Advances in Physical Vapour Deposition based on High Power Impulse Magnetron Sputtering (HIPIMS)
Submitting Institution
Sheffield Hallam UniversityUnit of Assessment
Electrical and Electronic Engineering, Metallurgy and MaterialsSummary Impact Type
TechnologicalResearch Subject Area(s)
Chemical Sciences: Analytical Chemistry, Macromolecular and Materials Chemistry
Engineering: Materials Engineering
Summary of the impact
    Ehiasarian and Hovsepian of the Materials and Engineering Research
      Institute (MERI) have achieved significant economic impact through
      industrial uptake of their innovations in High Power Impulse Magnetron
      Sputtering (HIPIMS). Exploiting these innovations, HIPIMS treatments have
      been used by manufacturers to enhance the surface properties of millions
      of pounds worth of products. Applications include industrial blades,
      components within jet turbines, replacement hip joints, metallised
      semiconductor wafers and satellite cryo-coolers. Patents based on
      Ehiasarian and Hovsepian's research have achieved commercial success. In
      the REF impact period, HIPIMS machines equipped to deliver MERI''s HIPIMS
      surface pre-treatment have achieved sales of over £5m, and income
        generated through SHU's HIPIMS-related licences has totalled £403,270.
      In 2010 Ehiasarian's group established the Joint Sheffield Hallam
        University-Fraunhofer IST HIPIMS Research Centre, the first such
      Centre in the UK. This has broadened the industrial uptake of MERI's
      HIPIMS technologies and stimulated a network of sub-system providers.
    Underpinning research
    Hovsepian joined MERI in 1997 as a Senior Research Fellow in what was the
      then Surface Coatings Research Centre led by Prof Dieter Munz (submitted
      for REF2001, retired 2003). Hovsepian was promoted to a personal Chair in
      2004 and assumed the Head of Research Centre role when Munz retired.
      Ehiasarian completed his PhD in the Surface Coatings Research Centre in
      2002, was appointed to a permanent independent researcher role in MERI in
      April 2004 (he was entered in RAE2008 as an Early Stage Researcher on that
      basis) and promoted to a personal Chair in 2011. Both Ehiasarian and
      Hovsepian were submitted by MERI in RAE2008 and both have been at SHU
      throughout the REF period.
    HIPIMS is a plasma vapour deposition (PVD) method for surface treatment
      and coating. It uses a powerful plasma discharge to generate an ionised
      vapour that is free of macro-particles. This vapour can be used either to
      pre-treat surfaces of target components or to deposit a range of coatings
      of specified composition and nanostructure. As detailed in section 4,
      surface pre- treatments and nano-scale coatings based on Ehiasarian and
      Hovsepian's HIPIMS advances have achieved a number of economic impacts,
      most obviously by enhancing the properties and utility of a range of
      end-products.
    MERI's contributions to HIPIMS originate from Ehiasarian's thesis work
      (supervised by Munz and other permanent staff, and partially supported by
      [i]) which focused on the plasma physics diagnostics of what was, at the
      time, a very new branch of PVD. A specific innovation that resulted from
      this was a methodology for achieving "fully-dense hard" HIPIMS coatings
      [1,A]. This methodology, based on use of short bursts of very intense
      driving currents, proved capable of eliminating the intergranular pores
      commonly found in PVD coatings. Subsequent research performed within MERI
      between 2002 and 2012 addressed the fundamental issues of:
    
      - HIPIMS coating microstructure, composition and adhesion [2.3,5];
 
      - plasma pre-treatment of substrates [3];
 
      - electrical gas discharge physics, plasma chemistry and distribution
        [4,6];
 
      - and field-controlled plasma manipulation within the HIPIMS chamber
        [4].
 
