Name: characterization of surface modifications by white light interferometry: applications in ion sputtering, laser ablation, and tribology experiments
Uploaded: 2013-02-27T12:00:00
Description: Watch this Scientific Journal Video about Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments at JoVE.com

The irradiated GaAs sample was provided by Yang Cui of the University of Illinois at Chicago. This work was supported under Contract No. DE-AC02-06CH11357 between UChicago Argonne, LLC and the U.S. Department of Energy and by NASA through grants NNH08AH761 and NNH08ZDA001N, and the Office of Vehicle Technologies of the U.S. Department of Energy under contract DE-AC02-06CH11357. The electron microscopy was accomplished at the Electron Microscopy Center for Materials Research at Argonne National Laboratory, a U.S. Department of Energy Office of Science laboratory, operated under Contract DE-AC02-06CH11357 by UChicago Argonne, LLC.

1. Hardware Alignment for General WLI Scan
To obtain quantitative information through WLI, the following steps may serve as a guideline. It is assumed that the operator has basic knowledge of interferometer operation. The guidelines are common regardless of the specific instrument. For some investigations, the specimen will be flat. For others, the specimen may be curved.
<ol>
	<li>Place the sample on the stage with the feature (ion sputtered crater, ion beam/ablated spot, or wear scar) faci...

Example 1
WLI is not widely used for surface characterization in tribological work, but it is in fact a powerful method for quantitative measurement of wear volumes for many contact geometries. WLI produces a full 3D representation of the surface that can be analyzed using any of several visualization software packages. These packages enable various types of measurements to be performed. For greater lateral resolution, images can be "stitched" together to produce wide-area information (several mm...

