skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Photosynthesis and structure of electroless Ni-P films by synchrotron x-ray irradiation

Abstract

The authors describe an electroless deposition method for thin films, based on the irradiation by an x-ray beam emitted by a synchrotron source. Specifically, Ni-P films were deposited at room temperature. This synthesis is a unique combination of photochemical and electrochemical processes. The influence of the pH value on the formation and structural properties of the films was examined by various characterization tools including scanning electron microscopy, x-ray diffraction, and x-ray absorption spectroscopy. Real time monitoring of the deposition process by coherent x-ray microscopy reveals that the formation of hydrogen bubbles leads to a self-catalysis effect without a preexisting catalyst. The mechanisms underlying the deposition process are discussed in details.

Authors:
; ; ; ; ; ; ; ; ;  [1];  [2];  [2];  [3];  [2];  [2];  [2];  [4];  [5]
  1. Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan and Department of Materials Science and Engineering, National Taiwan University, Taipei 106, Taiwan (China)
  2. (China)
  3. (China) and Institute of Optoelectronic Sciences, National Taiwan Ocean University, Keelung 202, Taiwan (China)
  4. (Korea, Republic of) and Department of Materials Science and Engineering, Pohang University of Science and Technology, Pohang 790-784 (Korea)
  5. (EPFL), CH-1015 Lausanne (Switzerland)
Publication Date:
OSTI Identifier:
20979376
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Vacuum Science and Technology. A, International Journal Devoted to Vacuum, Surfaces, and Films; Journal Volume: 25; Journal Issue: 3; Other Information: DOI: 10.1116/1.2731349; (c) 2007 American Vacuum Society; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ABSORPTION SPECTROSCOPY; BUBBLES; CATALYSIS; ELECTRODEPOSITION; HYDROGEN; IRRADIATION; NICKEL COMPOUNDS; PH VALUE; PHOTOSYNTHESIS; SCANNING ELECTRON MICROSCOPY; SYNCHROTRON RADIATION SOURCES; SYNCHROTRONS; TEMPERATURE RANGE 0273-0400 K; THIN FILMS; X RADIATION; X-RAY DIFFRACTION; X-RAY SPECTRA; X-RAY SPECTROSCOPY