    
    This work demonstrated that previously unobtainable wear-resistance and
      coverage properties could be realised using appropriate combinations of
      electric and magnetic fields to manipulate the parent plasmas of different
      source materials [4-6,ii-iv]. Further research studied process-microstructure-performance
	  relationships in HIPIMS-deposited thin films
      [2.3,5], particularly microstructure evolution and self-organisation
      phenomena.
    In 2007 the group's HIPIMS machinery was up-graded to industrial
      production grade with an automated system. Uniquely, within the University
      sector, this provided an ability to develop the industrial applicability
      of HIPIMS innovations. This up-scaling proved to be critical in realising
      technology transfer to the manufacturing sector and, so, achieving
      international impact. In particular, it enabled the development of
      coatings for auto- and aero-engine components [v,vi], cryogenic materials
      [vii], photovoltaic cell layers [viii], and biocompatible, antibacterial
      coatings [ix].
    In RAE2008, the strong research quality of the MERI Surface Coatings
      Research Centre, under which this work was submitted, was specifically
      highlighted in the final HEFCE feedback. The academic and industrial
      reputation of HIPIMS research at MERI was further consolidated in 2010
      with the establishment of the Joint Sheffield Hallam
        University-Fraunhofer HIPIMS Research Centre, partnered with the
      Fraunhofer Institute for Surface Engineering (Braunschweig, Germany) [B].
      This was the first such centre in the UK. Ehiasarian is its Director.
      Also, in 2010, EPSRC supported the establishment of a joint centre between
      University of Leeds, University of Sheffield and MERI to establish a "National
        Innovation Playground to Widen the Operational Envelope for Tribological
        PVD Coatings" [iv]. Within this collaboration, Ehiasarian and
      Hovsepian contributed HIPIMS solutions to tribological problems for UK
      industry.
    References to the research
    
[1] Ehiasarian, A.P., New, R., Munz, W.D., Hultman, L., Helmersson, U.
      and Kouznetsov, V., "Influence of high power densities on the composition
      of pulsed magnetron plasmas", Vacuum 65, 147 (2002).
      DOI: 10.1016/S0042-207X(01)00475-4 136 citations (WoS, Sept 2013)
      KEY REFERENCE
     
[2] Ehiasarian, A.P., Munz, W.D., Hultman, L., Helmersson, U. and Petrov,
      I., "High power pulsed magnetron sputtered CrNx films", Surface and
        coatings technology 163-164, 267 (2003)
      DOI: 10.1016/S0257-8972(02)00479-6 129 citations (WoS, Sept 2013)
     
[3] Ehiasarian, A.P.; Hovsepian, P.E., Hultman, L., and Helmersson, U.
      "Comparison of microstructure and mechanical properties of chromium
      nitride-based coatings deposited by high power impulse magnetron
      sputtering and by the combined steered cathodic arc/unbalanced magnetron
      technique", Solid Films 457, 270 (2004)
      DOI: 10.1016/j.tsf.2003.11.113 88 citations (WoS, Sept 2013)
      KEY REFERENCE
     
[4] Hecimovic, A., Burcalova, K. and Ehiasarian, A.P., "Origins of ion
      energy distribution function (IEDF) in high power impulse magnetron
      sputtering (HIPIMS) plasma discharge". Journal of Physics D: Applied
        Physics, 41, 095203 (2008)
      DOI: 10.1088/0022-3727/41/9/095203 25 citations (WoS, Sept 2013)
     
[5] Ehiasarian, A.P., Vetushka, A., Gonzalvo, Y.A., Safran, G., Szekely,
      L. and Barna, P.B., "Influence of high power impulse magnetron sputtering
      plasma ionization on the microstructure of TiN thin films", Journal of
        Applied Physics, 109, 104314 (2011)
      DOI: 10.1063/1.3579443 5 citations (WoS, Sept 2013)
      KEY REFERENCE
     
[6] Ehiasarian, A.P., Hecimovic, A., De Los Arcos, T., New, R.,
      Schulz-von der Gathen, V, Boke, M. and Winter, J., "High power impulse
      magnetron sputtering discharges: Instabilities and plasma
      self-organization", Applied Physics Letters, 100, 114101
      (2012)
      DOI: 10.1063/1.3692172 11 citations (WoS, Sept 2013)
     
