One type of atomic force microscopy (AFM) used for critical dimension (CD) metrology is commonly referred to as critical dimension atomic force microscopy (CD-AFM); it uses flared tips and two-dimensional surface sensing to enable scanning of features with near-vertical sidewalls. An important consideration in this type of CD-AFM metrology is the calibration uncertainty of the tip width. Standards for traceable tip width calibration have thus been developed both by national metrology institutes (NMIs) and commercial suppliers. The National Institute of Standards and Technology (NIST) has previously reported the implementation of a self-consistency tip width calibration using three CD-AFM tips to image each other. The results of this method were shown to be consistent with prior calibrations based on transmission electron microscope cross-sections. In the present work, the extension of this method to tips smaller than 50 nm is demonstrated, as well as the extension of the method to include a second lateral axis.

We demonstrate a hybrid "package-less" polydimethylsiloxane (PDMS)-complementary-metal-oxide-semiconductor (CMOS)-FR4 system for contact imaging. The system embeds the CMOS image sensor directly in a PDMS layer instead of the standard chip package to support microfluidic structures much larger and more complex than those in prior art. The CMOS/PDMS layer is self-aligned to form a continuous, flat surface to provide structural support for upper microfluidic layers. The system consists of five layers of PDMS implementing fluid channels, valves, chambers, and inlets/outlets. A custom CMOS image sensor with integrated signal conditioning circuits directly captures light from sample fluid for high optical collection efficiency. Owing to the flexibility afforded by the integration process, the system demonstrates, for the first time, integrated valves in contact imaging. Moreover, we present the first direct comparison of the optical performance of a CMOS image sensor and a photomultiplier tube (PMT) in identical contact-imaging conditions. Measurements show that our CMOS sensor achieves 17 dB better signal-to-noise ratio (SNR) compared to a commercial PMT across a broad range of integration times, with a maximum SNR of 47 dB. Chemiluminescent testing successfully shows signal detection for different analyte concentrations and integration times. The contact-imaging system demonstrates a detection limit of 25 μM of a 9,10-diphenylanthracene-based solution.

Methods exist for the creation of antireflective thin film layers; however, many of these methods depend on the use of high temperatures, harsh chemical etches, or are made with difficult pattern materials, rendering them unusable for many applications. In addition, most methods of light blocking are specifically designed to increase light coupling and absorption in the substrate, making them incompatible with some appli-cations that also require blocking transmission of light. A method of forming a simple, patternable light-blocking layer that drastically reduces both transmission and reflection of light without dependence on processes that could damage underlying structures using a light scattering matte coating over a partially antireflective thin film light-blocking layer is presented.

Since 2004 standards for calibration of critical dimension atomic force microscope (CD-AFM) tip width have been available both commercially and through national metrology institutes (NMIs) - such as the National Institute of Standards and Technology (NIST) in the United States. There have been inter-laboratory and inter-method comparisons performed on such samples, but less attention has been paid to the long-term stability of standards and monitoring for damage, wear, or contamination. Using three different CD-AFM instruments, we have tested the consistency and long-term stability of two independent reference calibrations for CD-AFM tip width. Both of these tip width calibrations were based on independently implemented transmission electron microscope (TEM) reference measurements. There were circumstances in which damage occurred or samples needed to be cleaned. Nevertheless, our results show agreement within the uncertainties and stability over a period exceeding 10 years.

The decreasing size of semiconductor features and the increasing structural complexity of advanced devices have placed continuously greater demands on manufacturing metrology, arising both from the measurement challenges of smaller feature sizes and the growing requirement to characterize structures in more than just a single critical dimension. For scanning electron microscopy, this has resulted in increasing sophistication of imaging models. For critical dimension atomic force microscopes (CD-AFMs), this has resulted in the need for smaller and more complex tips. Carbon nanotube (CNT) tips have thus been the focus of much interest and effort by a number of researchers. However, there have been significant issues surrounding both the manufacture and use of CNT tips. Specifically, the growth or attachment of CNTs to AFM cantilevers has been a challenge to the fabrication of CNT tips, and the flexibility and resultant bending artifacts have presented challenges to using CNT tips. The Korea Research Institute for Standards and Science (KRISS) has invested considerable effort in the controlled fabrication of CNT tips and is collaborating with the National Institute of Standards and Technology on the application of CNT tips for CD-AFM. Progress by KRISS on the precise control of CNT orientation, length, and end modification, using manipulation and focused ion beam processes, has allowed us to implement ball-capped CNT tips and bent CNT tips for CD-AFM. Using two different generations of CD-AFM instruments, we have evaluated these tip types by imaging a line/space grating and a programmed line edge roughness specimen. We concluded that these CNTs are capable of scanning the profiles of these structures, including re-entrant sidewalls, but there remain important challenges to address. These challenges include tighter control of tip geometry and careful optimization of scan parameters and algorithms for using CNT tips.