Citation Formats

Hsu, P.-C., Wang, C.-H., Yang, T.-Y., Hwu, Y.-K., Lin, C.-S., Chen, C.-H., Chang, L.-W., Seol, S.-K., Je, J.-H., Margaritondo, G., Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan, Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan, Department of Engineering and System Science, National Tsing Hua University, Hsinchu, 300, Taiwan, Department of Materials Science and Engineering, National Taiwan University, Taipei 106, Taiwan, Kinsus Interconnect Technology Co., Taoyuang 327, Taiwan, Department of Materials Science and Optoelectronic Engineering, National Sun Yat-Sen University, Kaoshung 804, Taiwan, X-ray Imaging Center, Pohang University of Science and Technology, Pohang 790-784, and Ecole Polytechnique Federale de Lausanne. Photosynthesis and structure of electroless Ni-P films by synchrotron x-ray irradiation. United States: N. p., 2007. Web. doi:10.1116/1.2731349.
Hsu, P.-C., Wang, C.-H., Yang, T.-Y., Hwu, Y.-K., Lin, C.-S., Chen, C.-H., Chang, L.-W., Seol, S.-K., Je, J.-H., Margaritondo, G., Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan, Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan, Department of Engineering and System Science, National Tsing Hua University, Hsinchu, 300, Taiwan, Department of Materials Science and Engineering, National Taiwan University, Taipei 106, Taiwan, Kinsus Interconnect Technology Co., Taoyuang 327, Taiwan, Department of Materials Science and Optoelectronic Engineering, National Sun Yat-Sen University, Kaoshung 804, Taiwan, X-ray Imaging Center, Pohang University of Science and Technology, Pohang 790-784, & Ecole Polytechnique Federale de Lausanne. Photosynthesis and structure of electroless Ni-P films by synchrotron x-ray irradiation. United States. doi:10.1116/1.2731349.
Hsu, P.-C., Wang, C.-H., Yang, T.-Y., Hwu, Y.-K., Lin, C.-S., Chen, C.-H., Chang, L.-W., Seol, S.-K., Je, J.-H., Margaritondo, G., Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan, Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan, Department of Engineering and System Science, National Tsing Hua University, Hsinchu, 300, Taiwan, Department of Materials Science and Engineering, National Taiwan University, Taipei 106, Taiwan, Kinsus Interconnect Technology Co., Taoyuang 327, Taiwan, Department of Materials Science and Optoelectronic Engineering, National Sun Yat-Sen University, Kaoshung 804, Taiwan, X-ray Imaging Center, Pohang University of Science and Technology, Pohang 790-784, and Ecole Polytechnique Federale de Lausanne. Tue . "Photosynthesis and structure of electroless Ni-P films by synchrotron x-ray irradiation". United States. doi:10.1116/1.2731349.
@article{osti_20979376,
title = {Photosynthesis and structure of electroless Ni-P films by synchrotron x-ray irradiation},
author = {Hsu, P.-C. and Wang, C.-H. and Yang, T.-Y. and Hwu, Y.-K. and Lin, C.-S. and Chen, C.-H. and Chang, L.-W. and Seol, S.-K. and Je, J.-H. and Margaritondo, G. and Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan and Institute of Physics, Academia Sinica, NanKang, Taipei 115, Taiwan and Department of Engineering and System Science, National Tsing Hua University, Hsinchu, 300, Taiwan and Department of Materials Science and Engineering, National Taiwan University, Taipei 106, Taiwan and Kinsus Interconnect Technology Co., Taoyuang 327, Taiwan and Department of Materials Science and Optoelectronic Engineering, National Sun Yat-Sen University, Kaoshung 804, Taiwan and X-ray Imaging Center, Pohang University of Science and Technology, Pohang 790-784 and Ecole Polytechnique Federale de Lausanne},
abstractNote = {The authors describe an electroless deposition method for thin films, based on the irradiation by an x-ray beam emitted by a synchrotron source. Specifically, Ni-P films were deposited at room temperature. This synthesis is a unique combination of photochemical and electrochemical processes. The influence of the pH value on the formation and structural properties of the films was examined by various characterization tools including scanning electron microscopy, x-ray diffraction, and x-ray absorption spectroscopy. Real time monitoring of the deposition process by coherent x-ray microscopy reveals that the formation of hydrogen bubbles leads to a self-catalysis effect without a preexisting catalyst. The mechanisms underlying the deposition process are discussed in details.},
doi = {10.1116/1.2731349},
journal = {Journal of Vacuum Science and Technology. A, International Journal Devoted to Vacuum, Surfaces, and Films},
number = 3,
volume = 25,
place = {United States},
year = {Tue May 15 00:00:00 EDT 2007},
month = {Tue May 15 00:00:00 EDT 2007}
}
