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AFM and Combined Optical Techniques

This application note briefly describes the basics of both optical and atomic force microscopy, followed by a discussion of some of the technical challenges of integrating these two distinct imaging modalities. In certain cases, the benefits and disadvantages of different approaches to design and integration are discussed. Lastly, a few examples of successful application of these combined imaging modalities are presented.

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AFM Applications in Polymer Science and Engineering
The atomic force microscope (AFM) is a powerful tool for characterizing polymer materials. It provides nanoscale information on a wide range of physical properties and behavior in addition to imaging morphology. This note describes the many capabilities and advantages of Asylum Research Cypher™ and MFP-3D™ AFMs for understanding polymers.
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AFM Characterization of Thin Films: High-Resolution Topography and Functional Properties

Asylum Research Cypher™ and MFP-3D™ atomic force microscopes (AFMs) provide valuable information for characterizing thin films and coatings. They quantify 3D roughness and texture with unmatched spatial resolution and measure nanoscale functionality including electrical, magnetic, and mechanical behavior.

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AM-FM Viscoelastic Mapping Mode
Information on mechanical properties is important in many applications. AM-FM Viscoelastic Mapping Mode lets you quickly and gently image viscoelastic properties including storage modulus and loss tangent with nanoscale spatial resolution. Its very wide operating range, from less than 1 MPa to hundreds of GPa, makes it a highly versatile technique. AM-FM Mode is available on all MFP-3D™ and Cypher™ family AFMs and is one of many options in Asylum’s NanomechPro™ Toolkit for nanomechanical measurements.
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Applications of the NanoRack Sample Stretching Stage to a Commercial Impact Copolymer
A commercial impact copolymer (ICP), a multicomponent material typically used in automotive and appliance applications where a balance of stiffness and toughness is needed, was studied with the NanoRack™ Sample Stretching Stage accessory on the MFP-3D™ Atomic Force Microscope to investigate material deformation and interface adhesion as a function of tensile stress. Effects of deformation were observed within both the polypropylene and ethylene propylene components, as well as at the interface between the two materials. There are no other direct measurement methods available to determine interfacial adhesive strength of polymer blends, and so AFM investigations of micro-domain deformation such as the one described here could be used ultimately to provide a direct determination of interfacial adhesion in complex polymer containing materials such as ICP. Studies of this kind improve our understanding of material structure-property relationships, ultimately enabling manufacture of better quality products.
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ARC2™ SPM Controller – Power, Speed, and Flexibility
The Asylum Research ARC2 SPM Controller is the most innovative controller for atomic force microscopy. The ARC2, based on the ground-breaking all-digital MFP-3D™ Controller, incorporates improved DACs, high voltage relays, a high speed digital link, and a new design for advanced power and flexibility.
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AR-PPLN Test Sample for Piezoresponse Force Microscopy
The AR-PPLN Test Sample is a convenient and reliable sample for practice, setup, and verification for a wide variety of Piezoresponse Force Microscopy (PFM) techniques. This includes, but is not limited to, imaging and point hysteresis loops. The reference sample has stripe domains permanently polarized for easy identification and optimization of PFM parameters
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Atomic Force Microscopy in Food Research
The application of atomic force microscopy (AFM) to food science may not seem an obvious one at first thought – after all what can a nano-technique such as AFM, more commonly associated with surface science labs, do for such an overtly macro and everyday material as food? The answer lies in the relationship between the structure of food and its function. Many of the desirable properties of the food that we enjoy rely upon nano- or microscale phenomena. In addition, the importance of structure on the nutritional impact of food is beginning to be understood both in terms of delivering nutrients to the body,1 and also in terms of its potential to exert protective effects against chronic diseases.2 In this article we will illustrate these areas using two examples of the AFM work being carried out at the Institute of Food Research (IFR) using the MFP-3D™ AFM from Asylum Research.
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Atomic Force Microscopy Tools for Electrical Characterization
The importance of characterizing electrical functionality on nanometer length scales continues to grow as devices shrink and new nanomaterials emerge. Oxford Instruments Asylum Research offers a variety of AFM tools to evaluate local electrical properties, including current, surface charge and potential, dielectric 
breakdown, conductivity, and permittivity. Special features and unique capabilities for Cypher™ and MFP-3D™ family AFMs provide more opportunities for meaningful electrical measurements on a wide range of systems.
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Automating Your Asylum Research AFM with the MacroBuilder Interface
