X‐ray diffraction study of low‐energy carbon‐ion implanted Si(001)

In the search for Si‐ and C‐based crystalline phases in low‐energy ion implanted and electron‐beam annealed Si surface layers, X‐ray diffraction (XRD) measurements were performed at grazing incidence on samples of large SiC nanocrystals grown on a 90 nm thick Si layer containing C atoms. Diffraction patterns and reciprocal space maps did not reveal XRD patterns originating from the nanocrystals or the implanted layer, but did show that distortions of the Si crystal structure were introduced into the implanted layer. After annealing, the strain in the implanted layer is reduced, possibly by carbon atoms that have moved to locations close to dislocations and dislocation loops. This investigation underpins the growth theory of the SiC nanocrystals on Si, with carbon atoms migrating to form the nanostructures. Copyright © 2007 John Wiley & Sons, Ltd.     

Surface cavities produced by high‐dose nitrogen ion implantation into silicon

Nitrogen ion implantation (24 keV, 4.6 × 10¹⁷ cm^?2) into (100) a p‐type silicon wafer material and a subsequent electron beam annealing at 1100 °C for 15 s under high vacuum conditions leads to the formation of an uneven surface in the implanted region caused by nitrogen bubbles beneath the surface. Annealing at 1200 °C for 300 s results in surface cavities with a mean diameter of 350 nm and a surface coverage of 3–4% and an average depth of ～60 nm. Nuclear reaction analysis reveals that the nitrogen concentration in the as‐implanted state exceeds 57 at%, the value of stoichiometric Si₃N₄. Annealing at 1100 °C for 15 s slightly reduces the nitrogen peak concentration, whereas annealing at 1200 °C for 300 s induces a significant alteration to the shape of the nitrogen depth profile coupled with the lowering of the concentration close to the stoichiometry of Si₃N₄. The results present a new method of producing sub‐micrometre cavities embedded in a thin silicon nitride film on wafer silicon which may lead to novel micro‐electronic and biotechnology applications. Copyright © 2007 John Wiley & Sons, Ltd.     

Effect of postcasting heat‐treatment on the structure and properties of semicrystalline phase‐inversion poly(vinylidene fluoride) membranes

Microporous PVDF membranes were prepared by immersion‐precipitation in 1‐octanol of casting dopes dissolved at different temperatures, with dissolution temperature affecting strongly the membrane microstructure. The effect of postcoagulation thermal annealing, which is an additional thermal parameter, on membrane microstructure and properties is probed herein. Membranes obtained were annealed at temperatures up to 160 °C, which is close to the melting point of PVDF polymer. Annealing leads to a substantial modification of the nano‐scale fine structure of the membranes, while the overall‐microporous structure is preserved. At elevated annealing temperatures, nano‐grains, fibrils, and stick‐like crystalline entities gradually eclipse, while globules develop more robust connections based on wide bands of crystal elements. Probing by X‐ray diffraction and dynamic scanning calorimetry shows that crystallinity increases when annealing temperature and time are increased. As regards mechanical properties, the tensile strength of the membranes can be enhanced substantially, up to about 10 times, upon appropriate high temperature prolonged annealing. © 2009 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 47: 1880–1893, 2009     

Study of thermal recrystallisation in Si implanted by 0.4-MeV heavy ions

A Si crystal layer on SiO₂/Si was implanted using 0.4-MeV Kr⁺, Ag⁺, and Au⁺ at ion fluences of 0.5 × 10¹⁵ to 5.0 × 10¹⁵ cm⁻². Subsequent annealing was performed at temperatures of 450° and 800° for 1 hour. The structural modification in a Si crystal influences ion beam channelling phenomena; therefore, implanted and annealed samples were investigated by Rutherford backscattering spectrometry under channelling (RBS-C) conditions using an incident beam of 2-MeV He⁺ from a 3-MV Tandetron in random or in aligned directions. The depth profiles of the implanted atoms and the dislocated Si atom depth profiles in the Si layer were extracted directly from the RBS measurement. The damage accumulation and changes in the crystallographic structure before and after annealing were studied by X-ray diffraction (XRD) analysis. Lattice parameters in modified silicon layers determined by XRD were discussed in connection to RBS-C findings showing the crystalline structure modification depending on ion implantation and annealing parameters.     

