Strain in Electroless Copper Films: Analysis by in situ X-Ray Diffraction and Curvature Methods

2013 ◽  
Vol 2013 (DPC) ◽  
pp. 001358-001388
Author(s):  
Simon Bamberg ◽  
Tobias Bernhard (corresponding author) ◽  
Laurence J. Gregoriades (presenting author) ◽  
Frank Brüning ◽  
Ralf Brüning ◽  
...  

Strain in chemically deposited copper films on polymer substrates was determined by means of in situ X-ray diffraction (XRD), deposit stress analyzer (DSA) and spiral contractometer (SC). The strain evolution of the films was studied as a function of copper film thickness and electroless copper bath parameters, during and after deposition. The results are not indicative of a preferred crystallite orientation or texturing in the deposit. The copper film stress is controllable over a wide range of some 100 MPa from compressive to tensile stress by appropriate variation of bath parameters (e.g. temperature, concentration of bath components such as nickel, stabilizer and formaldehyde). A higher tendency of blister generation for relaxed or compressively stressed films is apparent, which implies that a sufficient level of tensile stress throughout the deposition promotes film adhesion. An observable change from tensile to compressive film stress during the cooling of the sample from bath operation to rinse water temperature is discussed in terms of substrate-induced thermal stress to the copper film. In this context, the difference in the substrate materials required for XRD (polymer), DSA (copper) and SC (stainless steel) may be a significant factor contributing to the diverging measured stress behaviors of the methods. Moreover, it is questionable whether SC stress data can be compared with XRD and DSA stress data, due to the low resolution of the SC method (~60 MPa).

2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.


1999 ◽  
Vol 562 ◽  
Author(s):  
Michelle Chen ◽  
Suraj Rengarajan ◽  
Peter Hey ◽  
Yezdi Dordi ◽  
Hong Zhang ◽  
...  

ABSTRACTSelf-annealing properties of electroplated and sputtered copper films at room temperature were investigated in this study, in particular, the effect of copper film thickness, electrolyte systems used, as well as their level of organic additives for electroplating. Real-time grain growth was observed by transmission electron microscopy. Sheet resistance and X-ray diffraction measurements further confirmed the recrystallization of the electroplated copper film with time. The recrystallization of electroplated films was then compared with that of sputtered copper films.


1998 ◽  
Vol 536 ◽  
Author(s):  
R. Van de Krol ◽  
E. A. Meulenkamp ◽  
A. Goossens ◽  
J. Schoonman

AbstractElectrochemical lithium intercalation in nanostructured anatase TiO2 is investigated with in-situ X-ray diffraction. A complete and reversible phase transformation from tetragonal anatase TiO2 to orthorhombic anatase Li0.5TiO2 is observed. The difference of the XRD spectra before and after insertion can be fitted with the lattice parameters of the two phases as fit parameters. The maximum amount of lithium that can be dissolved in anatase TiO2 before the phase transformation occurs is found to be very small.


1999 ◽  
Vol 564 ◽  
Author(s):  
Michelle Chen ◽  
Suraj Rengarajan ◽  
Peter Hey ◽  
Yezdi Dordi ◽  
Hong Zhang ◽  
...  

AbstractSelf-annealing properties of electroplated and sputtered copper films at room temperature were investigated in this study, in particular, the effect of copper film thickness, electrolyte systems used, as well as their level of organic additives for electroplating. Real-time grain growth was observed by transmission electron microscopy. Sheet resistance and X-ray diffraction measurements further confirmed the recrystallization of the electroplated copper film with time. The recrystallization of electroplated films was then compared with that of sputtered copper films.


1998 ◽  
Vol 546 ◽  
Author(s):  
M. Hommel ◽  
O. Kraft ◽  
S. P. Baker ◽  
E. Arzt

AbstractA special micro-tensile tester was used to carry out tensile tests of thin copper films on substrates. The elastic strain in the film was measured in-situ using x-ray diffraction and the total strain with an external strain gage. From the elastic strains the stresses in the films were calculated and stress-strain curves were obtained. It was observed that the flow stress increases with decreasing film thickness. The method was also applied to investigate the mechanical behavior of films under cyclic loading.


