Name: in situ characterization of boehmite particles in water using liquid sem
Uploaded: 2017-09-27T13:00:00
Description: Watch this Scientific Journal Video about In Situ Characterization of Boehmite Particles in Water Using Liquid SEM at JoVE.com

We are grateful to the Pacific Northwest National Laboratory (PNNL) Nuclear Process Science Initiative (NPSI)-Laboratory Directed Research and Development (LDRD) fund for support. Dr. Sayandev Chatterjee provided the synthesized boehmite particles. Instrumental access was provided through a W. R. Wiley Environmental Molecular Sciences Laboratory (EMSL) General User Proposal. EMSL is a national scientific user facility sponsored by the Office of Biological and Environmental Research (BER) at PNNL. PNNL is operated by Battelle for the DOE under Contract DE-AC05-76RL01830.

1. Prepare AlOOH Liquid Sample
NOTE: Do not touch the specimen or anything inside the SEM chamber with bare hands. Powder free gloves should be worn at all times when handling the SALVI device and mounting it onto the SEM stage in order to avoid potential contamination during surface analysis.
<ol>
	<li>Make an AlOOH stock solution (1 mg/mL)
	<ol>
		<li>Dissolve 10 mg of AlOOH powder in 10 mL DI water to make the 1 mg/mL AlOOH stock solution.</li>
		<li>Ultrasonicate the sto...

<ol>
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SEM is a powerful technique in surface characterization of organic and inorganic materials on a nanoscale (nm) level with high resolution1. For example, it is widely used for analyzing the solid and dry samples such as geological materials26 and semiconductor27. However, it has limitations in characterizing the wet and liquid samples due to the incompatibility of liquid within the highly vacuumed environment required for electron microscopy<sup class...

Scanning Electron Microscope (SEM) has been widely applied to investigate a variety of specimens by producing high resolution imaging1. The energy dispersive x-ray spectroscopy (EDX) associated with the SEM enables the determination of elemental composition1. Traditionally, SEM is applied for imaging only dry and solid samples. In the last 30 years, Environmental SEM (ESEM) was developed for analyzing the partial hydrated samples in a vapor environment2,3,4,5. However, ESEM is unable to image the wet, fully fluid samples with desired high resolution6. Wet SEM cells were also developed to image wet specimens using SEM7,8; nevertheless, these cells were developed mainly for biological specimens and backscattered electron imaging, and are more accessible for applications with those designs9,10.
To address the challenges in analyzing various samples in their native liquid environment using SEM, we invented a vacuum compatible microfluidic device, System for Analysis at the Liquid Vacuum Interface (SALVI), to enable high spatial resolution secondary electron (SE) imaging and elemental analysis of liquid samples using the high vacuum mode in SEM. This novel technique includes the following unique features: 1) liquid is directly probed in a small aperture of 1 - 2 &#181;m in diameter; 2) liquid is held within the hole by surface tension; and 3) SALVI is portable and can be adapted to more than one analytical platform11,12,13,14,15,16,17,18.
SALVI consists of a 100 nm thick silicon nitride (SiN) membrane and a 200 &#181;m wide microchannel made of polydimethylsiloxane (PDMS) block. The SiN membrane window is applied to seal the microchannel. The fabrication details and key design considerations were detailed in previous papers and patents11,19,20. Currently, a leading manufacturer and distributor of consumable supply for microscopy has purchased the license to sell SALVI devices commercially for liquid SEM applications21,22.
The applications of SALVI in vacuum-based analytical instruments have been demonstrated using a variety of aqueous solutions and complex liquid mixtures including biofilms, mammalian cells, nanoparticles, and electrode materials12,14,17,20,23,24. However, most of the aforementioned work utilized time-of-flight secondary ion mass spectrometry (ToF-SIMS) as the key analysis tool, thus the application of liquid SEM with SALVI has not been explored fully. In this work, SALVI has been used to study larger non-spherical colloidal particles in liquid using liquid SEM imaging and EDX elemental analysis. The sample consists of AlOOH particles synthesized at our laboratory. Submicrometer-sized boehmite particles are known to exist in high-level radioactive waste at the Hanford site. They are slow to dissolve and may cause rheological problems in waste treatment. Therefore, it is important to have the capability to characterize boehmite particles in liquid25. This technical approach can be used to study boehmite in various physicochemical conditions for improved understanding of these particles and related rheological properties. These particles were utilized to demonstrate step-by-step how to apply SALVI to high vacuum SEM in order to study particles suspended in liquid. Key technical points for SALVI and SEM integration and SEM data acquisition are highlighted within the paper.
The protocol provides demonstration of the liquid sample analysis using SALVI and liquid SEM imaging, for those who are interested in utilizing this novel technique in diverse applications of liquid SEM in the future.