Sidewall sensing in critical dimension atomic force microscopes (CD-AFMs) usually involves continuous lateral dithering of the tip or the use of a control algorithm and fast response piezo actuator to position the tip in a manner that resembles touch-triggering of coordinate measuring machine (CMM) probes. All methods of tip position control, however, induce an effective tip width that may deviate from the actual geometrical tip width. Understanding the influence and dependence of the effective tip width on the dither settings and lateral stiffness of the tip can improve the measurement accuracy and uncertainty estimation for CD-AFM measurements. Since CD-AFM typically uses tips that range from 15 nm to 850 nm in geometrical width, the behavior of effective tip width throughout this range should be understood. The National Institute of Standards and Technology (NIST) has been investigating the dependence of effective tip width on the dither settings and lateral stiffness of the tip, as well as the possibility of material effects due to sample composition. For tip widths of 130 nm and lower, which also have lower lateral stiffness, the response of the effective tip width to lateral dither is greater than for larger tips. However, we have concluded that these effects will not generally result in a residual bias, provided that the tip calibration and sample measurement are performed under the same conditions. To validate that our prior conclusions about the dependence of effective tip width on lateral stiffness are valid for large CD-tips, we recently performed experiments using a very large non-CD tip with an etched plateau of approximately 2 μm width. The effective lateral stiffness of these tips is at least 20 times greater than typical CD-AFM tips, and these results supported our prior conclusions about the expected behavior for larger tips. The bottom-line importance of these latest observations is that we can now reasonably conclude that a dither slope of 3 nm/V is the baseline response due to the induced motion of the cantilever base.

We describe a method for fabricating an aperture on a fluidic cantilever device using SU-8 as a structural material. The device can ultimately be used for patch clamping, microinjections, fluidic delivery, fluidic deposition, and micromaterial removal. In the first generation of this device, the initial aperture diameter is 10 m and is fabricated on a silicon-on-insulator (SOI) wafer that is structurally used to define the aperture. The aperture can be reduced in size through mask design. This self-aligned process allows for patterning on the sharp tip projecting out of the fluidic plane on the cantilever and is batch fabricated, reducing the cost and time for manufacture. The initial mask, SOI device layer thickness, and the width of the base of the tip define the size of the aperture. The SU-8 micromachined cantilever includes an electrode and a force sensing mechanism. The cantilever can be easily integrated with an atomic force microscope or an optical microscope.

Cancer cells create a unique microenvironment that enables migration to distant organs. To better understand the tumor micro-environment, special tools and devices are required to monitor the interactions between different cell types and the effects of particular chemical gradients. Our study presents the design and optimization of a versatile chemotaxis device, the nano-intravital device (NANIVID), which consists of etched and bonded glass substrates that create a soluble factor reservoir. The device contains a customized hydrogel blend that is loaded with epidermal growth factor (EGF), which diffuses from the outlet to create a chemotactic gradient that can be sustained for many hours in order to attract specific cells to the device. A microelectrode array is under development for quantification of cell collection and will be incorporated into future device generations. Additionally, the NANIVID can be modified to generate gradients of other soluble factors in order to initiate controlled changes to the microenvironment including the induction of hypoxia, manipulation of extracellular matrix stiffness, etc. The focus of the article is to present the design and optimization of the device towards wide ranging applications of cancer cell dynamics and, ultimately, implantation for investigations.

We demonstrate the fabrication of micropore and nanopore features in hollow antiresonant reflecting optical waveguides to create an electrical and optical analysis platform that can size select and detect a single nanoparticle. Micropores (4 μm diameter) are reactive-ion etched through the top SiO(2) and SiN layers of the waveguides, leaving a thin SiN membrane above the hollow core. Nanopores are formed in the SiN membranes using a focused ion-beam etch process that provides control over the pore size. Openings as small as 20 nm in diameter are created. Optical loss measurements indicate that micropores did not significantly alter the loss along the waveguide.