Asylum Research provides full-function MFP-3D™ and Cypher™ Atomic Force Microscopes (AFMs) with superior capabilities that require no programming to perform advanced imaging and measurements. For more advanced, automated, and custom experiments, Asylum also provides a user-driven programming language called IGOR Pro. The MacroBuilder™ interface allows you to easily set up and run a sequence of measurements unattended while automatically varying parameters – and without writing any code. The MacroBuilder interface is provided as a standard capability on all MFP-3D and Cypher AFMs.
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Band Excitation Scanning Probe Microscopies: Traveling through the Fourier Space
In the two decades since the emergence of the first commercial Scanning Probe Microscopes (SPMs), force-based SPMs have become primary tools for exploring and manipulating matter on the nanoscale. The rapid growth in the number of SPM imaging modes and microscope platforms is contrasted by the fact that the most common operational mode – periodically exciting and synchronously measuring the cantilever probe response – has stayed the same. The last several years have seen a number of approaches for SPM beyond simple periodic excitation. Here, we summarize the principles and recent advances of one such technique: band excitation (BE) SPM, a universal method for broad-band SPM measurements applicable to all ambient and liquid SPM modes. BE is implemented exclusively on the Cypher™ and MFP-3D™ AFMs from Asylum Research.
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Bimodal Dual AC™ Imaging
An exclusive measurement ability, Dual AC, has been developed by Asylum Research for use on the MFP-3D™ and Cypher™ AFMs. Since its introduction, the number of applications for Dual AC has increased dramatically. This note will give you an introduction to bimodal imaging, just one of many Dual AC techniques that can be performed on Asylum’s AFMs.
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BioHeater™ Closed Fluid Cell Accessory for the MFP-3D™ AFM
The BioHeater is a temperature controlled sample stage for the MFP-3D AFM for heating samples in liquids from ambient to 80°C. It is ideal for many applications such as protein conformational changes, enzymatic activity, lipid phase transitions and others.
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blueDrive™ Photothermal Excitation
Asylum Research’s blueDrive Photothermal Excitation option for the Cypher™ atomic force microscope (AFM) family makes tapping mode techniques simpler, more stable, and more quantitative. Tapping mode is by far the dominant choice in the world of AFM, measuring not just topography, but also mechanical, electrical, and magnetic properties. Typically, piezoacoustic excitation is used to drive the cantilever oscillation. Though piezo drive is favored for design simplicity, the response of the cantilever is often far from ideal. Asylum’s blueDrive excitation mechanism produces an almost perfect response by directly exciting the cantilever photothermally. This provides significant performance and ease of use benefits for all tapping mode
techniques.
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CalibratAR™ Microscale 3D Calibration Reference
The CalibratAR Calibration Reference can be used on many types of microscopes for characterization and/or calibration purposes. This includes but is not limited to scanning probe, atomic force, scanning electron and optical microscopes, as well as stylus and optical profilers. The reference sample design incorporates features in three orthogonal directions for three dimensional characterization.
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Charge Writing and Detection by Electric Scanning Probe Techniques
Understanding the generation mechanisms and dissipation behavior of electric charge on the surface and in the bulk of insulating materials is of importance to the study of a variety of phenomena. These include triboelectrification and electrostatic discharge (ESD), as well as to several current and future applications, such as cable insulation, laser printer and photocopier xerography, charge based data storage, plastic material recycling, and electret field-effect transistors, microphones, and dust filters. Remarkably, the charging and discharging mechanisms of insulators are often not understood in detail, and even today the identity of the charge carriers remains obscure in many cases.1,2,3 A convenient tool for investigating these mechanisms is the atomic force microscope (AFM) because the charging can be realized with the same probe used for the analysis, and electric field sensitive AFM modes such as Electrostatic Force Microscopy (EFM) and Kelvin Probe Force Microscopy (KPFM), also known  as Scanning Kelvin Probe Microscopy (SKPM), provide highly resolved spatial information of the charge distribution with extremely high sensitivity. Accordingly, these methods have been used since their invention for the study of charging and discharging phenomena on insulators.
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Closed Fluid Cell Accessory for the MFP-3D™ AFM

The Closed Fluid Cell allows fluid imaging in a completely sealed and enclosed environment on MFP-3D AFMs.

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Contact Resonance Viscoelastic Mapping Mode

Asylum Research’s Contact Resonance Viscoelastic Mapping Mode option for the MFP-3D™ and Cypher™ S Atomic Force Microscopes (AFMs) enables high resolution, quantitative imaging of both elastic storage modulus and viscoelastic loss modulus. It is just one of the many nanomechanical tools in Asylum’s NanomechPro™ Toolkit. The contact resonance technique is particularly well suited for characterizing moderate to high modulus materials in the range of about 1 GPa to 200 GPa.

