More Like this

1. Evaluating scanning electron microscopy for the measurement of small-scale topography

   https://doi.org/10.1088/2051-672X/ad49b9  

   Chadha, Vimanyu; Miller, Nathaniel; Ding, Ruikang; Beschorner, Kurt E; Jacobs, Tevis David (May 2024, Surface Topography: Metrology and Properties)

   Abstract For predicting surface performance, multiscale topography analysis consistently outperforms standard roughness metrics; however, surface-characterization tools limit the range of sizes that can be measured. Therefore, we evaluate the use of scanning electron microscopy (SEM) to systematically measure small-scale topography. While others have employed SEM for similar purposes, the novelty of this investigation lies in the development and validation of a simple, flexible procedure that can be applied to a wide range of materials and geometries. First, we established four different options that can be used for sample preparation, and we measured quantitative topography of each using the SEM. Then the power spectral density (PSD) was used to compare topography among the four preparations, and against other techniques. A statistical comparison of PSDs demonstrated that SEM topography measurements outperformed AFM measurements at scales below 100 nm and were statistically indistinguishable from (highly labor-intensive) TEM measurements down to 16 nm. The limitations of SEM-based topography are quantified and discussed. Overall, the results show a simple generalizable method for revealing small-scale topography. When combined with traditional stylus profilometry, this technique characterizes surface topography across almost seven orders of magnitude, from 1 cm down to 16 nm, facilitating the use of physical models to predict performance. 

   more » « less
2. Comparison between shadow imaging and in-line holography for measuring droplet size distributions

   https://doi.org/10.1007/s00348-023-03633-8  

   Erinin, Martin A; Néel, Baptiste; Mazzatenta, Megan T; Duncan, James H; Deike, Luc (May 2023, Experiments in Fluids)

   Kähler, C; Longmire, E; Westerweel, J (Ed.)

   Abstract A direct comparison of the droplet size and number measurements using in-line holography and shadow imaging is presented in three dynamically evolving laboratory scale experiments. The two experimental techniques and image processing algorithms used to measure droplet number and radii are described in detail. Droplet radii as low as$$r = 14$$ $r=14$ µm are measured using in-line holography and$$r = 50$$ $r=50$ µm using shadow imaging. The droplet radius measurement error is estimated using a calibration target (reticle) and it was found that the holographic technique is able to measure droplet radii more accurately than shadow imaging for droplets with$$r \le 625$$ $r\le 625$ µm. Using the measurements of droplet number and size we quantitatively cross-validate and assess the accuracy of the two measurement techniques. The droplet size distributions,N(r), are measured in all three experiments and are found to agree well between the two measurement techniques. In one of the laboratory experiments, simultaneous measurements of droplets ($$r \ge 14$$ $r\ge 14$ µm, using holography) and dry aerosols ($$0.07 \lessapprox r \lessapprox 2$$ $0.07⪅r⪅2$ µm, using an scanning mobility particle sizer and$$0.15 \lessapprox r \lessapprox 5$$ $0.15⪅r⪅5$ µm using an optical particle sizer) are reported, one of the first such comparison to the best of our knowledge. The total number and volume of droplets is found to agree well between both techniques in the three experiments. We demonstrate that a relatively simple shadow imaging technique can be just as reliable when compared to a more sophisticated holographic measurement technique over their common droplet radius measurement range. The agreement in results is shown to be valid over a large range of droplet concentrations, which include experiments with relatively sparse droplet concentrations as low as 0.02 droplets per image. Advantages and disadvantages for the two techniques are discussed in the context of our results. The main advantages to in-line holography are the greater accuracy in droplet radius measurement, greater spatial resolution, larger depth of field, and the high repetition rate and short pulse duration of the laser light source. In comparison, the main advantages to shadow imaging are the simpler experimental setup, image processing algorithm, and fewer computer resources necessary for image processing. Droplet statistics like number and size are found to be very reliable between the two methods for large range of droplet densities,$${\mathcal {P}}_{r>50}$$ $P_{r>50}$, ranging from$$10^{-4} \le {\mathcal {P}}_{r>50} \le 10^{-1}$$ ${10}^{-4}\le P_{r>50}\le {10}^{-1}$cm$$^{-3}$$ ${}^{-3}$, when the two techniques are implemented as shown in this paper. 

   more » « less
3. Electric-Field-Assisted Contact Mode AFM-Based Nanolithography with Low Stiffness Conductive Probes

   https://doi.org/10.1115/1.4054316  

   Zhou, Huimin; Jiang, Yingchun; Dmuchowski, Christopher M; Ke, Changhong; Deng, Jia (April 2022, Journal of Micro and Nano-Manufacturing)

