Atomic force microscopy sample preparation

Diblock copolymers PEO-fo-PS have been prepared using PEO macroinitiator and ATRP techniques [125]. The macroinitiator was synthesized by the reaction of monohydroxy-functionalized PEO with 2-chloro-2-phenylacetyl-chloride. MALDI-TOF revealed the successful synthesis of the macroinitiators. The ATRP of styrene was conducted in bulk at 130 °C with CuCl as the catalyst and 2,2 bipyridine, bipy, as the ligand. Yields higher than 80% and rather narrow molecular weight distributions (Mw/Mn < 1.3) were obtained. The surface morphology of these samples was investigated by atomic force microscopy, AFM. 

FIGURE 7.16. The peptide KFEs (of sequence FKFEFKFE) self-assembles in aqueous solution into left-handed helical ribbons, (a) Atomic force microscopy image (500 nm x 500 nm) of a peptide solution deposited over mica 8 min after preparation, (b) Same sample, 4 days after preparation (1 pm x 1 pm). 

The oldest microscopy technique for materials analysis was optical microscopy. Even to this day, for feature sizes above 1 pm, this is one of the most popular tools. For smaller features, electron microscopy techniques such as scanning electron microscopy (SEM) and transmission electron microscopy (TEM) are the tools of choice. A third family of microscopy includes scanning probe tools such as scanning tunneling microscopy (STM) and atomic force microscopy (AFM). In these relatively recent techniques, sample preparation concerns are of minor importance compared to other problems, such as vibration isolation and processing of atomically sharp probes. Therefore, the latter techniques are not discussed here. This chapter is aimed at introducing the user to general specimen preparation steps involved in optical and electron microscopy [3 7], which to date are the most common... 

Graphene has been prepared by different methods pyrolysis of camphor under reducing conditions (CG), exfoliation of graphitic oxide (EG), conversion of nanodiamond (DG) and arc evaporation of SiC (SG). The samples were examined by X-ray diffraction (XRD), transmission electron microscopy, atomic force microscopy, Raman spectroscopy and magnetic measurements. Raman spectroscopy shows EG and DG to exhibit smaller in-plane crystallite sizes, but in combination with XRD results EG comes out to be better. The CG, EG and DG samples prepared by us have BET surface areas of 46,... 

Atomic force microscopy. Scanning electron microscopes do not provide the necessary resolution for analyzing detail morphology of certain membrane layers of very fine pore sizes such as those suitable for ultrafiltration and gas separation. While transmission electron microscopes are capable of examining very small scale structures, the technique is limited to only very thin specimens. This makes sample preparation for a multilayered membrane very difficult and tedious. 

A new alternative to solve this problem is atomic force microscopy (AFM) which is an emerging surface characterization tool in a wide variety of materials science fields. The method is relatively easy and offers a subnanometer or atomic resolution with little sample preparation required. The basic principle involved is to utilize a cantilever with a spring constant weaker than the equivalent spring between atoms. This way the sharp tip of the cantilever, which is microfabricated from silicon, silicon oxide or silicon nitride using photolithography, mechanically scans over a sample surface to image its topography. Typical lateral dimensions of the cantilever are on the order of 100 pm and the thickness on the order of 1 pm. Cantilever deflections on the order of 0.01 nm can be measured in modem atomic force microscopes. 

Atomic force microscopy is a powerful method for surface characterization. It is based on an interaction between a tip mounted to a cantilever and the substrate. The latter is systematically scanned to obtain a three-dimensional picture of its surface (Figure 3.105). Contrary to other methods in high-resolution microscopy, the samples can be examined at ambient conditions, and even nonconducting materials do not require coating with a metallic conductor, so the effort for sample preparation is markedly reduced. 

In this study, we reported the preparation of mesoporous Ti02 materials via the sol-gel method involving a co-assembly of titanium (IV) isopropoxide and mainly neutral soluble starch CTMACl is used only for comparative reason. Ethanol and cyclohexane were used as solvents. The effect of key parameters, including surfactant removal process either by washing and/or by calcination and the solvent nature are discussed. Ti02 samples were characterized by means of N2 adsorption-desorption experiments, X-ray Diffraction analysis, UV-vis spectrophotometer. Scanning Electron Microscopy and Atomic Force Microscopy. 

At both routes, the determination of the size and shape of the nanoparticles is a prerequisite for description of the optical properties. Besides atomic force microscopy (AFM) and scanning electron microscopy (SEM), transmission electron microscopy (TEM) is the most powerful method to determine size and shape distributions of the nanoparticle assemblies. However, extensive sample preparation that is often required can cause preparation effects, and the TEM micrographs sometimes are not representative of the whole nanoparticle-containing insulating material. Therefore, an experimental material is required which can be investigated very easily without extensive TEM preparation. 

The thickness ho of the PDMS films on top of the PDMS brush, as measured by ellipsometry, was varied in the range of 30-150 nm. All films were obtained by spin-coating dilute heptane solutions directly (Mito the coated substrates. As indicated in Fig. 4, isothermal dewetting of the thin polymer films, i.e., the retraction of a contact line, was followed in real time (0 by optical microscopy. The morphology of the rim was also investigated by atomic force microscopy (AFM). More details on sample preparation and dewetting measurements can be found in [146, 147],... 

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