New method for the measurement of stress in thin drying gel layers, produced during the formation of ceramic membranes

Voncken, J. H. L.; Lijzenga, C.; Kumar, Krishnankutty-Nair P.; Keizer, Klaas; Burggraaf, A.J.; Bonekamp, B.C.

doi:10.1007/bf00543940

Cited by 33 publications

(17 citation statements)

References 25 publications

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“…Hence sol-gel processing offers merits over other techniques, such as high purity, homogeneity, stoichiometry control, the ability to coat large and complex area substrates, ease of processing and the possibility of lowering processing temperatures. 24,25 Techniques such as Raman scattering (RS), 26 -28 optical fluorescence, 29 x-ray diffraction (XRD), 26,30 laser reflectance, 16 cantilever beam deflection 31 and wafer curvature 32 measurements have been used to determine the stress in ferroelectric materials in general and extensively of lead titanate. To the best of the author's knowledge, no extensive Raman studies exist concerning the evaluation of stress in sol-gel-derived BT thin films although RS has been used in the study of the physical properties of BT.…”

Section: Introductionmentioning

confidence: 99%

Investigations of micro‐stress and phase transition in sol–gel‐derived multideposited coatings of barium titanate using Raman spectroscopy

Gupta

2002

J Raman Spectroscopy

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Thin films of barium titanate (BaTiO 3 ; BT) of various thicknesses (20, 60, 120, 160 and 200 nm) were deposited by a modified sol-gel route on M-plane sapphire [Al 2 O 3 : (1010)] substrates. Raman spectroscopy (RS) and x-ray diffraction (XRD) were used to evaluate the stress and structural changes with respect to film thickness and establish a correlation. Raman bands and x-ray peak intensities of 20 nm thick films were too weak to reveal any structural information. Structurally, all other films showed a polycrystalline nature and the average grain size increased with increasing thickness. From the changes in the lattice parameters and one of the Raman modes [B 1 + E (TO)], an inverse relation between the compressive stress and film thickness was found at room temperature. Excellent agreement was found for stress values from both measurements. The ferroelectric to paraelectric phase transition (T C ) was estimated from the temperature dependence of one of the lattice phonon (∼310 cm −1 ) wavenumber position (!, cm −1 ) and linewidth (0, cm −1 ). This is one of the phonons belonging to the tetragonal phase. For thin films, these 'order parameters' did not show apparent anomaly and were qualitatively evaluated from the loss of intensity of this mode. The values of T C in thin films differ from those of the bulk counterpart. Almost an exponential decrease in the stress was observed with increasing thickness for the films due to the structural changes or lattice parameter relaxation. This behavior of T C is discussed using the conventional Landau-Devonshire theoretical formulation.

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Section: Introductionmentioning

confidence: 99%

Investigations of micro‐stress and phase transition in sol–gel‐derived multideposited coatings of barium titanate using Raman spectroscopy

Gupta

2002

J Raman Spectroscopy

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“…Under conditions of small deflection and film thickness relative to substrate thickness, 6 is related to the stress in the film, s, by Stoney's equation [9]: s = E, d, ! / (3L2 ( 1-VJ df) 6 where E, is Young's modulus of the substrate, d, is the substrate thickness, d, is the film thckness and v, is the substrate Poisson ratio.…”

Section: Solvent Exchanged A2 Solsmentioning

confidence: 99%

“…We have used a beam bending technique [8] to measure the change in solvation stress in a thin film as a result of adsorption [9]. The method employs the measurement of both the kinetics and the magnitude of change in stress induced in a porous f i l m as a result of changing the overlying relative vapor pressure, P/P,.…”

Section: Introductionmentioning

confidence: 99%

Preparation of Microporous Films with Sub Nanometer Pores and their Characterization Using Stress and FTIR Measurements

et al. 1996

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We have used a novel technique, measurement of stress isotherms in microporous thin films, as a means of characterizing porosity. The stress measurement was carried out by applying sol-gel thin films on a thin silicon substrate and monitoring the curvature of the substrate under a controlled atmosphere of various vapors. The magnitude of macroscopic bending stress developed in microporous films depends on the relative pressure and molar volume of the adsorbate and reaches a value of 180 MPa for a relative vapor pressure, PPo = 0.001, of methanol. By using a series of molecules, and observing both the magnitude and the kinetics of stress development while changing the relative pressure, we have determined the pore size of microporous thin films. FTIR measurements were used to acquire adsorption isotherms and to compare pore emptying to stress development. about 80% of the change in stress takes place with no measurable change in the amou9t adsorbed. We show that for sol-gel films, pore diameters can be controlled in the range of 5 -8 A by "solvent templating".

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“…In the past, optical fluorescence [12], X-ray diffraction (XRD) [13], wafer curvature measurements [14], cantilever beam deflection [15], laser reflectance [16] and Raman spectroscopy [17][18][19][20][21][22][23][24] have been used for stress analysis of ferroelectric materials. Among them, XRD and Raman 3 spectroscopy are the most popular techniques, as they are powerful tools for non-destructive investigation of structure.…”

Section: Introductionmentioning

confidence: 99%

Raman Spectroscopy and X-ray Diffraction Studies of Stress Effects in PbTiO<inf>3</inf> Thin Films

Bartasyte

Chaix‐Pluchery

Santiso

et al. 2007

2007 Sixteenth IEEE International Symposium on the Applications of Ferroelectrics

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A systematic study of domain structure and residual stress evolution with film thickness and of phase transition in c/a epitaxial PbTiO 3 /LaAlO 3 films using X-ray diffraction and Raman spectroscopy is reported. Both techniques revealed that the films are under tensile residual stress in the film plane and that a-domains are more stressed than c-domains. The two components of the large A 1 (TO) Raman modes are associated with a-and c-domains and their intensity ratio correlates to the volume fraction of a-domains. The evolution of the Raman signature with temperature revealed that the spectrum of a-domains disappears around 480°C whereas c-domains present an anomaly in their spectrum at 500°C but maintain a well-defined Raman signature up to 600°C.2

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New method for the measurement of stress in thin drying gel layers, produced during the formation of ceramic membranes

Cited by 33 publications

References 25 publications

Investigations of micro‐stress and phase transition in sol–gel‐derived multideposited coatings of barium titanate using Raman spectroscopy

Investigations of micro‐stress and phase transition in sol–gel‐derived multideposited coatings of barium titanate using Raman spectroscopy

Preparation of Microporous Films with Sub Nanometer Pores and their Characterization Using Stress and FTIR Measurements

Raman Spectroscopy and X-ray Diffraction Studies of Stress Effects in PbTiO<inf>3</inf> Thin Films

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