Hybrid metrology, e.g., the combination of several measurement techniques to determine critical dimensions, is an increasingly important approach to meet the needs of the semiconductor industry. A proper use of hybrid metrology may yield not only more reliable estimates for the quantitative characterization of 3-D structures but also a more realistic estimation of the corresponding uncertainties. Recent developments at the National Institute of Standards and Technology (NIST) feature the combination of optical critical dimension (OCD) measurements and scanning electron microscope (SEM) results. The hybrid methodology offers the potential to make measurements of essential 3-D attributes that may not be otherwise feasible. However, combining techniques gives rise to essential challenges in error analysis and comparing results from different instrument models, especially the effect of systematic and highly correlated errors in the measurement on the χ function that is minimized. Both hypothetical examples and measurement data are used to illustrate solutions to these challenges.

We compare the speed and effectiveness of two genetic optimization algorithms to the results of statistical sampling via a Markov chain Monte Carlo algorithm to find which is the most robust method for determining real space structure in periodic gratings measured using critical dimension small angle X-ray scattering. Both a covariance matrix adaptation evolutionary strategy and differential evolution algorithm are implemented and compared using various objective functions. The algorithms and objective functions are used to minimize differences between diffraction simulations and measured diffraction data. These simulations are parameterized with an electron density model known to roughly correspond to the real space structure of our nanogratings. The study shows that for X-ray scattering data, the covariance matrix adaptation coupled with a mean-absolute error log objective function is the most efficient combination of algorithm and goodness of fit criterion for finding structures with little foreknowledge about the underlying fine scale structure features of the nanograting.

Optical 3D nanostructure metrology utilizes a model-based metrology approach to determine critical dimensions (CDs) that are well below the inspection wavelength. Our project at the National Institute of Standards and Technology is evaluating how to attain key CD and shape parameters from engineered in-die capable metrology targets. More specifically, the quantities of interest are determined by varying the input parameters for a physical model until the simulations agree with the actual measurements within acceptable error bounds. As in most applications, establishing a reasonable balance between model accuracy and time efficiency is a complicated task. A well-established simplification is to model the intrinsically finite 3D nanostructures as either periodic or infinite in one direction, reducing the computationally expensive 3D simulations to usually less complex 2D problems. Systematic errors caused by this simplified model can directly influence the fitting of the model to the measurement data and are expected to become more apparent with decreasing lengths of the structures. In this paper we identify these effects using selected simulation results and present experimental setups, e.g., illumination numerical apertures and focal ranges, that can increase the validity of the 2D approach.

Optimizing the extraction of information from x-ray measurements while minimizing exposure time is an important area of research in a variety of fields. The semiconductor industry is reaching a point where the traditional optical metrologies need to be augmented in order to better resolve the critical dimensions of structures with feature sizes below 10 nm. Critical dimension small angle x-ray scattering (CDSAXS) is one measurement technique that is capable of characterizing detailed features of periodic nanostructures. As currently implemented, the measurement utilizes the combined scattering from up to 60 different angles. Reducing the number of angles would dramatically improve the feasibility of CDSAXS for implementation in a fabrication setting, but currently there are no clear guidelines as to which angles provide the most information to minimize the uncertainty in the shape of the target structure while maximizing the throughput. In order to develop guidelines for optimizing the angle selection, simulation studies were conducted on a wide variety of structures with subsets of the full angular range to identify which angles minimized the overall shape uncertainty. Analyzing sets of two angle pairs (including all combinations between 0 deg and 60 deg) provides guidance on which angles best constrain the samples. For select samples, higher numbers of angles were included to explore the impact of additional information on the model uncertainty. In general, low angles (<3 deg) best contributed to minimizing the line-width uncertainty, while higher angles near high curvature regions of the scattering profile best constrained the height of the structure. The minimum uncertainty was generally achieved with combinations of the two. This simulation approach can be used to minimize the number of angles measured on real samples and significantly reduce the measurement time.

Nanoscale wear affects the performance of atomic force microscopy (AFM)-based measurements for all applications including process control measurements and nanoelectronics characterization. As such, methods to prevent or reduce AFM tip wear is an area of active research. However, most prior work has been on conventional AFMs rather than critical dimension AFM (CD-AFM). Hence, less is known about CD-AFM tip-wear. Given that tip-wear directly affects the accuracy of dimensional measurements, a basic understanding of CD-AFM tip wear is needed. Toward this goal, we evaluated the wear performance of electron beam deposited CD-AFM tips. Using a continuous scanning strategy, we evaluated the overall wear rate and tip lifetime and compared these with those of silicon-based CD-AFM tips. Our data show improved tip lifetime of as much as a factor of five and reduced wear rates of more than 17 times. Such improvements in wear rate means less measurement variability and lower cost.