2020 ◽  
Vol 12 (29) ◽  
pp. 33377-33385
Author(s):  
Gül Dogan ◽  
Umut T. Sanli ◽  
Kersten Hahn ◽  
Lutz Müller ◽  
Herbert Gruhn ◽  
...  

2012 ◽  
Vol 433-440 ◽  
pp. 683-688
Author(s):  
Liu Wei Ding ◽  
Hao Ran Geng ◽  
Jing Hua Xu

Cu-38Zn thin film (wt %) was deposited on the unheated microscope glass at the nanometer scale by DC magnetron sputtering. Subsequently, the nanocrystalline films were dealloyed in H2SO4 aqueous solution etching of zinc component, resulting in the formation of nanoscale porous copper film with average porous diameter of approximately 94 nm. The films microstructure and element composition were characterized by X-ray diffraction and scanning electron microscopy. The experimental results show that Cu-38Zn films are quasi-amorphous structure, porous copper film with different porous sizes is prepared by selective dissolution of zinc atoms from a nanocrystalline dual-phase film under free corrosion conditions, the grain size of the Cu-Zn films has an important effect on the dealloying process and the microstructures of the nanoscale copper films.


2011 ◽  
Vol 172-174 ◽  
pp. 1243-1248
Author(s):  
Benoît Malard ◽  
Jan Pilch ◽  
Petr Šittner ◽  
Remi Delville ◽  
Caroline Curfs

Recovery processes responsible for evolution of microstructures in 0.1mm thin cold-drawn Ni-Ti shape memory alloy wire heat treated by DC electric pulse were investigated by combination of in-situ tensile stress - strain, electrical resistance and X-ray diffraction measurements. The X-ray data were used to obtain direct experimental information on the evolution of the phase fractions, internal strain and defects in the microstructure evolving through activation of a sequence of recovery processes during the short time electropulse treatment. It is shown that superelastic functional properties of the treated Ni-Ti wire can be precisely set by controlling the progress of the recovery processes by prescribing the time evolution of temperature T(t) and tensile stress s(t) (displacement control) in the treated wire.


2019 ◽  
Vol 8 (1) ◽  
pp. 309-319 ◽  
Author(s):  
Shahid Ali Khan ◽  
Muhammad Ismail ◽  
Yasir Anwar ◽  
Aliya Farooq ◽  
Bassam Oudh Al Johny ◽  
...  

Abstract Plant-based materials are reported to have a wide range of applications in the environmental and biomedical sectors. In this report, we present an economic and environmentally friendly supported turmeric powder (TP) biomass for the support of Ag, Ni and Cu nanoparticles (NPs) designated as Ag@TP, Ni@TP and Cu@TP. The in situ syntheses of the stated NPs were achieved in aqueous medium using NaBH4 as a reducing agent. The prepared NPs were applied for the degradation of o-nitrophenol (ONP), m-nitrophenol (MNP), p-nitrophenol (PNP), methyl orange (MO), Congo red (CR), rhodamine B (RB) and methylene blue (MB). Initially, Ag@TP, Ni@TP and Cu@TP were screened for the MO dye and antibacterial activity, where Ag@TP displayed the strongest catalytic activity for MO and bactericidal activities as compared to Ni@TP and Cu@TP. The quantity of metal ions adsorbed onto the TP was investigated by atomic absorption spectroscopy. The Ag@TP, Ni@TP and Cu@TP were characterized through X-ray diffraction (XRD), attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, thermal gravimetric analysis (TGA), energy-dispersive X-ray spectroscopy (EDS) and field emission scanning electron microscope (FESEM) analysis.


1998 ◽  
Vol 13 (10) ◽  
pp. 2962-2968 ◽  
Author(s):  
W-M. Kuschke ◽  
A. Kretschmann ◽  
R-M. Keller ◽  
R. P. Vinci ◽  
C. Kaufmann ◽  
...  

The textures of thin copper films were determined quantitatively by measuring (111) pole figures with x-ray diffraction. Measurements were performed on a variety of samples, differing in copper film thickness and deposition technique, diffusion barrier material, and the presence or absence of a cap layer. Texture changes due to an annealing treatment were also recorded and correlated with stress measurements by the wafer-curvature technique. It is found that the deposition method (PVD vs CVD) has a strong effect on texture, barrier layer effects range from negligible to significant depending on the barrier material, and the effect of a cap layer is insignificant.


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