Photocatalytic Activity for Water Decomposition to Hydrogen over Nitrogen‐doped TiO2 Nanoparticle

Nitrogen-doped TiO2 nanoparticle photocatalysts were obtained by an annealing method with gaseous ammonia and nitrogen. The influence of dopant N on the crystal structure was characterized by XRD, XPS, BET, TEM and UV-Vis spectra. The results of XRD indicate that, the crystal phase transforms from anatase to rutile structure gradually with increase of annealing temperature from 300 to 700 ℃. XPS studies indicate that the nitrogen atom enters the TiO2 lattice and occupies the position of oxygen atom. Agglomeration of particles is found in TEM images after annealing. BET results show that the specific surface areas of N-doped samples from 44.61 to 38.27 m2/g are smaller than that of Degussa TiO2. UV-Vis spectra indicate that the absorption threshold shifts gradually with increase of annealing temperature, which shows absorption in the visible region. The influence of annealing condition on the photocatalytic property has been researched over water decomposition to hydrogen, indicating that nitrogen raises the photocatalytic activity for hydrogen evolution, and the modified TiO2 annealed for 2 h at 400 ℃ under gas of NH3/N2 (V/V＝1/2) mixture shows better efficiency of hydrogen evolution. Furthermore, the N-doped TiO2 nanoparticle catalysts have obvious visible light activity, evidenced by hydrogen evolution under visible light (λ＞400 nm) irradiation. However, the catalytic activity under visible light irradiation is absent for Degussa as reference and the N-doped TiO2 annealed at 700 ℃.     

Study in the effect of annealing on hydrogen retention properties of C‐90%SiC films

Carbon‐rich silicon carbide (C‐90%SiC) films as hydrogen barriers were deposited on the surface of stainless steel substrates with magnetron sputtering, and then bombarded by argon ion beam. In order to remove the argon atoms reserved during films preparation, some samples with the prepared C‐90%SiC films were thermally annealed for 30 min at 473, 673 and 873 K in vacuum, respectively. These samples together with the un‐annealed ones were then irradiated by a 5 keV hydrogen ion beam. SEM was used to investigate the surface micrograph of those films and SIMS was used to measure the mass spectra of positive species and the depth distribution of argon and hydrogen in the samples. A remarkable decrease in hydrogen intensity in the substrates with annealing indicates that annealing for removing argon can effectively improve hydrogen retention properties of the C‐90%SiC films. Copyright © 2008 John Wiley & Sons, Ltd.     

Surface properties of hydrosilylated polyolefins annealed in supercritical carbon dioxide

Two hydrosilylated polyolefin compounds are obtained by reacting polypropylene (PP) and polyethylene (PE) with di‐ and multi‐functional hydride‐terminated poly(dimethylsiloxane) (dH‐PDMS and mH‐PDMS), respectively. The PDMS‐rich surface layers on these two samples show different Si concentrations but similar thicknesses. Samples of these materials are annealed in supercritical carbon dioxide (scCO₂) at various temperatures and pressures for different periods of time. On the PP/dH‐PDMS sample, an increase in the annealing temperature does not affect the Si concentration up to 120°C. However, the Si concentration is sharply reduced at T = 150°C at which point the surface appears to be covered by SiO₂ particles. Annealing the PP/dH‐PDMS sample for short times leads to submicron scale SiO₂ particle formation on the surface. The particles form aggregated clusters that spread all over the surface uniformly when the annealing time is extended. However, Si concentration on the PE/mH‐PDMS sample surface is enhanced as the annealing temperature increases, reaching a maximum at an annealing temperature of 100°C. No particle formation is observed on the PE/mH‐PDMS sample surface. The contact angle of both samples is found to increase with annealing temperature. Increasing the scCO₂ pressure leads to a higher Si concentration on the surfaces of both samples. On the other hand, increasing the CO₂ pressure leads to opposite trends in contact angle with the PP/dH‐PDMS sample exhibiting an increasing contact angle and the PE/mH‐PDMS sample exhibiting a decreasing one. Copyright © 2007 John Wiley & Sons, Ltd.     

