Author: Spradlin, J.K.
Paper Title Page
TUIOB01 Energetic Condensation Growth of Nb Thin-films 309
 
  • M. Krishnan, C. James, E.F. Valderrama
    AASC, San Leandro, California, USA
  • A.D. Batchelor, P. Maheshwari, F.A. Stevie
    NCSU AIF, Raleigh, North Carolina, USA
  • H.L. Phillips, C.E. Reece, J.K. Spradlin, A-M. Valente-Feliciano, X. Zhao
    JLAB, Newport News, Virginia, USA
  • K.I. Seo
    NSU, Newport News, Virginia, USA
  • Z.H. Sung
    ASC, Tallahassee, Florida, USA
 
  Funding: Funded by DE-FG02-08ER85162 and DE-SC0004994. The Jefferson Science Associates, LLC effort supported by DE-AC05-06OR23177, with supplemental funding from the American Recovery and Reinvestment Act.
This paper describes Energetic Condensation Growth of Nb films using a cathodic arc plasma, whose 40-120eV ions enable sufficient surface mobility to ensure that the lowest energy state (crystalline structure with minimal defects) is accessible to the film. Hetero-epitaxial films of Nb were grown on a-plane sapphire and MgO crystals with good superconducting properties and crystal size (10mm × 20mm) limited only by substrate size. The substrates were heated to 700 deg C and coated at 300, 500 and 700 deg C. Film thickness varied from ~0.25μm up to >3μm. Residual resistivity ratio (RRR) values (up to a record RRR-554 on MgO and RRR-328 on a-sapphire) vary with substrate annealing and deposition temperatures. XRD spectra and pole figures reveal that RRR increases as the crystal structure of the Nb film becomes more ordered, consistent with fewer defects and hence longer electron mean free path. A transition from Nb(110) to Nb(100) orientation on the MgO(100) lattice occurs at higher temperatures. SIMS depth profiles, EBSD and SEM images complement the XRD data. Crystalline structure in Nb on amorphous borosilicate substrates has implications for future, lower-cost SRF cavities.
 
slides icon Slides TUIOB01 [8.959 MB]  
 
THPO028 SIMS and TEM Analysis of Niobium Bicrystals 776
 
  • P. Maheshwari, A.D. Batchelor, D.P. Griffis, F.A. Stevie, C. Zhou
    NCSU AIF, Raleigh, North Carolina, USA
  • G. Ciovati, R. Myneni, J.K. Spradlin
    JLAB, Newport News, Virginia, USA
  • M. Rigsbee
    Materials Science and Engineering, Raleigh, USA
 
  The behaviour of interstitial impurities(C,O,N,H) on the Nb surface with respect to grain boundaries may affect cavity performance. Large grain Nb makes possible the selection of bicrystal samples with a well defined grain boundary. In this work, Dynamic SIMS was used to analyze two Nb bicrystal samples, one of them heat treated and the other non heat treated (control). H levels were found to be higher for the non heat treated sample and a difference in the H intensity and sputtering rate was also observed across the grain boundary for both the samples. TEM results showed that the bicrystal interface showed no discontinuity and the oxide layer was uniform across the grain boundary for both the samples. TOF-SIMS imaging was also performed to analyze the distribution of the impurities across the grain boundary in both the samples. C was observed to be segregated along the grain boundary for the control sample, while H and O showed a difference in signal intensity across the grain boundary. Crystal orientation appears to have an important role in the observed sputtering rate and impurity ion signal differences both across the grain boundary and between samples  
 
THPO042 Crystallographic Orientation of Epitaxial Transition Observed for Nb (BCC) on Cu and MgO (FCC) Single-Crystals 818
 
  • K.I. Seo
    NSU, Newport News, Virginia, USA
  • M. Krishnan, E.F. Valderrama
    AASC, San Leandro, California, USA
  • H.L. Phillips, C.E. Reece, J.K. Spradlin, A-M. Valente-Feliciano, X. Zhao
    JLAB, Newport News, Virginia, USA
 
  Niobium thin films were grown on (001) MgO (or Cu) single-crystal using a coaxial energetic deposition. The quality of the substrate surface and epitaxial Nb layers were investigated by the XRD and pole figure measurements. Depending on growth temperature, in-plane XRD show Kurdjumov-Sachs (KS) as well as Nishiyama-Wassermann (NW) epitaxial relationships for (110) and (001) Nb on (001) MgO. Calculation of the interface energy in rigid lattice models finds one KS and two NW minima. For the NW case the optimal atomic diameter ratio dbcc/dfcc=0.866 and 1.061, whereas for the KS case it is at dbcc/dfcc=0.919. Transitions of this type are usually induced by a change in the lattice parameter ratio resulting from a relaxation process in the early stage of the growth.  
poster icon Poster THPO042 [1.156 MB]  
 
THPO044 Structural Characterization of Nb Films Deposited by ECR Plasma Energetic Condensation on Crystalline Insulators 819
 
  • X. Zhao, H.L. Phillips, C.E. Reece, J.K. Spradlin, A-M. Valente-Feliciano
    JLAB, Newport News, Virginia, USA
  • H. Baumgart, D. Gu
    ODU, Norfolk, Virginia, USA
  • K.I. Seo
    NSU, Newport News, Virginia, USA
 
