AFM-IR Spectroscopy

We developed an approach for analysis of reflectance spectra with bands of interference origin, for thin porous nanostructured layers on silicon wafers and made the automatic reflectometry equipment to examine optical characteristics (reflectance coefficient, refractive index) in the visible, near- infrared and mid- infrared range. The method is applied to por-Si, por-CoSi2 and por-A Os layers on c-Si substrate. The reflectance spectra, recorded at different light incidence angles permit to detect both the refractive index and layer thickness simultaneously. TEM, AFM, IR spectroscopy investigations of these layers confirmed the presence of Si nanocrystals. 

Awatani T, Midorikawa H, Kojima N, Ye J, Marcott C. Morphology of water transport channels and hydrophobic clusters in Nation from high spatial resolution AFM-IR spectroscopy and imaging. Electrochemistry Communications 2013 30 5. 

Shekhah et al. [146] used LBL or liquid phase epitaxy to fabricate porous MOF thin films. The two components, copper (II) acetate (Cu[ac]2> and 1,3,5-benzenetricar-boxylic acid (Hjbtc), were dissolved in ethanol and the substrate was immersed into each solution in a cyclic way. Each immersion was followed by rinsing with ethanol. By starting with Cu(ac)2, a linear increase of thickness of the deposited HKUST-1 layer with the number of (alternating) immersion cycles in Cu(ac)2 and H3btc was observed. The thickness of deposited film was monitored by AFM, IR spectroscopy and X-ray-photoelectron spectroscopy. 

SAXS), IR spectroscopy, NMR, transmission electron microscopy (TEM), or atomic force microscopy (AFM) and the thermal transitions by DSC and DMA. 

An indication of such a morphological transition is a pronounced enhancement of oxide film roughness at a thickness of 11 nm, observed by AFM, as shown in Fig. 5.5. The appearance of this surface ripple corresponds to the first potential peak in Fig. 5.4. An investigation using differential IR spectroscopy revealed that the peak position, width and degree of symmetry of the Si-O absorption bands... 

ID IQ 2D 2D-NMR 2h2o 2Q 3Q 9BEN A1 ABS AC ACM ACN AFM Al-CSM ALMA-i5 Al-m-EPDM AN AO APT ASTM ATR ATR-IR B/S BABA Two-dimensional Single-quantum One-dimensional Deuteron solid-state NMR Deuterated water Double-quantum Triple-quantum 9 borobicyclo [3, 3, 1] nonane Amide 1 Acrylonitrile-butadiene-styrene terpolymer Accelerator Acrylate rubber Acrylonitrile Atomic Force Microscopy Aluminium salt of chlorosulfonate polyethylene Allyl-rf5 methacrylate Aluminium salt of maleated EPDM Acrylonitrile 1-Allyl oxyoctane Attached Proton Test American Standards for Testing and Materials Attenuated total reflectance spectroscopy Attenuated total reflectance-IR spectroscopy Butadiene/styrene Back-to-back... 

Table 3 lists some ionization properties of functionalized gold-thiol monolayers and relevant alkylsiloxane monolayers together with the appropriate bulk values. Monolayers with carboxylate terminal groups show abnormal wetting behaviour, which makes it difficult to determine accurately their surface pKa values308. Apart from contact angle titration, other methods were also used to study proton transfer equilibria at the mono-layer surfaces, such as quartz crystal microbalance (Table 3, line 1), measurements of the adhesion force between the monolayer deposited at the surface of an AFM tip and the same monolayer deposited on the substrate (chemical force microscopy, Table 3, lines 3, 4, 15), FT-IR spectroscopy (Table 3, line 7), adsorption of polyelectrolytes (Table 3, line 5) and differential capacitance measurements (Table 3, lines 12, 13). 

From examining the spectroscopic characteristics of diamond films, many insights into their structure may be obtained. Most of all the Raman spectroscopy, XRD and electron energy loss spectroscopy (EELS) provide valuable information. Other methods like IR-spectroscopy and XPS shed light on the surface structure. These techniques are supplemented by microscopy methods, for example, by AFM and STM, so altogether the morphology of the films surface can be studied in quite some detail. 

