beginning an experiment, place a four neck 500 milliliter round bottom flask onto the heating mantle. And secure the middle neck with a metal claw clamp.Add magnetic stir bar to the round bottom flask and place a glass funnel in the middle neck of the flask. Make sure the safety and input stopcocks are open. Add 1.51 grams of manganese II acetylacetonate through the funnel into the round bottom flask.And add 20 milliliters of allylamine and 40 milliliters of di-benzyl ether to the flask. Attach a condenser to the left neck of the flask and use a metal claw clamp to secure the condenser to the flask. Add the glass elbow adapter to the top of the condenser and attach the rotovap trap to the right neck of the round bottom flask.Lace the glass elbow adaptor on top of the rotovap trap. And fold the rubber stopper on the middle neck of the round bottom flask. So the sides cover the neck of the flask.Use plastic conical joint clips to secure the glassware neck connections. And place the temperature probe into the smallest neck in the brown bottom flask. Use a neck cap and an O-ring to tighten and secure the probe and the reaction mixture without touching the glass.And connect the temperature probe to the input of the temperature controller. Connect the heating mantle to the output of the temperature controller and turn on the stir plate to begin vigorous stirring of the solution. Open the air free nitrogen tank to slowly begin flowing nitrogen into the system and use the regulator to adjust the flow until a steady stream of bubbles forms in the middle of mineral oil bubbler.Then turn on the cold water in the fume hood to the condenser and close this For nanoparticle synthesis turn on the temperature controller to start the reaction. And monitor the changes that occur in the temperature throughout the experiment. At 280 degrees Celsius turn off the nitrogen tank and close the right stopcock.The temperature will be held at 280 degrees Celsius for 30 minutes. During this time, the reaction color will change to a green tone indicating manganese oxide formation. When the reaction is cool to room temperature, turn off the temperature controller, stir plate and water and decant the manganese oxide nano-particles solution into a clean 500 milliliter beaker.Add two times the volume of 200 proof ethanol to the beaker. And split the nanoparticle mixture equally between four centrifuge tubes. After capping sediment the nano-particles by centrifugation and discard the brown clear supernatant.Add five milliliters of hexane to each tube. And re-suspend the nano-particles by vortexing. Add any extra nano-particles solution and the 200 proof ethanol to the tubes until each is three quarters full and centrifuge the nano-particles again.Re-suspend each tube of nano-particles in five milliliters of hexane with vortexing and pool the four tubes of solution into two tubes. Bring the volume in each tube up to three quarters full with 200 proof ethanol and centrifuge the nano-particles again. Discard the nearly colorless and clear a supernatant.And re-suspend the nano-particles in five milliliters of hexane with vortexing. Pour the entire volume of both tubes into a 20 milliliter glass scintillation vile. And evaporate the hexane in a fume hood overnight.The next morning place the vile at 100 degrees Celsius for 24 hours to dry out the nano-particles before using a spatula to break up the powder. To assess the nano-particle size and surface morphology, use a mortar and pestle to pulverize the manganese oxide nano-particles into a thin powder, and add five milligrams of the powder to a 15 milliliter conical centrifuge tube. Add 10 milliliters of 200 proof ethanol to the tube and bath sonicate the nanoparticle mixture for five minutes until the nano-particles are fully re-suspended.Immediately upon re-suspension, add three five microliter drops of nano-particle solution into a 300 mesh copper grid support film of carbon type B.After air drying assess the nanoparticle shape and size by TEM according to standard protocols with a beam strength of 200 kilovolts a spot size of one and a 300 X magnification. To determine the nanoparticle bulk composition, use a spatula to transfer some of the fine nanoparticle powder onto an x-ray diffraction sample holder. And collect the x-ray diffraction spectra of the manganese oxide particles according to standard protocols.Use a two theta range from 10 to 110 degrees to view the manganese oxide and manganese to three oxide peaks. To determine the nanoparticle surface composition add dry manganese oxide nanoparticle powder to an FTIR sample holder and collect the FTIR spectrum of the nano-particles according to standard protocols between the 4, 400 inverse centimeter wavelength range with a four centimeter resolution. Ideal TEM images consist of individual dark rounded octagonal nano-particles with minimal overlap.If a high concentration of manganese oxide nano-particles are suspended in ethanol, or too many drops of nano-particles suspension are added to the T and grid each image will consist of large agglomerations of nano-particles. If a low nano-particle concentration is prepared in ethanol the nano-particles will be separated but too sparsely distributed on the TEM grid. Overall, a decrease in the ratio of allylamine di benzyl ether yields smaller manganese oxide nano-particles with less variation in size, except when allylamine alone is used producing similar size nano-particles to the 30 30 ratio.X-ray diffraction can be used to determine the crystal structure and phase of the nano-particles. The x-ray diffraction sample peaks can then be matched to x-ray diffraction peaks from known compounds. To facilitate estimation of the nanoparticle composition, here FTIR spectrum manganese oxide nano-particles after background correction can be observed.All spectra show the symmetric and asymmetric methylene peaks associated with groups. In addition to the aminal radicle bending vibration peaks associated with groups. Furthermore, all nanoparticle FTIR spectra contain manganese oxygen and manganese oxygen manganese bond vibrations around 600 inverse centimeters which confirmed the composition found through x-ray diffraction.To ensure an accurate temperature reading, the temperature probe do not touch the glass. The level of silicone oil and rate of nitrogen flow should also be carefully monitored. Metal oxide nano-particles can be made hydrophilic through polymer or lipid encapsulation to enhance their biocompatibility.Targeting agents can be also touch to light nanoparticle accumulation in vivo.

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