  • Examines the evolution of the microstructure of Ni-P deposits with varying P content. Explains that electroless Ni-P was deposited on Cu-coated glass slides in a commercial nickel sulfate-sodium hypophosphite both held at 363K. Deposits of differing composition were prepared by varying the pH of the bath from 2.5 to 6.5 in increments of 1.0. Uses energy dispersive x-ray analyses from the electron microprobe and from the scanning transmission electron microscope (STEM) to semi-quantitatively determine the P content of the deposits as a function of pH. Finds that an amorphous-to-crystalline transformation occurs in the vicinity of 9.5 at .%P, the materialmore » being amorphous for P contents larger than 9.5 atomic percent, corresponding to a bath pH of less than or equal to4.5. Suggests that phosphorous segregation during deposition plays a role in the observed grain size variation, and a qualitative model for this is presented.« less
  • An electroless Ni-Zr-P composite film and a Ni-Nb-P composite film were plated and their heat-treating behaviors were investigated. The addition of 20g dm/sup -3/ of metallic powder resulted in a composite film that contained 21.2 weight percent (w/o) of Zr. (13.8 atom percent (a/o)), or 4.8 w/o of Nb. (2.9 a/o), respectively. Both metallic powders were dispersed uniformly throughout the film. The metallic Ni formed by the crystallization on the Ni-P matrix diffused into the metallic powders, and the amorphous Ni-Zr and Ni-Nb phases were formed by heat-treatment at 500/sup 0/ or 300/sup 0/C. Some parts of the amorphous Ni-Zrmore » phases and the metallic Ni phases combined to form intermetallic compounds by heat-treatment at 600/sup 0/C. The nickel-rich parts of the amorphous Ni-Nb phase were converted into a metastable Ni-Nb phase (zeta phase) or a Ni-Nb solid solution by heat-treatment at 700/sup 0/C. The longer heating time at 400/sup 0/C increased the amount of the Ni-Zr amorphous phase: however, it decreased the reactivity of the amorphous Ni-Zr phase. The same heat-treatment of 400/sup 0/C did not give the considerable change on the amorphous Ni-Nb phase.« less
  • This paper addresses the structural characteristics and phase transformation behaviour of plain electroless Ni-P coating and electroless Ni-P-Si{sub 3}N{sub 4}, Ni-P-CeO{sub 2} and Ni-P-TiO{sub 2} composite coatings. The X-ray diffraction patterns of electroless Ni-P-Si{sub 3}N{sub 4}, Ni-P-CeO{sub 2} and Ni-P-TiO{sub 2} composite coatings are very similar to that of plain electroless Ni-P coating, both in as plated and heat-treated conditions. Selected area electron diffraction (SAED) patterns obtained on the Ni-P matrix of Ni-P-Si{sub 3}N{sub 4}, Ni-P-CeO{sub 2} and Ni-P-TiO{sub 2} composite coatings exhibit diffuse ring patterns resembling the one obtained for plain electroless Ni-P coating. Phase transformation behaviour studied bymore » differential scanning calorimetry (DSC) indicates that the variation in crystallization temperature and the energy evolved during crystallization of plain electroless Ni-P coating and electroless Ni-P-Si{sub 3}N{sub 4}, Ni-P-CeO{sub 2} and Ni-P-TiO{sub 2} composite coatings is not significant. The study concludes that incorporation of Si{sub 3}N{sub 4}, CeO{sub 2} and TiO{sub 2} particles in the Ni-P matrix does not have any influence on the structure and phase transformation behaviour of electroless Ni-P coatings.« less
  • In contrast to recent theoretical electronic structure calculations and analysis of electron energy-loss (ELS) spectra, surface extended-x-ray-absorption fine-structure measurments establish the local structural equivalence of p(2 x 2) and c(2 x 2) oxygen on Ni(100). In both cases the oxygen atoms chemisorb in the fourfold hollow site with an O-Ni bond length of 1.96 +- 0.03 A (i.e., d/sub perpendicular/ = 0.86 +- 0.07 A). In the light of the present results the large ELS frequency shift (14 meV) between the p(2 x 2) and c(2 x 2) phases remains a puzzle.
  • The Pt L/sub 3/ edge and the Ni K edge extended x-ray-absorption fine-structure (EXAFS) measurements have been made on amorphous (Ni/sub x/Pt/sub 100-//sub x/)/sub 75/P/sub 25/ alloys at three low temperatures as well as at room temperature. With a limited k range, the Fourier transforms of the Pt L/sub 3/ and the Ni K EXAFS for amorphous Ni-Pt-P alloys exhibit extremely broad peaks which manifest an unusually large disorder of the system. As the maximum k range of the transformation is extended with an enhanced signal-to-noise ratio, these broad major peaks in the Fourier transforms still remain broad and beginmore » to split into two and finally into three. The relative magnitudes and the thermal variation of these three split peaks strongly indicate the existence of subshells for different atomic pairs such as Pt-P, Pt-Ni, and Pt-Pt. Though it is not possible, at present, to determine the degree of asymmetry in the radial distribution of each subshell, a rough simulation of the split peaks in the Fourier transforms of the Pt L/sub 3/ EXAFS data at 7 K for two compositions of amorphous Ni-Pt-P provides further evidence for the existence of separate subshells for different atomic pairs. Moreover, while the thermal disorder is apparently greater for a Pt-Pt pair subshell than those of the two other subshells, the structural disorder seems to be greater for a Pt-Ni pair subshell than that for a Pt-Pt subshell.« less