C at 95% relative humidity, favoring moisture condensation on the metal surface. Upon removal from the packages the surface of the steel samples has been studied by IR spectroscopy (IRS), using the method of attenuated total reflectance (ATRMVTIR), X-ray photoelectron spectroscopy (XPES), X-ray structural analysis (XSRDA), atomic-force microscopy (AFM) and scanning electron microscopy (SEM). 

IR has been used in addition to many other techniques to anaiyze poiymer and copoiymer compositions, either by itseif or in addition to other techniques. Recentiy, the characterization by spatiai differentiation of submicrometer domains in poly(hydroxyalkanoate) copolymer by the combination of atomic force microscopy (AFM) and IR spectroscopy was reported [9, 10]. This new capability resulting from the combination of two single instruments enables the spectroscopic characterization of microdomainforming polymers at levels not previously possible. 

In order to understand the behavior of surfaces after surface modification, it is essential to examine their surface composition and structure in detail. A large number of techniques are available, and it is often desirable to combine several of these methods. The techniques used to monitor surface properties include scanning electron microscopy (SEM), optical profilometry, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, imaging ellipsometry, and water contact angle measurements. 

SHG) [610], total internal reflection fluorescence (TIRF) spectroscopy [611], UV/Vis spectroscopy, IR spectroscopy, ellipsometry [612], quartz crystal microbalance (QCM) [613], STM [614], and AFM (see Refs. [618-623] for review of in sitn spectroscopies). From those, only the vibrational methods (SHG, SERS, and IR spectroscopy) are able to provide information on both the chemical composition and the strnctnre of the species adsorbed. The IR SEC experiment is simpler and more accessible than SHG and SERS, making IR spectroscopy the dominant tool for stndying electrochemical reactions at metallic electrodes [616, 617, 624-641]. 

Other uses of an IR microscope in forensic analysis include the examination of fibers, drugs, and traces of explosives. For example, oxidation of hair can occur chemically or by sunlight oxidation of cystine to cysteic acid can be seen in hair fibers by FTIR microscopy (Robotham and Izzia). Excellent examples in full color of FTIR imaging microscopy can be found on the websites of companies like PerkinElmer and Thermo Fisher Scientific. Our limitations in use of gray scale make many of the examples unsuited for reproduction in the text. A novel IR microscope combined with atomic force microscopy, the nanoIR platform from Anasys Instruments (www.anasysinstruments.com), permits nanoscale IR spectroscopy, AFM topography, nanoscale thermal analysis, and mechanical testing. 

It is only very recently that we have seen the first results of detection by infrared and Raman spectroscopy of organometallic complexes within cells. The first experiments were carried out with microscopes attached to infirared or Raman spectrometers, followed by other studies taking advantage of new techniques, specifically AFM-IR and surface-enhanced Raman spectroscopy (SERS). 

AFM-IR is a cutting-edge technique set up in 2005 by A. Dazzi, a physicist at the University of Paris 11, under the name of PT-IR (photothermally induced resonance), which has revolutionized the domain of infrared spectroscopy [149,150]. It is based on the coupling of an AFM with a tunable pulsed infrared laser emitting in the mid-infrared region (1200-3200 cm ). The sample is laid on the upper surface of a zinc selenide prism, analogous to the one used for ATR... 

The application of AFM and other techniques has been discussed in general terms by several workers [350-353]. Other complementary techniques covered in these papers include FT-IR spectroscopy, Raman spectroscopy, NMR spectroscopy, surface analysis by spectroscopy, GC-MS, scanning tunnelling microscopy, electron crystallography, X-ray studies using synchrotron radiation, neutron scattering techniques, mixed crystal infrared spectroscopy, SIMS, and XPS. Applications of atomic force spectroscopy to the characterisation of the following polymers have been reported polythiophene [354], nitrile rubbers [355], perfluoro copolymers of cyclic polyisocyanurates of hexamethylene diisocyanate and isophorone diisocyanate [356], perfluorosulfonate [357], vinyl polymers... 

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