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CoolerHeater Accessory for the MFP-3D™ AFM
The CoolerHeater accessory for the MFP-3D™ uses a Peltier element to heat and cool small samples within the range of -30°C to +120°C, ideal for a wide range of thermally-controlled experiments.
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Crack Propagation in Bone Captured with In Situ Mechanical Testing During AFM
Bone, like all tissues, is built from structural elements starting at the nanometer scale. The generally complex and hierarchical arrangement of these basic elements into progressively larger structural features renders bone an anisotropic and anatomically distinct material adapted to specific loads and loading cases. Due to the hierarchical structure and complexity of bone, the uncovering of structure-function relationships, i.e. the origin of material properties such as strength, toughness, and fatigue resistance, is usually a non-trivial task. Atomic force microscopy (AFM) offers an approach to overcome some of these difficulties. Because AFM allows for imaging in ambient – even hydrated conditions – it is feasible to perform in situ micro-mechanical testing experiments while conducting imaging. Here we present first data obtained from a micro-tensile testing apparatus, demonstrating the power of this technique.
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Digital Access Module™ Controller Accessory
The Digital Access Module is an optional hardware accessory for the MFP-3D™ Controller that allows user access to the digital operations of the controller. The Digital Access Module enables applications such as photon counting, synchronization of user experiments to the AFM scan, and general purpose digital I/O control.
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Electrochemistry Cell for the MFP-3D™ AFM
The Electrochemistry Cell (EC Cell) for Asylum Research MFP-3D Atomic Force Microscopes enables studies of deposition, oxidation, corrosion, and mass transfer of metals and other materials. Nanoscale topographical changes can be precisely monitored in situ as induced by electrochemical reactions. The cell provides for heating from ambient to 60ºC (optional) and can be operated in a fully sealed configuration.
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ESM of Li-ion Conductive Materials for Energy Generation and Storage
Electrochemical strain microscopy (ESM) is a novel scanning probe microscopy (SPM) technique for the Cypher™ and MFP-3D™ Atomic Force Microscopes (AFMs) that is capable of probing electrochemical reactivity and ionic flows in solids with unprecedented resolution. ESM’s capabilities are invaluable for investigating and improving performance for a broad range of energy technologies, including batteries and fuel cells for electric vehicles and grid storage. This note describes applications of ESM for Li-ion electrolytes and cathode and anode materials.
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Force Scanning with the MFP-3D™ AFMs: Two Capabilities In One
Atomic force microscopy (AFM) is able to reveal many properties about a material. Most commonly, it is used to obtain topographical information, but it can also probe mechanical stiffness, electrical conductance, resistivity, and magnetism.
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GetReal™ Automated Probe Calibration
You would never say that you are “2.5 Volts tall” or that you “gained 1.5 Volts on holiday.” The Volt is the wrong unit to measure height and weight. It’s difficult to interpret until converted to real, physical units. Yet in the world of atomic force microscopy (AFM), many of us are accustomed to seeing the cantilever deflection, amplitude, and force measured in Volts. That’s because the conventional process to calibrate the cantilever is not trivial, requires a stiff sample, and poses some risk of damage to the tip. Asylum Research’s GetReal automated probe calibration feature, exclusive to our MFP-3D™ and Cypher™ families of AFMs, makes this calibration simple, safe, and accurate. So don’t settle for Volts. GetReal!
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Humidity Sensing Cell Accessory for the MFP-3D™ AFM
The Humidity Sensing Cell is an accessory for the MFP-3D which independently measures humidity conditions with a sensor located within a sealed sample cell. This accessory also allows for simple humidity control. It is ideal for experiments where relative humidity plays an important role, such as crystal growth.
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iDrive™ Magnetic Actuated Cantilever for Effortless Cantilever Tunes in Fluid
iDrive uses a proprietary cantilever holder and cantilevers for tapping mode (AC mode) imaging of soft samples in fluid. It simplifies fluid imaging by eliminating the piezo shaker and the multitude of resonance peaks mechanically coupled from the holder and fluid. iDrive uses a patented technique where a small oscillating current flows through the cantilever legs in the presence of a magnetic field causing it to vibrate. It is exclusively available for Asylum’s MFP-3D™ and Cypher™ AFMs.
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Interactions Between Oil Droplets Probed by Force Spectroscopy with the MFP-3D™ AFM