The surface of solid materials determines to a large extent properties of interest for those materials: electronically, structurally, and chemically. In many areas of research, the addition of material (for instance, thin film deposition by pulsed laser/magnetron sputtering deposition, physical/chemical vapor deposition), removal of material (reactive ion etching, ion sputtering, laser ablation, etc.), or some other processes, need to be characterized. Additionally, surface modification through interaction with energetic light pulses or charged particles has numerous applications and is of fundamental interest. Tribology, the study of friction and wear, is another area of interest. On a benchtop scale, a multitude of tribological test geometries exist. Non-conformal contact geometries may be used, and a ball or cylinder may be slid or rotated against a flat surface, another ball, or cylinder, for a length of time, and the amount of material that is removed is measured. Because the wear scar is three-dimensional and irregular in nature, optical profilometry may be the only technique suitable for obtaining accurate wear volume measurements. Common analysis tasks include also surface roughness parameters, step height, loss of material volume, trench depth, and so on; all of them can be obtained additionally to simple 2D and 3D topography visualization.
Optical profilometry refers to any optical method that is used to reconstruct the profile of surfaces. Profilometric methods include white light interferometric, laser, or confocal methods. Some optical profilometers obtain information through approaches based on conventional diffraction-limited microscope objectives. For example, a scanning laser may be integrated with a microscope to obtain topographic and true color information of surfaces. A second method uses a technique which exploits the extremely small depth of focus of conventional objectives to assemble a series of in-focus "image slices" of the surface to obtain a 3D topographic map.
In this work we show how a white light interferometric microscope/profilometer enables the measurement of the amount of material lost during mechanical wear processes, or during material etching processes such as ion sputtering craters or laser ablation. Most attention is paid to methodology of this method to illustrate its large installed capacity that makes it widely available and attractive for numerous applications. Most types of WLI employ the Mirau technique, which uses a mirror internal to the microscope objective to cause interference between a reference light signal and the light reflected from the sample surface. The choice of Mirau interferometry is dictated by simple convenience, because the entire Mirau interferometer can be fit inside the microscope objective lens and coupled to a regular optical microscope (Figure 1). A series of two-dimensional interferograms are acquired with a video camera, and software assembles a 3D topographic map. The white light source supplies broad spectrum illumination which helps to overcome the "fringe order" ambiguity inherent to a monochromatic source. A monochromatic source of light may be used to obtain more accurate measurement of shallow topographic features. The lateral resolution is fundamentally limited to &lambda;/2 (numerical aperture, NA=1), but in most instances is larger, being determined by the NA of the objective, which is in turn connected to magnification/field-of-view size. Table 1 in Ref. 1 has a direct comparison of all mentioned parameters. Depth resolution approaches &asymp;1 nm, being a function of the interferometric nature of the technique. Further information on Mirau WLI can be found in Refs. 2, 3. An introduction on white light interferometric approach can be found in Ref. 4.
Other methods for analysis of surfaces are atomic force microscopy (AFM), scanning electron microscopy (SEM), and stylus profilometry. The WLI technique compares favorably to these methods and has its own advantages and drawbacks that are due to the optical nature of the method.
The AFM is capable of obtaining 3D images and thus corresponding cross sections, but AFM has a limited scanning ability in the lateral (&lt;100 &mu;m) and depth (&lt;10 &mu;m) axes. In contrast to those, the main advantage of WLI is the flexible field-of-view (FOV) of up to a few millimeters with simultaneous real 3D imaging capability. In addition, as we will demonstrate it has wide vertical scanning range capacity, allowing one to solve a variety of problems of surface modification simply. Researchers who have worked with AFM are aware of the problem with plane positioning of a sample when measuring prolonged features of low vertical gradients. Generally, one may think of WLI/OP as an "express" technique over AFM. Of course, there are a number of areas for which only AFM is suitable: when lateral features to be resolved have characteristic dimensions smaller than the lateral resolution of WLI, or instances where data from WLI is ambiguous due to unknown or complex optical properties of a sample in a way that affects the accuracy of measurements (to be discussed later), etc.
The SEM is a powerful way to look at surfaces, being very flexible in terms of the FOV size with large depth of focus, larger than any conventional optical microscope can offer. At the same time, 3D imaging by SEM is cumbersome, particularly as it requires taking of stereo-pair images that then are converted to 3D images by the anaglyphic method, or through observing with optical viewers, or used for direct calculation of depths between different points of interest on a sample.5 By contrast, WLI/OP profilometry offers easy-to-use 3D reconstruction with simultaneously flexible FOV. WLI scans through the full height range needed for the particular sample (from nanometers to hundreds of microns). WLI is unaffected by the electrical conductivity of the sample material, which may be a problem with SEM. WLI clearly does not require a vacuum. On the other hand there are a number of applications for which SEM provides superior information: lateral features to be resolved of characteristic dimensions below the lateral resolution of WLI, or cases where different parts of a sample can be topographically distinguished only when secondary electron emission coefficients differ.
One more technique for surface inspection, which is widely used in secondary ion mass spectrometry6 and in the field of microelectromechanical systems characterization7 is stylus profilometry. This technique is popular because of its simplicity and robustness. It is based on direct mechanical contact scanning of a stylus tip over the sample surface. This is a coarse contact tool, which is able to scan along a single line at a time. It makes 3D surface raster-scan imaging extremely time consuming. Another drawback of the stylus technique is the difficulty of measuring surface features of high aspect ratio and of size comparable with its characteristic tip size (submicron to several microns typically) that implies a tip radius and a tip apex angle. An advantage of stylus profilometry is its insensitivity to varying optical properties of a sample, which can affect the accuracy of WLI/OP measurements (to be discussed later).
The surface maps in the present article were obtained using a conventional Mirau-type WLI (Figure 1). Many companies such as Zygo, KLA-Tencor, nanoScience, Zemetrics, Nanovea, FRT, Keyence, Bruker, and Taylor Hobson produce commercial table-top OP instruments. The acquired maps were reconstructed and processed using commercial software of the type that is commonly used for WLI, scanning electron, or probe microscopy. The software has the ability to perform mathematical manipulations of the surface, cross section profile analysis, void and material volume calculations, and plane correction. Other software packages may automate some of these features.