[i] EPSRC GR/R32420/01, PI Munz "Droplet Free Metal Ion Source for PVD
      Hard Coating Production" £76k (2001-03)
    [ii] EPSRC EP/0049202/1, PI Ehiasarian "Fundamentals of High Power
      Impulse Magnetron Sputtering (HIPIMS) - Plasma Studies and Materials
      Synthesis" £190k (2006-09)
    [iii] EU FP6, PI Hovsepian "CORRAL- Corrosion Protection with Perfect
      Atomic Layers" £61k (2008-11)
    [iv] EPSRC EP/H050116/1 PI Hovsepian "National Innovation
      Playground to Widen the Operational Envelope for Tribological PVD Coatings"
      total £3.5m, to SHU £389k (2010)
    [v] EU FP6 project, Hovsepian and Ehiasarian Investigators "INNOVATIAL"
      total €12.5M, to SHU €1.1M (2005-9).
    [vi] Mahle GmbH (Brazil), PI Ehiasarian "Licence agreement for
      HIPIMS coating recipes for automotive engine piston rings" £50k (2013)
    [vii] STFC RAL, PI Ehiasarian "Regenerator Technology for
      Stirling and Pulse Tube Cryogenic Coolers" £40k (2008-11)
    [viii] EPSRC EP/J011398/1, PI Ehiasarian "High Efficiency CuInSe2
      Photovoltaic Modules Deposited at Low Temperature by HIPIMS" £329k
      (2012-15)
    [ix] Biomet (UK/USA), PI Ehiasarian "Licence agreement for HIPIMS
      coating recipes, for use on metal-on-metal hip implants" £300k (2012-14)
      £100k of which is in the REF period
    Details of the impact
    MERI's HIPIMS research has achieved three streams of economic impact:
      roll out of HIPIMS surface pre-treatment methods through coating system
      manufacturers; direct collaboration with product manufacturers; and
      discipline leading activities associated with the joint SHU-Fraunhofer
      HIPIMS Research Centre.
    Economic impact by roll out of HIPIMS surface pre-treatment methods
          and other patents
    In parallel with their academic research and publications, Ehiasarian and
      Hovsepian have developed a portfolio of patents to protect the IP in their
      HIPIMS innovations. Commercially, the most important of these has proved
      to be EP1260603B1 [A] (filed 2001, granted 2006, validated in 12 EU
      states), relating to the HIPIMS surface pre-treatment stage in the coating
      production process [1]. This patent has been monetised by equipping
      coating systems with special (licensed) modules that deliver the
      pre-treatment described in [A]. MERI's HIPIMS pre-treatment technology has
      been licensed non-exclusively in this way to four leading PVD coating
      system manufacturers: Ionbond AG (Switzerland) [C]; SVS Vacuum
        Coating Technologies GmBH & Co (Germany); Hauzer Techno
        Coating AG (The Netherlands) [D]; and CemeCon AG (Germany).
      This has achieved two classes of beneficiary: the coating system
      manufacturers, whose systems have been enhanced through incorporation of
      the MERI module; and system purchasers, who have acquired the capability
      of producing enhanced components. HIPIMS technology has become a key
      activity of Hauzer Techno Coating (~200 employees) [D] and CemeCon
      in the REF impact period.
    Licence revenue paid to SHU (at a rate of €50k for entry to the programme
      and €25k for each sale or retrofit of a coatings system) explicitly links
      the system manufacturers and purchasers to the research described in section
        2. In the REF impact period, six licensed systems have been
      manufactured and two more retro-fitted. These have generated more than £5m
      of sales to the manufacturer beneficiaries and £238,089 of
        licence income to SHU. All licences (including those established
      before the REF period) will run through to expiry of the patent [A] in
      2021. As a result, the operators of ten coating systems have been beneficiaries
      in the "system purchasers" sense over the REF impact period. Ehiasarian
      and Hovsepian have no direct interaction with the "system purchasers", so
      their specific uses of HIPIMS, and the associated sales figures, are in
      commercial confidence. However, typical applications are known to include
      wear and oxidation-resistant coatings for automotive engine components,
      resulting in longer lifespans and higher operating temperatures, and
      special coatings for dry high-speed machining tools, which yield enormous
      improvements in cutting-tool lifetimes and machining speeds. Each of the
      ten HIPIMS systems equipped with the MERI surface pre-treatment stage has
      the capacity to produce £10+m of components per year. Systems have been
      operating on two shifts per day to produce a range of high-value
      components [C,D].
    In 2006 a further patent application was made to protect bias power
      supply designs developed within an industrial collaboration. This was
      granted in the UK (GB0607269B) and China (CN101461032B) [E] and remains in
      application stage in Europe, Korea and Japan. It is co-owned by SHU, Hauzer
        Techno Coating [D] and Huettinger Electronic Sp z.o.o. [F],
      with Ehiasarian and Hovsepian the leading inventors. This technology was
      commercialised in 2010, the two industrial co-owners retaining
      manufacturing and sales rights. Within the REF impact period, it has
      resulted in power supply unit sales exceeding £1m (beneficiaries Hauzer,
      Huettinger and their clients) and licence income to SHU of
      £15,181k.
    Later patent filings by Ehiasarian and Hovsepian cover aspects such as
      differing coating types and technical advances such as high rate
      deposition, rare metal ion etching and inductively coupled etching. These
      have not earned any income in the REF impact period, but have been
      maintained within the overall IP portfolio due to their continued
      commercial potential.
    Economic impact by direct collaboration with product manufacturers
    Within the second impact stream identified above, Ehiasarian has
      delivered or started delivering collaborative and/or licensed research to
      a series of large manufacturers. In each case, the manufacturer is a
        beneficiary through enhancements made to their products. These
      include large licence contracts with Mahle (£50k)
      [vi] and Biomet (£100k pa for three years) [ix] to develop
      coatings for automotive piston rings and metal-on-metal hip implants,
      respectively. Additional collaborations yielding economic impact
        through product enhancement include:
    