Understanding the interactions between the colloidal particles found in emulsions is important to a range of applications from the food and pharmaceutical industries through to oil recovery and mineral flotation. The interactions which occur between emulsion droplets are of huge importance in determining the functional properties of such systems. These interactions can be modified by the adsorption at the oil-water interface of surface-active species such as small molecule surfactants, proteins or polymers. However, the physical interactions which occur between emulsified oil droplets have traditionally been a difficult area to study, with work historically being carried out on model rigid colloidal particles.1 This has changed recently following the development of methods to attach oil droplets to atomic force microscope (AFM) cantilevers. These methods have demonstrated that the measurements are sensitive to the nature of the interfacial film2 and have allowed detailed study of the force interactions between single pairs of droplets, including recent mathematical modeling.4 In this application note we will illustrate the advantages of studying a real fluid droplet system, capturing effects in the AFM data which are unique to deformable particles with a mobile interfacial layer. All work for this note was performed with an MFP-3D-BIO™ AFM from Asylum Research.
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Measuring Surface Roughness with Atomic Force Microscopy
Surface roughness at the nanoscale and below plays a crucial role in determining the functional performance of many devices. Understanding and characterizing nanoscale and even sub-angstrom roughness is becoming increasingly important in our ability to continue exploring and building devices at ever smaller length scales.
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MFP-3D™ Extended Head for High Feature Samples
As sample features increase in height, a larger Z-range is required. Asylum esearch has developed the MFP-3D Extended Head for use in its MFP-3D Atomic Force Microscopy (AFM) Systems. The new head design allows a scan range of 40 μm in Z for samples with higher features, and in particular, for bioscience applications including living cells and plant imaging.
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MicroAngelo™ – Built-in Nanolithography and Nanomanipulation
Nanolithography and manipulation capabilities have actually been around for quite some time. Remember the famous 1990 IBM image of Xe atoms manipulated using STM? Today’s demanding applications require incredibly precise and flexible instrumentation. The MicroAngelo features built into Asylum’s MFP-3D™ and Cypher™ AFM systems offer the most comprehensive capabilities and highest precision available for nanolithography and manipulation.
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NanoRack™ Sample Stretching Stage for the MFP-3D™ AFM
The NanoRack Sample Stretching Stage provides the first direct measurement method for observing nanoscale features and effects of materials under stress control. The NanoRack stage is available as an option for MFP-3D AFMs.
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New Scanning Probe Techniques for Analyzing Organic Photovoltaic Materials and Devices
Organic solar cells hold promise as an economical means of harvesting solar energy due to their ease of production and processing. However, the efficiency of such organic photovoltaic (OPV) devices is currently below that required for widespread adoption. The efficiency of an OPV is inextricably linked to its nanoscale morphology. High-resolution metrology can play a key role in the discovery and optimization of new organic semiconductors in the lab, as well as assist the transition of OPVs from the lab to mass production. We review the instrumental issues associated with the application of scanning probe microscopy techniques such as photoconductive atomic force microscopy and time-resolved electrostatic force microscopy that have been shown to be useful in the study of nanostructured organic solar cells. These techniques offer unique insight into the underlying heterogeneity of OPV devices and provide a nanoscale basis for understanding how morphology directly affects OPV operation. Finally, we discuss opportunities for further improvements in scanning probe microscopy to contribute to OPV development. All measurements and imaging discussed in this application note were performed with an Asylum Research MFP-3D-BIO™ Atomic Force Microscope.
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ORCA™ – Conductive AFM Imaging Using the MFP-3D™ AFM
Conductive AFM is a powerful current sensing technique for electrical characterization of conductivity variations in resistive samples. It allows current measurements in the range of hundreds of femtoamps to ten microamps. Conductive AFM can simultaneously map the topography and current distribution of a sample. It is a measurement useful in a wide variety of material characterization applications including thin dielectric films, ferroelectric films, nanotubes, conductive polymers, and others.
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Petri Dish Holder and Heater Accessoriesfor the MFP-3D™ AFM
The MFP-3D Petri Dish accessories are ideal sample holders for mammalian cells that are cultured and imaged in Petri dishes. They are available in two configurations: the Petri Dish Holder, which provides a modified plate for Petri dishes, and the Petri Dish Heater, which provides heating to the sample from ambient to 45°C. The Heater is ideal for sensitive cell experiments that require near-native conditions. Both options accommodate a variety of Petri dish models.
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Photoconductive AFM for Understanding Nanostructures and Device Physics of Organic Solar Cells
Plastic solar cells are emerging as alternative energy sources for the future because of their potential for cheap roll-to-roll printing, ease of processing, light weight and flexibility. However, their current performance is still low for practical applications which partially originate from the poor understanding of device physics and nanoscale morphology of the photoactive layer. Photoconductive atomic force microscopy is a powerful characterization tool to better understand the complex optoelectronic and morphological phenomena of organic solar cells at the nanoscale. All data for this work was obtained using the MFP-3D™ Atomic Force Microscope.