<table border="1">
 <tbody>
 <tr>
 <td>Single crystal substrates of Si, GaAs and Cu </td>
 <td></td>
 <td></td>
 <td>for sputtering and ablation </td>
 </tr>
 <tr>
 <td>Pure metal alloys </td>
 <td></td>
 <td></td>
 <td>for tribology examples</td>
 </tr>
 </tbody>
</table>

characterization of surface modifications by white light interferometry: applications in ion sputtering, laser ablation, and tribology experiments

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. From the measured surface, 3D topographic maps can be subsequently analyzed using a variety of software packages to extract the information that is needed.
In this article we describe how white light interferometry, and optical profilometry (OP) in general, combined with generic surface analysis software, can be used for materials science and engineering tasks. In this article, a number of applications of white light interferometry for investigation of surface modifications in mass spectrometry, and wear phenomena in tribology and lubrication are demonstrated. We characterize the products of the interaction of semiconductors and metals with energetic ions (sputtering), and laser irradiation (ablation), as well as ex situ measurements of wear of tribological test specimens.
Specifically, we will discuss:
<ol class="lroman">
	<li>Aspects of traditional ion sputtering-based mass spectrometry such as sputtering rates/yields measurements on Si and Cu and subsequent time-to-depth conversion.</li>
	<li>Results of quantitative characterization of the interaction of femtosecond laser irradiation with a semiconductor surface. These results are important for applications such as ablation mass spectrometry, where the quantities of evaporated material can be studied and controlled via pulse duration and energy per pulse. Thus, by determining the crater geometry one can define depth and lateral resolution versus experimental setup conditions.</li>
	<li>Measurements of surface roughness parameters in two dimensions, and quantitative measurements of the surface wear that occur as a result of friction and wear tests.</li>
</ol>
Some inherent drawbacks, possible artifacts, and uncertainty assessments of the white light interferometry approach will be discussed and explained.

<img alt="Figure 1" src="/files/ftp_upload/50260/50260fig1.jpg" /> 
 Figure 1. Photograph of a simple profilometer used in the present study: a multiple objective turret is seen in the picture. Two objectives are standard (10x and 50x), and two are Mirau objectives (10x and 50x). This microscope has an intermediate magnification feature that enables step-wise magnification multipliers of 0.62, 1.00, 1.25, or 2.00 to be selected. <a href="https://www.jove.com/fi...

Watch this Scientific Journal Video about Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments at JoVE.com

Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments

White light microscope interferometry is an optical, noncontact and quick method for measuring the topography of surfaces. It is shown how the method can be applied toward mechanical wear analysis, where wear scars on tribological test samples are analyzed; and in materials science to determine ion beam sputtering or laser ablation volumes and depths.

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. ...

characterization-surface-modifications-white-light-interferometry

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Fabrication And Characterization Of Photonic Crystal Slow Light Waveguides And Cavities

Slow light has been one of the hot topics in the photonics community in the past decade, generating great interest both from a fundamental point of view and for its considerable potential for practical applications. Slow light photonic crystal waveguides, in particular, have played a major part and have been successfully employed for delaying optical signals1-4 and the enhancement of both linear5-7 and nonlinear devices.8-11
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To attain these exciting results, a robust repeatable fabrication protocol must be developed. In this paper we take an in-depth look at our fabrication protocol which employs electron-beam lithography for the definition of photonic crystal patterns and uses wet and dry etching techniques. Our optimised fabrication recipe results in photonic crystals that do not suffer from vertical asymmetry and exhibit very good edge-wall roughness. We discuss the results of varying the etching parameters and the detrimental effects that they can have on a device, leading to a diagnostic route that can be taken to identify and eliminate similar issues.
The key to evaluating slow light waveguides is the passive characterization of transmission and group index spectra. Various methods have been reported, most notably resolving the Fabry-Perot fringes of the transmission spectrum20-21 and interferometric techniques.22-25 Here, we describe a direct, broadband measurement technique combining spectral interferometry with Fourier transform analysis.26 Our method stands out for its simplicity and power, as we can characterise a bare photonic crystal with access waveguides, without need for on-chip interference components, and the setup only consists of a Mach-Zehnder interferometer, with no need for moving parts and delay scans.
When characterising photonic crystal cavities, techniques involving internal sources21 or external waveguides directly coupled to the cavity27 impact on the performance of the cavity itself, thereby distorting the measurement. Here, we describe a novel and non-intrusive technique that makes use of a cross-polarised probe beam and is known as resonant scattering (RS), where the probe is coupled out-of plane into the cavity through an objective. The technique was first demonstrated by McCutcheon et al.28 and further developed by Galli et al.29