      - a £100k project funded by OC Oerlikon Balzers (2006-10), to
        develop HIPIMS coating deposition technology to allow writing of
        miniaturised 3D-Integrated microelectronics devices. The company has
        integrated this capability into its Clusterline 200 system, a
        multi-stage coating machine, leading to sales exceeding €20m;
 
      - a 2008-11 collaboration with the Space Science Technology Department
        of the Rutherford Appleton Laboratory (RAL) [vii], through which
        coatings developed by the Ehiasarian group overcame a long-standing
        issue with RAL's cryo-coolers for satellite applications. This work led
        to the satellites being judged flight worthy and superior to competitor
        technologies [G];
 
      - a 2011 collaboration with The Gillette Company (USA) which
        resulted in a granted patent (US7966909B) [H] for a new HIPIMS-based
        process for manufacturing razor blades with high aspect ratio cutting
        edge and, therefore, improved shaving properties. The patent is the
        property of Gillette with Ehiasarian and Hovsepian listed as named
        inventors;
 
      - a 3-year (from 2013) research and development contract with Rolls
          Royce to develop HIPIMS technologies appropriate to aero-engine
        turbine blades [J].
 
    
    Economic impact through discipline leading activities
    The symbiotic joint SHU-Fraunhofer HIPIMS Research Centre provides
      technical and infrastructural benefits to both partners. The resultant
      "critical mass" of HIPIMS expertise encompasses the capability needed both
      to deliver large projects and also to support strategic industrial
      development programmes in the UK, Germany and worldwide. This has resulted
      in a large EPSRC-supported collaboration on high efficiency solar-cell
      glass panels [viii] with Pilkingtons (UK), Gencoa (UK) and
      Von Ardenne (Germany). The Joint Centre has also started to deliver
      HIPIMS expertise to other companies such as Bosch and DOT GmbH,
      Germany [B]. Since the prime function of the Fraunhofer IST is KT
      and technology transfer, it can be viewed as a beneficiary under
      REF impact, as can the collaborating industrial partners.
    A further broadening of the MERI HIPIMS group's impact relates to the
      discipline-leading activities through which it has expanded the field of
      HIPIMS and, in particular, its industrial uptake. This expansion has
      stimulated the development of a network of sub-system and component
      providers who are a final group of beneficiaries. This includes
      providers of analytical equipment, specialist power supplies and magnetron
      systems and targets. This network is demonstrated by, for example the ~20
      industrial exhibitors at the 2012 and 2013 annual International
      Conferences on HIPIMS [K] run by MERI and the Fraunhofer IST.
    Sources to corroborate the impact 
    [A] Patent EP1260603B1 http://www.google.com/patents/EP1260603B1?cl=en
    [B] The Joint Sheffield Hallam University-Fraunhofer HIPIMS Research
        Centre is noted on
        http://hipims.fraunhofer.de/en/collaboration/ and can be
      corroborated by the Director of Fraunhofer IST, corroborating source 1
    [C] Chief Technical Officer Ionbond AG, corroborating source 2
    [D] CEO Hauzer Techno Coating AG, corroborating source 3
    [E] Patent GB0607269B CN101461032B https://www.google.com/patents/CN101461032B?cl=en
    [F] CEO Huettinger Electronik Sp. z.o.o., corroborating source
      4
    [G] Quotes from representative of, Space Science Technology Department,
      Rutherford Appleton Laboratory, UK in relation to HIPIMS coatings
      developed for satellite cryo-coolers
      http://rseeccleston.blogspot.co.uk/2013/01/meri-pvd-coatings-heading-for-space.html
    [H] Patent US7966909B www.google.co.uk/patents/US7966909
    [J] Head of Surface Engineering, Rolls Royce, corroborating source 5
    [K] International Conference on Fundamentals and Industrial Applications
      of HIPIMS industrial exhibitors lists 2012
        http://extra.shu.ac.uk/hipimsconference/program.php (bottom of page)
      and 2013 http://www.hipimsconference.com/