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Piezoresponse Force Microscopy with Asylum Research AFMs
Electromechanical coupling is one of the fundamental mechanisms underlying the functionality of many materials. These include inorganic macro-molecular materials, such as piezo- and ferroelectrics, as well as many biological systems. This application note discusses the background, techniques, problems and solutions to piezoresponse force microscopy (PFM) measurements using the MFP-3D™ and Cypher™ AFMs from Asylum Research.
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PolyHeater™ Dry Sample Thermal Accessory for the MFP-3D™ AFM
The PolyHeater is a thermal accessory for the MFP-3D that allows controlled heating of dry samples from ambient to 300°C, or from ambient to 400º C in the special high temperature PolyHeater+ version. The PolyHeater is designed for imaging and measurements in ambient air and is ideal for materials science samples such as polymers, thin films and others.
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Scanning Microwave Impedance Microscopy (sMIM)
Scanning Microwave Impedance Microscopy (sMIM) enables high resolution electrical characterization with Asylum Research MFP-3D™ and Cypher S™ atomic force microscopes (AFMs). sMIM distinguishes between changes in capacitance and resistance, allowing it to operate on a wide range of linear and non-linear materials including conductors, semiconductors, and insulators. sMIM provides higher lateral resolution (<50 nm) and superior signal-to-noise (>10X) while operating up to 80X faster and at lower power compared to competing technologies. sMIM is based on proprietary shielded AFM probes and electronics developed by PrimeNano, Inc. and is available integrated exclusively with Asylum AFMs.
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Scanning Probe Techniques for Engineering Nanoelectronic Devices
A growing toolkit of scanning probe microscopy-based techniques is enabling new ways to build and investigate nanoscale electronic devices. Here we review several advanced techniques to characterize and manipulate nanoelectronic devices using an atomic force microscope (AFM). Starting from a carbon nanotube (CNT) network device that is fabricated by conventional photolithography (micron-scale resolution) individual carbon nanotubes can be characterized, unwanted carbon nanotubes can be cut, and an atomic-sized transistor with single molecule detection capabilities can be created. These measurement and manipulation processes were performed with the MFP-3D™ AFM with the Probe Station Option and illustrate the recent progress in AFM-based techniques for nanoelectronics research.
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Simultaneous AFM and Optical Phase Contrast Using the MFP-3D™ AFM
Optical phase contrast microscopy is a popular technique for imaging low contrast, transparent samples such as cells in fluid. This technique is now standard on the MFP-3D-BIO™ Atomic Force Microscope, enabling simultaneous AFM and phase contrast imaging.
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Simultaneous Atomic Force and Fluorescence Microscopy Using the MFP-3D™ AFM
Combining Atomic Force Microscopy (AFM) and fluorescence microscopy (FM) has long been of interest for biologists. These two types of microscopies individually provide unique information about samples.
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Turnkey Glovebox Solutions for Asylum Research AFMs
Isolated environments are now essential for many research applications. Asylum Research has developed glovebox solutions for its Cypher™ and MFP-3D™ Atomic Force Microscopes. This provides a controlled environment while enabling maximum performance of the AFM. The glovebox is ideal for AFM applications including electrochemistry, batteries, photovoltaics, organic semiconductors, OLEDs, etc.
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VFM3™ Variable Field Module for Magnetic AFM Applications
The Variable Field Module (VFM3) is an ideal option for researchers who want to apply high magnetic fields to their atomic force microscopy experiments.
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Ztherm™ Modulated Thermal Analysis Option for Asylum Research AFMs
Ztherm combines powerful conventional and new advanced thermal analysis capabilities with the high resolution of AFM, and adds patent pending compensation for thermally-induced cantilever bending and measurement of contact stiffness and dissipation for the highest sensitivity and resolution available. The Ztherm Option provides highly localized heating with sensitivity to ≤10-22 liter (sub-zeptoliter) materials property changes, more than an order of magnitude improvement in volume over that previously available with commercial systems. The Ztherm Option is available for the Asylum Research MFP-3D™ and Cypher™ AFM Systems. The Ztherm option utilizes and includes Anasys ThermaLever™ probes.
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Magnetic Force Microscopy Under Applied Perpendicular Fields with Asylum Research AFMs

Understanding and engineering magnetic properties at the nanoscale is one of the key challenges in developing next-generation data storage and logic elements. The Variable Field Module (VFM3) accessory for Asylum Research MFP-3D AFMs allows us to directly observe magnetic configurations at the nanoscale using magnetic force microscopy (MFM) while the sample is under either in-plane or out-of plane applied magnetic fields.

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