Characterisation and properties of magnetron sputtered nanoscale bi‐layered Ni/Ti thin films and effect of annealing

Single‐bi‐layer of Ni–Ti thin film was deposited using DC and RF magnetron sputtering technique by layer‐wise deposition of Ni and Ti on Si(100) substrate in the order of Ni as the bottom layer and Ti as the top layer. The deposition of these amorphous as‐deposited thin films was followed by annealing at 300 °C, 400 °C, 500 °C, and 600 °C temperature with 1‐h annealing time for each to achieve crystalline thin films. This paper describes the fabrication processes and the novel characterization techniques of the as‐deposited as well as the annealed thin films. Microstructures were analysed using FESEM and HRTEM. Nano‐indentation and AFM were carried out to characterize the mechanical properties and surface profiles of the films. It was found that, for the annealing temperatures of 300 °C to 600 °C, the increase in annealing temperature resulted in gradual increase in atomic‐cluster coarsening with improved ad‐atom mobility. Phase analyses, performed by GIXRD, showed the development of silicide phases and intermetallic compounds. Cross‐sectional micrographs exhibited the inter‐diffusion between the two‐layer constituents, especially at higher temperatures, which resulted either in amorphization or in crystallization after annealing at temperatures above 400 °C. Copyright © 2015 John Wiley & Sons, Ltd.     

The microstructure and magnetic properties of Ni<Subscript>0.4</Subscript>Zn<Subscript>0.6</Subscript>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript> films prepared by spin-coating method

Nickel zinc ferrite (Ni_0.4Zn_0.6Fe₂O₄) films on Si (100) substrate were synthesized using a spin-coating method. The crystallinity of the Ni_0.4Zn_0.6Fe₂O₄ films with the thickness of about 386 nm became better as the annealing temperature increased. The films have smooth surface, relatively good packing density and uniform thickness. The volatilization of Zn is serious at 900 °C. With the increase of annealing temperature, the saturation magnetization M _s increases in the temperature ranging from 400 to 700 °C, however, decreases above 700 °C, and the coercivity H _c increases in the temperature range 400–800 °C, decreases above 800 °C. After annealed at 700 °C for 2 h in air with the heating rate 2 °C/min, the film shows a maximum saturation magnetization M _s of 349 emu/cc and low coercivity H _c of 66 Oe. The M _s is higher than others which prepared by this method, however, the H _c is lower. The M _s of Ni_0.4Zn_0.6Fe₂O₄ films annealed at 700 °C increases with increasing annealing time and the H _c changes slightly.     

Aging and cold crystallization of melt‐extruded poly(trimethylene terephthalate) films

We analyzed the thermal crystallization, glass‐transition behavior, and mechanical properties of melt‐extruded poly(trimethylene terephthalate) (PTT) films to investigate their physical aging and annealing effects. The physical aging and annealing of PTT films had an influence on the glass‐transition temperature, recrystallization behavior, and mechanical properties. When samples were aged at an ambient temperature, the crystallization temperature decreased largely within 5 h, the heat of crystallization increased, and the breaking stress and breaking elongation increased. The glass‐transition temperature of annealed samples, which was obtained from differential scanning calorimetry and dynamic mechanical measurements, increased with increasing annealing temperature below 80 °C but decreased above that temperature. In addition, the glass‐transition temperature and modulus of annealed samples were largely affected by the annealing time; in particular, they increased sharply within 1 h on annealing at 50 °C. Consequently, the change in the glass‐transition temperature on annealing was ascribed to the fact that the molecular constraint due to recrystallization and the mobility of rigid amorphous PTT chains competed with each other, being dependent on the annealing temperature. The mechanical properties of aged samples were closely related to their cold‐crystallization behavior. © 2001 John Wiley & Sons, Inc. J Polym Sci Part B: Polym Phys 39: 1920–1927, 2001     

Thickness and temperature‐dependent study of Co/Si interface

Thin films of cobalt (10, 40, and 100 nm) are deposited on Si substrate by electron beam physical vapor deposition technique. After deposition, 4 pieces from each of the wafers of silicon substrate were cut and annealed at a temperature of 200°C, 300°C, and 400°C for 2 hours each, separately. X‐ray diffraction, atomic force microscopy, and transmission electron microscopy (TEM) are used to study the structural and morphological characteristics of the deposited films. To obtain TEM images, Co films are deposited on Cu grids; so far, no such types of TEM images of Co films are reported. Structural studies confirm nanocrystalline nature with hexagonal close packed structure of the deposited Co film at lower thickness, while at higher thickness, film structure transforms to amorphous with lower surface roughness value. The particle sizes in all the cases are in the range of 3 to 5 nm. Micro‐Raman spectroscopy is also used to study the phase formation and chemical composition as a function of thickness and temperature. The results confirm that the grown films are of good quality and free from any impurity. Studies show the silicide formation at the interface during deposition. The appearance of new band at 1550 cm⁻¹ as a result of annealing indicates the structural transformation from CoSi to CoSi₂, which further enhances at higher annealing temperatures.     

Effects of gold‐induced crystallization process on the structural and electrical properties of germanium thin films

Gold‐induced (Au‐) crystallization of amorphous germanium (α‐Ge) thin films was investigated by depositing Ge on aluminum‐doped zinc oxide and glass substrates through electron beam evaporation at room temperature. The influence of the postannealing temperatures on the structural properties of the Ge thin films was investigated by employing Raman spectra, X‐ray diffraction, and scanning electron microscopy. The Raman and X‐ray diffraction results indicated that the Au‐induced crystallization of the Ge films yielded crystallization at temperature as low as 300°C for 1 hour. The amount of crystallization fraction and the film quality were improved with increasing the postannealing temperatures. The scanning electron microscopy images show that Au clusters are found on the front surface of the Ge films after the films were annealed at 500°C for 1 hour. This suggests that Au atoms move toward the surface of Ge film during annealing. The effects of annealing temperatures on the electrical conductivity of Ge films were investigated through current‐voltage measurements. The room temperature conductivity was estimated as 0.54 and 0.73 Scm⁻¹ for annealed samples grown on aluminum‐doped zinc oxide and glass substrates, respectively. These findings could be very useful to realize inexpensive Ge‐based electronic and photovoltaic applications.     

Studies on the migration in PA6‐OMMT nanocomposites: effect of annealing on migration as evidenced by ARXPS (angle resolved X‐ray photoelectron spectroscopy)

The present paper deals with experiments in which the angle resolved X‐ray photoelectron spectroscopy (ARXPS) technique was applied to investigate the phenomenon of migration in polyamide 6 with organically modified montmorillonite (PA6‐OMMT) nanocomposites. This is the first time ARXPS was used, to gain a more detailed insight into the migration process. Curve‐fitting analyses are reported which enable the differentiation between a manual mixture of PA6 with OMMT at room temperature from a nanocomposite structure. The ARXPS technique was applied to annealed samples at 250, 275, and 285°C, for 2 hr, and with three take of angles, α, of 90, 60, and 30°. The depth of the layer investigated is 9 nm in case the sample surface is well defined. By tilting the take‐off angle of the beam‐out electrons one can determine the intensity of the signals at various distances from the surface within the investigated layer. The concentration gradient of the Si signals is observed. The rate of migration is found to be more rapid in the layer closest to the surface. The intensity of the Si signals in the investigated layer is found to be 1.8 to 9.1 times that of the same composite sample at room temperature. This ratio determines the extent of migration. At temperatures higher than 250°C and times of annealing greater than 30 min a decrease in the extent of migration is observed. This decrease is explained by the gradual decomposition of the surfactant and the consequent removal of the polymeric matrix molecules from the migrating exfoliated units, culminating in denuded alumino‐silicate layers. These layers aggregate to noncolloidal microcomposite particles which do not migrate. The concentration of the exfoliated units decreases with consequent decrease in migration. A gradient of decreasing concentration of Si2p signals was observed after various times of annealing, where the gradient becomes more uniform with increase in time. Copyright © 2008 John Wiley & Sons, Ltd.     

Defect Characterization of 6H-SiC Studied by Slow Positron Beam

The defect formation and annealing behavior in as-grown and electron-irradiated 6H-SiC wafers were investi-gated by variable-energy slow positron beam. For the n-type as-grown samples, it was found that annealing decreased the defect concentration due to recombination with interstitial, and when it was annealed at 1400 ±C for 30 min in vacuum, a 20 nm thick Si layer was found on the top of SiC substrate, which is a direct proof of the Si atom diffusing to the surface when annealed at the high temperature stages. During the high temperature annealing stage, we found an obvious surface effect occurred that induced the higher S parameter close to the surface. This may be caused by the diffusion of the Si atoms to the surface during annealing. After 10 MeV electron irradiation of the n-type 6H-SiC, the positron effective diffusion length decreased from 86.2 nm to 39.1 nm. This shows that there are some defects created in n-type 6H-SiC. But in the p-type 6H-SiC irradiated by 10 MeV electrons, the change is very small. This may be because of the opposite charge of the vacancy defects. The same annealing behavior as that of as-grown 6H-SiC samples was also observed for the 1.8 MeV electron-irradiated 6H-SiC samples except that after being annealed at 300 ±C, its defect concentration increased. This may be explained as the generation of carbon vacancies, due to either the recombination between divacancies and silicon interstitial, or the charge of the charge states.     

Synthesis of W‐doped TiO2 by low‐temperature hydrolysis: Effects of annealing temperature and doping content on the surface microstructure and photocatalytic activity

A series of tungsten‐doped Titania photocatalysts were synthesized using a low‐temperature method. The effects of dopant concentration and annealing temperature on the phase transitions, crystallinity, electronic, optical, and photocatalytic properties of the resulting material were studied. The X‐ray patterns revealed that the doping delays the transition of anatase to rutile to a high temperature. A new phase W_yTi_1‐yO₂ appeared for 5.00 wt% W‐TiO₂ annealed at 900 °C. Raman and diffuse reflectance UV–Vis spectroscopy showed that band gap values decreased slightly up to 700 °C. X‐ray photoelectron spectroscopy showed that surface species viz. Ti³⁺, Ti⁴⁺, O^2?, oxygen‐vacancies, and adsorbed OH groups vary depending on the preparation conditions. The photocatalytic activity was evaluated via the degradation of methylene blue using LED white light. The degradation rate was affected by the percentage of dopants. The best photocatalytic activity was achieved with the sample labeled 5.00 wt% W‐TiO₂ annealed at 700 °C.     

Influence of thermal annealing on the microstructure,hardness and corrosion behavior of TiAlSiCuN nanocomposite films

Nanocomposite TiAlSiCuN films were deposited on high speed steels by filtered magnetic arc ion plating. Detailed properties of the films annealed at various temperatures are studied. After thermal annealing at different temperatures ranging from 400 to 800 °C, changes in the film micro‐structure, chemical and phase composition, surface morphology, hardness and polarization curve properties were systematically characterized by X‐ray diffraction, X‐ray photoelectron spectroscopy, scanning electron microscopy, nano‐indenter and electrochemical workstation, respectively. It was found that the TiAlSiCuN films could be fully oxidized at 800 °C, Al and Ti atoms all diffused outwards and formed dense protective Al₂O₃ and TiO₂ layer. Simultaneously, the TiAlN phase gradually disappeared. The films annealed at 400 °C obtained the highest hardness because of the certain grain growth and little generated oxides. Besides, the certain formation of dense protective Al₂O₃ layer made the TiAlSiCuN film annealed at 600 °C present the least corrosion current density and the corrosion voltage. Copyright © 2016 John Wiley & Sons, Ltd.     

Influence of the annealing conditions on the polarization and electromechanical response of high‐energy‐electron‐irradiated poly(vinylidene fluoride trifluoroethylene) copolymer

In this study, we investigated the influence of annealing conditions before irradiation on the ferroelectric and electromechanical properties of uniaxially stretched high‐energy‐electron‐irradiated poly(vinylidene fluoride trifluoroethylene) (HEEIP) copolymer (68/32 mol %) films. For films annealed at one fixed temperature before the irradiation (one‐step annealing), the highest crystallinity, which was highly desirable for enhancing the electromechanical response, was obtained only for films annealed between 132 and 136 °C. In addition, annealing over 10 h in this temperature window resulted in a large increase in the crystal lamellar thickness, which was required for reducing the polarization hysteresis to a minimum in the HEEIP samples. For improvements in the mechanical qualities of the uniaxially stretched films, a two‐step annealing procedure was investigated; that is, before the irradiation, the films were first annealed at a lower temperature to release the mechanical stress in the films due to the stretching and then were annealed in the high‐temperature window to raise the crystallinity and crystalline size. The experimental results indicated that this approach could produce uniaxially stretched HEEIP films with much improved mechanical qualities. Furthermore, the uniaxially stretched HEEIP films with this two‐step annealing exhibited the same electromechanical response as or an even higher one than that from the one‐step‐annealed HEEIP films. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 797–806, 2003     

Investigating Pb diffusion across buried interfaces in Pb(Zr0.2Ti0.8)O3 thin films via time‐of‐flight secondary ion mass spectrometry depth profiling

The diffusion of Pb through Pb(Zr_0.2Ti_0.8)O₃(PZT)/Pt/Ti/SiO₂/Si thin film heterostructures is studied by using time‐of‐flight secondary ion mass spectrometry depth profiling. The as‐deposited films initially contained 10 mol% Pb excess and were thermally processed at temperatures ranging from 325 to 700°C to promote Pb diffusion. The time‐of‐flight secondary ion mass spectrometry depth profiles show that increasing processing temperature promoted Pb diffusion from the PZT top film into the buried heterostructure layers. After processing at low temperatures (eg, 325°C), Pb⁺ counts were low in the Pt region. After processing at elevated temperatures (eg, 700°C), significant Pb⁺ counts were seen throughout the Pt layer and into the Ti and SiO₂ layers. Intermediate processing temperatures (400, 475, and 500°C) resulted in Pb⁺ profiles consistent with this overall trend. Films processed at 400°C show a sharp peak in PtPb⁺ intensity at the PZT/Pt interface, consistent with prior reports of a Pt₃Pb phase at this interface after processing at similar temperatures.     

Influence of the Synthetic Conditions on the Structural and Electrochemical Properties of Carbon Nano‐Onions

Thermal annealing of nanodiamonds with diameters of a few nanometers (in an inert atmosphere and at temperatures in the range: 1500–1800 °C) leads to the formation of carbon nano‐onions (CNOs) with diameters between 5 and 6 nm, which correspond to nanostructures with six to eight graphitic layers. The resulting spherical CNO structures were thermally modified under different atmospheres and characterized by SEM, TEM, thermogravimetric analysis and spectroscopic (Raman and diffuse reflectance infrared Fourier transform/FTIR) spectroscopy. The electrochemical properties of the CNOs prepared under different conditions were determined and compared. The results reveal that the CNOs show different structures with predominant spherical “small” carbon nano‐onions. The aim of this article is to investigate the impact of the CNO′s synthesis conditions on the resulting structures and study the effect of further thermal modifications on the sizes, shapes and homogeneity of these carbon nanostructures.     

Multitechnique characterization of thin films of immiscible polymer systems: PS–b‐PMMA diblock copolymers and PS–PMMA symmetric blends

Immiscible polymer systems are known to form various kinds of phase‐separated structures capable of producing self‐assembled patterns at the surface. In this study, different surface characterization methods were utilized to study the surface morphology and composition produced after annealing thin polymer films. Two different SIMS techniques—static time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) and dynamic nano‐SIMS—were used, complemented by x‐ray photoelectron spectrometry (XPS) and atomic force microscopy (AFM). Thin films (spin‐coated onto silicon wafers) of polystyrene (PS)–poly(methyl methacrylate) (PMMA) symmetric blends and diblock copolymers of similar molecular weight were investigated. Surface enrichment by PS was found on all as‐cast samples. The samples were annealed at 160 °C for different time periods, after which the blend and the copolymer films exhibited opposite behaviour as seen by ToF‐SIMS and XPS. The annealed blend surface presented an increase in the PMMA concentration whereas that of copolymers showed a decrease in PMMA concentration compared with the as‐cast sample. For blends, the nano‐SIMS as well as AFM images revealed the formation of phase‐separated domains at the surface. The composition information obtained from ToF‐SIMS and XPS, as well as the surface mapping by nano‐SIMS and AFM, allowed us to conclude that PS formed phase separated droplet‐like domains on a thin PMMA matrix on annealing. The three‐dimensional nano‐SIMS images showed that the PS droplets were supported inside a rim of PMMA and that these droplets continued from the surface like columnar rods into the film until the substrate interface. In the case of annealed copolymer samples, the AFM images revealed topographical features resembling droplet‐like domains on the surface but there was no phase difference between the domains and the matrix. In the case of copolymers, owing to the covalent bonding between the blocks, complete phase separation was not possible. The three‐dimensional nano‐SIMS images showed domain structures in the form of striations inside the film, which were not continuous until the substrate interface. Information from the different techniques was required to gain an accurate view of the surface composition and topographical changes that have occurred under the annealing conditions. Copyright © 2005 John Wiley & Sons, Ltd.