  Funding: Authored by Jefferson Science Associates, LLC under U.S. DOE Contract No. DE-AC05-06OR23177.
An energetic condensation thin film coating technique with an electron cyclotron resonance (ECR) induced plasma ion source is used to deposit Nb thin films on crystalline insulating substrates, such as a-plane and c-plane sapphire (Al2O3) and on magnesium oxide, MgO (100), (110), and (111). Heteroepitaxial Nb films were produced by ECR deposition with regulated substrate temperature. The residual resistance ratio (RRR) of about 1 micron thick films reach unprecedented values (350 - 450) on a-plane (11-20) sapphire substrates. The epitaxial relationship of Nb/crystalline substrate is found to be strongly influenced by the substrate bias voltage (adding to the initial Nb+ kinetic energy), the substrate crystalline orientation, and heating conditions. At low substrate temperature, the Nb films demonstrated non-epitaxial crystalline textures, revealed by XRD Pole Figure technique and Electron Backscattering Diffraction (EBSD). The texture might be caused by “Volmer-Weber” growth mode, i.e. island growth, at low surface adatom mobility. This study shows that the film’s crystal structural character has great impact on its RRR/Tc value.
 
 
THPO064 Structural Properties of Niobium Thin Films Deposited on Metallic Substrates by ECR Plasma Energetic Condensation 877
 
  • J.K. Spradlin, H.L. Phillips, C.E. Reece, A-M. Valente-Feliciano, X. Zhao
    JLAB, Newport News, Virginia, USA
  • D. Gu
    ODU, Norfolk, Virginia, USA
  • K.I. Seo
    NSU, Newport News, Virginia, USA
 
  Funding: Authored by Jefferson Science Associates, LLC under U.S. DOE Contract No. DE-AC05-06OR23177.
Particle accelerator technologies rely on SRF cavities to create the accelerating gradient for beam lines. Solid niobium cavities are widely employed throughout the community despite high material, fabrication, and operation cost. New thin film technologies are being explored for the suitability of niobium coatings for accelerating cavities. Thin layers of high-quality niobium would be deposited on a base material that has lower material and fabrication cost. Copper is a strong candidate for the cavity base due to availability, cost, machinability, and potentially improved performance characteristics of the niobium SRF surface. Initial results of TEM, EBSD and XRD analyses of niobium thin films grown on copper substrates under controlled conditions are presented to demonstrate the feasibility of the technology and establish lower limits of performance characteristics. Correlation of RRR data with the structure of niobium thin films will demonstrate the importance of thin film structural quality.
 
 
THPO074 SRF Multilayer Structures based on NbTiN 920
 
  • A-M. Valente-Feliciano, H.L. Phillips, C.E. Reece, J.K. Spradlin
    JLAB, Newport News, Virginia, USA
  • A.D. Batchelor, F.A. Stevie
    NCSU AIF, Raleigh, North Carolina, USA
  • R.A. Lukaszew
    The College of William and Mary, Williamsburg, USA
  • K.I. Seo
    NSU, Newport News, Virginia, USA
 
  Funding: Authored by Jefferson Science Associates, LLC under U.S. DOE Contract No. DE-AC05-06OR23177.
For the past three decades, bulk niobium has been the material of choice for SRF cavities applications. In the recent years, RF cavities performances have approached the theoretical limit for bulk niobium. For further improvement of RF cavity performance for future accelerator projects, an interesting alternative has been recently proposed by Alex Gurevich with the Superconductor-Insulator-Superconductor multilayer approach, using the benefit of the higher critical field Hc2 of higher-Tc superconductors without being limited with their lower Hc1. JLab is pursuing this approach with the development of multilayer structures based on NbTiN via magnetron sputtering and High Power Impulse Magnetron Sputtering (HiPIMS). Insulators such as, AlN, Al2O3 and MgO are being investigated as candidates for the insulator layers. This paper present the preliminary results on the characteristics of NbTiN and insulator layers and a first attempt of a NbTiN-based multilayer structure on bulk Nb and thick Nb films.
 
 
THPO079 Surface Preparation of Metallic Substrates for Quality SRF Thin Films 936
 
  • J.K. Spradlin, O. Trofimova, A-M. Valente-Feliciano
    JLAB, Newport News, Virginia, USA
 
  Funding: Authored by Jefferson Science Associates, LLC under U.S. DOE Contract No. DE-AC05-06OR23177.
Surface preparation is an essential prerequisite for thin film depositions. Rough or chemically impure surfaces adversely affect the nature of the thin film. Understanding the properties of the substrate and how they influence the quality of the thin film is necessary to transfer thin film deposition technologies to SRF cavity applications. A substrate that is flat, has sufficient grain size, and is chemically pure is the ideal starting point for thin film depositions. A method for copper substrate preparation is reviewed for niobium thin film deposition that provides epitaxy on large and fine grain copper as well as single crystal copper. Preliminary data on niobium and aluminum substrate preparation will also be included.
 
poster icon Poster THPO079 [0.637 MB]