<table width="2033">
	<tbody>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Carbon Coater</td>
			<td style="width:311px;">Cressington</td>
			<td style="width:196px;">208 Carbon</td>
			<td style="width:1237px;">It is accompanied with thickness monitor MTM-10.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">SEM</td>
			<td style="width:311px;">FEI</td>
			<td>Quanta 3D FEG</td>
			<td style="width:1237px;">It provides highly resolved scanning electron microscopy and elemental analysis.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">System for Analysis at the Liquid Vacuum Interface (SALVI)</td>
			<td style="width:311px;">Pacific Northwest National Laboratory</td>
			<td>N/A</td>
			<td style="width:1237px;">SALVI is a unique, vacuum compatible microfluidic cell that enables the characterization of the liquid sample using vacuu- based scientific instrument.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">PEEK Union</td>
			<td style="width:311px;">Valco</td>
			<td>ZU1TPK</td>
			<td>The polyether ether ketone union is used for connecting the inlet and outlet of SALVI</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Syringe</td>
			<td style="width:311px;">BD</td>
			<td>309659</td>
			<td style="width:1237px;">1 mL</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Pipette</td>
			<td style="width:311px;">Thermo Fisher Scientific</td>
			<td>21-377-821</td>
			<td style="width:1237px;">Range: 100 to 1,000 mL</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Pipette Tip 1</td>
			<td style="width:311px;">Neptune</td>
			<td>2112.96.BS</td>
			<td style="width:1237px;">1,000 &#181;L</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Pipette Tip 2</td>
			<td style="width:311px;">Rainin</td>
			<td>17001865</td>
			<td style="width:1237px;">20 &#181;L</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Syringe Pump</td>
			<td style="width:311px;">Harvard Apparatus</td>
			<td>70-2213</td>
			<td style="width:1237px;">It is used to inject the liquid sample into the SALVI device.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">pH meter</td>
			<td style="width:311px;">Fisher Scientific/accumet</td>
			<td>13-636-AP72</td>
			<td style="width:1237px;">It is used for measuring the pH of AlOOH in DI water.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Barnstead Ultrapure Water System, UV/UF</td>
			<td style="width:311px;">Thermo Scientific Barnstead</td>
			<td style="width:196px;">Nanopure diamond D11931</td>
			<td style="width:1237px;">It is used for producing DI water.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Centrifuge tubes</td>
			<td style="width:311px;">Fisher scientific/Falcon</td>
			<td>15-527-90</td>
			<td style="width:1237px;">15 mL</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Bransonic ultrasonic cleaner</td>
			<td style="width:311px;">Sigma-Aldrich</td>
			<td>2510</td>
			<td style="width:1237px;">It is used to ultrasonicate the AlOOH liquid sample.</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">Balance</td>
			<td style="width:311px;">Mettler Toledo</td>
			<td>11106015</td>
			<td style="width:1237px;">XS64</td>
		</tr>
		<tr height="20">
			<td height="20" style="width:289px;height:20px;">AlOOH</td>
			<td style="width:311px;">Pacific Northwest National Laboratory</td>
			<td>N/A</td>
			<td style="width:1237px;">It is synthesized by scientists at Pacific Northwest National Laboratory.</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">xT microscope Control</td>
			<td>FEI</td>
			<td>Quanta 3D FEG</td>
			<td>Default microscope control software of SEM Quanta 3D FEG</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">EDAX Genesis software</td>
			<td style="width:311px;">EDAX</td>
			<td>N/A</td>
			<td style="width:1237px;">The software is used for collecting the EDX elemental information of the samples.</td>
		</tr>
		<tr height="21">
			<td height="21" style="width:289px;height:21px;">Teflon tubing</td>
			<td>SUPELCO</td>
			<td>58697-U</td>
			<td style="width:1237px;">It is used for introducing the sample into the microchannel and holding adequate volume of liquid.</td>
		</tr>
	</tbody>
</table>

in situ characterization of boehmite particles in water using liquid sem

In situ imaging and elemental analysis of boehmite (AlOOH) particles in water is realized using the System for Analysis at the Liquid Vacuum Interface (SALVI) and Scanning Electron Microscopy (SEM). This paper describes the method and key steps in integrating the vacuum compatible SAVLI to SEM and obtaining secondary electron (SE) images of particles in liquid in high vacuum. Energy dispersive x-ray spectroscopy (EDX) is used to obtain elemental analysis of particles in liquid and control samples including deionized (DI) water only and an empty channel as well. Synthesized boehmite (AlOOH) particles suspended in liquid are used as a model in the liquid SEM illustration. The results demonstrate that the particles can be imaged in the SE mode with good resolution (i.e., 400 nm). The AlOOH EDX spectrum shows significant signal from the aluminum (Al) when compared with the DI water and the empty channel control. In situ liquid SEM is a powerful technique to study particles in liquid with many exciting applications. This procedure aims to provide technical know-how in order to conduct liquid SEM imaging and EDX analysis using SALVI and to reduce potential pitfalls when using this approach.

The representative results are presented to show how the particles are imaged and analyzed using in situ liquid SEM imaging coupled with EDX. The results include SE images and EDX spectra. The SE images were obtained at 100,000X and 200,000X magnification levels in Figure 1. Figure 1a depicts the SE image of the AlOOH, Figure 1b DI water, and Figure 1c the hole ...

Watch this Scientific Journal Video about In Situ Characterization of Boehmite Particles in Water Using Liquid SEM at JoVE.com

In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

We present a procedure for real-time imaging and elemental composition analysis of boehmite particles in deionized water by in situ liquid Scanning Electron Microscopy.

In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

In situ imaging and elemental analysis of boehmite (AlOOH) particles in water is realized using the System for Analysis at the Liquid Vacuum Interface ...

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