Use of photonic crystal slow light waveguides and cavities has been widely adopted by the photonics community in many differing applications. Therefore fabrication and characterization of these devices are of great interest. This paper outlines our fabrication technique and two optical characterization methods, namely: interferometric (waveguides) and resonant scattering (cavities).

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We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

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Gas sampling from laboratory-scale flames with online analysis of all species by mass spectrometry is a powerful method to investigate the complex mixture of chemical compounds occurring during combustion processes. Coupled with tunable soft ionization via synchrotron-generated vacuum-ultraviolet radiation, this technique provides isomer-resolved information and potentially fragment-free mass spectra.

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Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of biosensing devices. We report on a protocol of using KrF and ArF lasers irradiating Si (001) samples immersed in a liquid environment with low number of pulses and operating at moderately low pulse fluences to induce Si wettability modification. Wafers immersed for up to 4 hr in a 0.01% H2O2/H2O solution did not show measurable change in their initial contact angle (CA) ~75&#176;. However, the 500-pulse KrF and ArF lasers irradiation of such wafers in a microchamber filled with 0.01% H2O2/H2O solution at 250 and 65 mJ/cm2, respectively, has decreased the CA to near 15&#176;, indicating the formation of a superhydrophilic surface. The formation of OH-terminated Si (001), with no measurable change of the wafer&#8217;s surface morphology, has been confirmed by X-ray photoelectron spectroscopy and atomic force microscopy measurements. The selective area irradiated samples were then immersed in a biotin-conjugated fluorescein-stained nanospheres solution for 2 hr, resulting in a successful immobilization of the nanospheres in the non-irradiated area. This illustrates the potential of&#160;the method for selective area biofunctionalization and fabrication of advanced Si-based biosensing architectures. We also describe a similar protocol of irradiation of wafers immersed in methanol (CH3OH) using ArF laser operating at pulse fluence of 65 mJ/cm2 and in situ formation of a strongly hydrophobic surface of Si (001) with the CA of 103&#176;. The XPS results indicate ArF laser induced formation of Si&#8211;(OCH3)x compounds responsible for the observed hydrophobicity. However, no such compounds were found by XPS on the Si surface irradiated by KrF laser in methanol, demonstrating the inability of the KrF laser to photodissociate methanol and create -OCH3 radicals.

We report on a process of in situ alteration of HF treated Si (001) surface into a hydrophilic or hydrophobic state by irradiating samples in microfluidic chambers filled with&#160;H2O2/H2O solution (0.01%-0.5%) or methanol solutions using pulsed UV laser of a relative low pulse fluence.

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We present a compact reflection digital holographic system (CDHM) for inspection and characterization of MEMS devices. A lens-less design using a diverging input wave providing natural geometrical magnification is demonstrated. Both static and dynamic studies are presented.

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Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

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The authors present a method for fabricating stable white-light-emitting electrochemical cells utilizing emission from exciplexes formed between a blue-emitting fluorene polymer and aromatic amines.

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Protocols for the synthesis of microspheres from polymers, the manipulation of microspheres, and micro-photoluminescence measurements are presented.

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A protocol for the production of simple structured organic light-emitting diodes (OLEDs) is presented.

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex ...