The use of transmission and analytical electron microscopy in studying reactions and phase transformations in thin film

1993 ◽  
Vol 51 ◽  
pp. 842-843
Author(s):  
K. Barmak
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Phase Transformations ◽  
Analytical Electron Microscopy ◽  
Ex Situ ◽  
Multilayer Thin Films ◽  
Absolute Concentration ◽  
Analytical Electron ◽  
Deposition Step

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.

Surface Structural Characterization and Mechanical Testing by Nanoindentation Measurements of Hybrid Polymer/clay Nanostructured Multilayer Films

2002 ◽  
Vol 17 (7) ◽  
pp. 1622-1633 ◽  
Author(s):  
Xiaowu Fan ◽  
Mi-Kyoung Park ◽  
Chuanjun Xia ◽  
Rigoberto Advincula
Keyword(s):  
Thin Films ◽  
Quartz Crystal ◽  
Ex Situ ◽  
Multilayer Thin Films ◽  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force ◽  
Diallyldimethylammonium Chloride

Nanostructured montmorillonite/poly(diallyldimethylammonium chloride) multilayer thin films were fabricated up to 100 layers thick by stepwise alternating polyelectrolyte and clay deposition from solution. The structure and morphology of the films were characterized by x-ray diffraction, ellipsometry, atomic force microscopy, and quartz crystal microbalance ex situ and in situ measurements. The mechanical properties were tested by nanoindentation. The hardness of the multilayer thin film was 0.46 GPa. The thin film's modulus was correlated to its ordering and anisotropic structure. Both hardness and modulus of this composite film were higher than those of several other types of polymer thin films.

scholarly journals Thin film stress and microstructure analysis by energy-dispersive diffraction

2014 ◽  
Vol 70 (a1) ◽  
pp. C724-C724
Author(s):  
Christoph Genzel
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Residual Stress ◽  
Film Growth ◽  
High Energy ◽  
Energy Dispersive ◽  
Film Stress ◽  
Ex Situ ◽  
Near Surface

The most important advantage of energy dispersive (ED) diffraction compared with angle dispersive methods is that the former provides complete diffraction patterns in fixed but arbitrarily selectable scattering directions. Furthermore, in experiments that are carried out in reflection geometry, the different photon energies E(hkl) of the diffraction lines in an ED diffraction pattern can be taken as an additional parameter to analyze depth gradients of structural properties in the materials near surface region. For data evaluation advantageous use can be made of whole pattern methods such as the Rietveld method, which allows for line profile analysis to study size and strain broadening [1] or for the refinement of models that describe the residual stress depth distribution [2]. Concerning polycrystalline thin films, the features of ED diffraction mentioned above can be applied to study residual stresses, texture and the microstructure either in ex-situ experiments or in-situ to monitor, for example, the chemical reaction pathway during film growth [3]. The main objective of this talk is to demonstrate that (contrary to a widespread opinion) high energy synchrotron radiation and thin film analysis may fit together. The corresponding experiments were performed on the materials science beamline EDDI at BESSY II which is one of the very few instruments worldwide that is especially dedicated to ED diffraction. On the basis of selected examples it will be shown that specially tailored experimental setups allow for residual stress depth profiling even in thin films and multilayer coatings as well as for fast in situ studies of film stress and microstructure evolution during film growth.

In-Situ Investigation of Cu-In-Se Reactions by Thin Film Calorimetry

1997 ◽  
Vol 485 ◽  
Author(s):  
D. Wolf ◽  
G. Müller
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Equilibrium Phase ◽  
Reaction Times ◽  
Practical Interest ◽  
Ex Situ ◽  
In Situ Observation ◽  
Flux Agent ◽  
In Situ Investigation

AbstractStudies of the reaction path during annealing of Cu-In-Se thin films for solar cell absorbers have been limited up to now to ex-situ analyses of the phase composition by X-Ray Diffraction (XRD) after processing by a specific temperature-time program. As an indirect method, the application of ex-situ XRD is not sufficient for the determination of reaction temperatures and reaction times for setting up a general model of CIS-formation.We show in this paper that the use of a calorimetric method (Thin Film Calorimetry, TFC) offers the advantage of a direct (in-situ) observation of thin film reactions. Special care is taken to use film thicknesses of practical interest for industrial application (1.5 – 3 μm). In a first step we show results of binary reactions in the Cu-In, In-Se and Cu-Se systems. Their knowledge is necessary for understanding the processes involved in the ternary CIS-layers. It turned out that thin Cu-In and Cu-Se films react already at room temperature and behave as predicted by the bulk equilibrium phase diagrams during heating. In-Se thin films show prominent exothermic reactions starting with the melting of In. The first phase to be formed is generally In2Se which is then converted to more Se-rich compounds. In ternary Cu-In-Se films (Cu/In = 1.00) we observe transitions of the Cu-Se-system which can be attributed to the decomposition of CuSe2 and CuSe. Consequences for the model of improved CIS-growth by a Cu-Se flux agent are discussed.

Application of analytical electron microscopy to the study of partitioning of silicon in a 2 wt% Si eutectoid steel

1978 ◽  
Vol 36 (1) ◽  
pp. 616-617
Author(s):  
N. Ridley ◽  
S.A. Al-Salman ◽  
G.W. Lorimer
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
Analytical Electron Microscopy ◽  
Eutectoid Steel ◽  
Minimum Diameter ◽  
Thin Foils ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Transformation Front

The application of the technique of analytical electron microscopy to the study of partitioning of Mn (1) and Cr (2) during the austenite-pearlite transformation in eutectoid steels has been described in previous papers. In both of these investigations, ‘in-situ’ analyses of individual cementite and ferrite plates in thin foils showed that the alloying elements partitioned preferentially to cementite at the transformation front at higher reaction temperatures. At lower temperatures partitioning did not occur and it was possible to identify a ‘no-partition’ temperature for each of the steels examined.In the present work partitioning during the pearlite transformation has been studied in a eutectoid steel containing 1.95 wt% Si. Measurements of pearlite interlamellar spacings showed, however, that except at the highest reaction temperatures the spacing would be too small to make the in-situ analysis of individual cementite plates possible, without interference from adjacent ferrite lamellae. The minimum diameter of the analysis probe on the instrument used, an EMMA-4 analytical electron microscope, was approximately 100 nm.

TEM studies of solid-state reactions in sputter-deposited Nb/Al multilayer thin films

1996 ◽  
Vol 54 ◽  
pp. 1020-1021
Author(s):  
F. Ma ◽  
S. Vivekanand ◽  
K. Barmak ◽  
C. Michaelsen
Keyword(s):  
Thin Films ◽  
Solid State ◽  
Stoichiometric Composition ◽  
Analytical Electron Microscopy ◽  
Grain Structure ◽  
Solid State Reactions ◽  
Multilayer Thin Films ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sputter Deposited

Solid state reactions in sputter-deposited Nb/Al multilayer thin films have been studied by transmission and analytical electron microscopy (TEM/AEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The Nb/Al multilayer thin films for TEM studies were sputter-deposited on (1102)sapphire substrates. The periodicity of the films is in the range 10-500 nm. The overall composition of the films are 1/3, 2/1, and 3/1 Nb/Al, corresponding to the stoichiometric composition of the three intermetallic phases in this system.Figure 1 is a TEM micrograph of an as-deposited film with periodicity A = dA1 + dNb = 72 nm, where d's are layer thicknesses. The polycrystalline nature of the Al and Nb layers with their columnar grain structure is evident in the figure. Both Nb and Al layers exhibit crystallographic texture, with the electron diffraction pattern for this film showing stronger diffraction spots in the direction normal to the multilayer. The X-ray diffraction patterns of all films are dominated by the Al(l 11) and Nb(l 10) peaks and show a merging of these two peaks with decreasing periodicity.

Determination of Thermal Conductivity of Amorphous Silicon Thin Films via Non-Contacting Optical Probing

2006 ◽  
Vol 326-328 ◽  
pp. 689-692
Author(s):  
Seung Jae Moon
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Thermal Conductivity ◽  
Amorphous Silicon ◽  
Optical Transmission ◽  
Film Deposition ◽  
Transmission Measurement ◽  
Conductive Heat ◽  
Optical Transmission Measurement

The thermal conductivity of amorphous silicon (a-Si) thin films is determined by using the non-intrusive, in-situ optical transmission measurement. The thermal conductivity of a-Si is a key parameter in understanding the mechanism of the recrystallization of polysilicon (p-Si) during the laser annealing process to fabricate the thin film transistors with uniform characteristics which are used as switches in the active matrix liquid crystal displays. Since it is well known that the physical properties are dependent on the process parameters of the thin film deposition process, the thermal conductivity should be measured. The temperature dependence of the film complex refractive index is determined by spectroscopic ellipsometry. A nanosecond KrF excimer laser at the wavelength of 248 nm is used to raise the temperature of the thin films without melting of the thin film. In-situ transmission signal is obtained during the heating process. The acquired transmission signal is fitted with predictions obtained by coupling conductive heat transfer with multi-layer thin film optics in the optical transmission measurement.

Interfacial adhesion of nanoporous zeolite thin films

2006 ◽  
Vol 21 (2) ◽  
pp. 505-511 ◽  
Author(s):  
Lili Hu ◽  
Junlan Wang ◽  
Zijian Li ◽  
Shuang Li ◽  
Yushan Yan
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Interfacial Adhesion ◽  
Interfacial Strength ◽  
Future Generation ◽  
In Situ Growth ◽  
Seeded Growth ◽  
Si Substrates ◽  
Film Substrate

Nanoporous silica zeolite thin films are promising candidates for future generation low-dielectric constant (low-k) materials. During the integration with metal interconnects, residual stresses resulting from the packaging processes may cause the low-k thin films to fracture or delaminate from the substrates. To achieve high-quality low-k zeolite thin films, it is important to carefully evaluate their adhesion performance. In this paper, a previously reported laser spallation technique is modified to investigate the interfacial adhesion of zeolite thin film-Si substrate interfaces fabricated using three different methods: spin-on, seeded growth, and in situ growth. The experimental results reported here show that seeded growth generates films with the highest measured adhesion strength (801 ± 68 MPa), followed by the in situ growth (324 ± 17 MPa), then by the spin-on (111 ± 29 MPa). The influence of the deposition method on film–substrate adhesion is discussed. This is the first time that the interfacial strength of zeolite thin films-Si substrates has been quantitatively evaluated. This paper is of great significance for the future applications of low-k zeolite thin film materials.

scholarly journals Thin film bi-epitaxy and transition characteristics of TiO2/TiN buffered VO2 on Si(100) substrates

MRS Advances ◽  
2016 ◽  
Vol 1 (37) ◽  
pp. 2635-2640 ◽  
Author(s):  
Adele Moatti ◽  
Reza Bayati ◽  
Srinivasa Rao Singamaneni ◽  
Jagdish Narayan
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Magnetic Properties ◽  
Frequency Factor ◽  
Misfit Strain ◽  
Buffer Layers ◽  
Intrinsic Defects ◽  
Domain Matching Epitaxy ◽  
Out Of Plane

ABSTRACTBi-epitaxial VO2 thin films with [011] out-of-plane orientation were integrated with Si(100) substrates through TiO2/TiN buffer layers. At the first step, TiN is grown epitaxially on Si(100), where a cube-on-cube epitaxy is achieved. Then, TiN was oxidized in-situ ending up having epitaxial r-TiO2. Finally, VO2 was deposited on top of TiO2. The alignment across the interfaces was stablished as VO2(011)║TiO2(110)║TiN(100)║Si(100) and VO2(110) /VO2(010)║TiO2(011)║TiN(112)║Si(112). The inter-planar spacing of VO2(010) and TiO2(011) equal to 2.26 and 2.50 Å, respectively. This results in a 9.78% tensile misfit strain in VO2(010) lattice which relaxes through 9/10 alteration domains with a frequency factor of 0.5, according to the domain matching epitaxy paradigm. Also, the inter-planar spacing of VO2(011) and TiO2(011) equals to 3.19 and 2.50 Å, respectively. This results in a 27.6% compressive misfit strain in VO2(011) lattice which relaxes through 3/4 alteration domains with a frequency factor of 0.57. We studied semiconductor to metal transition characteristics of VO2/TiO2/TiN/Si heterostructures and established a correlation between intrinsic defects and magnetic properties.

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