   Abstract Electric-field-assisted atomic force microscope (E-AFM) nanolithography is a novel polymer-patterning technique that has diverse applications. E-AFM uses a biased AFM tip with conductive coatings to make patterns with little probe-sample interaction, which thereby avoids the tip wear that is a major issue for contact-mode AFM-based lithography, which usually requires a high probe-sample contact force to fabricate nanopatterns; however, the relatively large tip radius and large tip-sample separation limit its capacity to fabricate high-resolution nanopatterns. In this paper, we developed a contact mode E-AFM nanolithography approach to achieve high-resolution nanolithography of poly (methyl methacrylate) (PMMA) using a conductive AFM probe with a low stiffness (~0.16 N/m). The nanolithography process generates features by biasing the AFM probe across a thin polymer film on a metal substrate. A small constant force (0.5-1 nN) applied on the AFM tip helps engage the tip-film contact, which enhances nanomachining resolution. This E-AFM nanolithography approach enables high-resolution nanopatterning with feature width down to ~16 nm, which is less than one half of the nominal tip radius of the employed conductive AFM probes. 

   more » « less
4. Atomic Force Microscopy (AFM) Analysis of an Object Larger and Sharper than the AFM Tip

   https://doi.org/10.1017/S1431927619014697  

   Chen, Zhe; Luo, Jiawei; Doudevski, Ivo; Erten, Sema; Kim, Seong H. (January 2019, Microscopy and Microanalysis)

   Abstract Atomic force microscopy (AFM) is typically used for analysis of relatively flat surfaces with topographic features smaller than the height of the AFM tip. On flat surfaces, it is relatively easy to find the object of interest and deconvolute imaging artifacts resulting from the finite size of the AFM tip. In contrast, AFM imaging of three-dimensional objects much larger than the AFM tip height is rarely attempted although it could provide topographic information that is not readily available from two-dimensional imaging, such as scanning electron microscopy. In this paper, we report AFM measurements of a vertically-mounted razor blade, which is taller and sharper than the AFM tip. In this case, the AFM height data, except for the data collected around the cutting edge of the blade, reflect the shape of the AFM tip. The height data around the apex area are effectively the convolution of the AFM tip and the blade cutting edge. Based on computer simulations mimicking an AFM tip scanning across a round sample, a simple algorithm is proposed to deconvolute the AFM height data of an object taller and sharper than the AFM tip and estimate its effective curvature. 

   more » « less
5. Measurement of the surface hydrophobicity of engineered nanoparticles using an atomic force microscope

   https://doi.org/10.1039/c8cp04676j  

   Fu, Wanyi; Zhang, Wen (January 2018, Physical Chemistry Chemical Physics)

   Determination of the surface hydrophobicity or wettability of nanomaterials and nanoparticles (NPs) is often challenged by the heterogeneous properties of NPs that vary with particle size, shape, surface charge, aggregation states, and surface sorption or coating. This study first summarized inherent limitations of the water contact angle, octanol–water partition coefficient ( K ow ) and surface adsorption of probe molecules in probing nanomaterial hydrophobicity. Then, we demonstrated the principle of a scanning probe method based on atomic force microscopy (AFM) for the local surface hydrophobicity measurement. Specifically, we measured the adhesion forces between functionalized AFM tips and self-assembled monolayers (SAMs) to establish a linear relationship between the adhesion forces and water contact angles based on the continuum thermodynamic approach (CTA). This relationship was used to determine the local surface hydrophobicity of seven different NPs ( i.e. , TiO 2 , ZnO, SiO 2 , CuO, CeO 2 , α-Fe 2 O 3 , and Ag), which agreed well with bulk contact angles of these NPs. Some discrepancies were observed for Fe 2 O 3 , CeO 2 and SiO 2 NPs, probably because of surface hydration and roughness effects. Moreover, the solution pH and ionic strength had negligible effects on the adhesion forces between the AFM tip and MWCNTs or C 60 , indicating that the hydrophobicity of carbonaceous nanomaterials is not influenced by pH or ionic strength (IS). By contrast, natural organic matter (NOM) appreciably decreased the hydrophobicity of MWCNTs and C 60 due to surface coating of hydrophilic NOM. This scanning probe method has been proved to be reliable and robust toward the accurate measurement of the nanoscale hydrophobicity of individual NPs or nanomaterials in liquid environments. 

   more » « less