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Development of Ultrananocrystalline Diamond (UNCD) Coatings

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Development of Ultrananocrystalline Diamond (UNCD) Coatings Development of Ultrananocrystalline Diamond (UNCD) Coatings Presented by Jeffrey Elam Argonne National Laboratory Materials, Sensors & Automation, and Glass Project Review June 21-24, 2004 Arlington, Virginia A U.S. Department of Energy Office of Science Laboratory Operated by The University of Chicago Office of Science U.S. Department of Energy Project Summary • Goal: - Use UNCD to achieve significant energy savings in IOF industries - First application – SiC multipurpose mechanical pump seals • Challenge: - Develop technology to take UNCD from laboratory to market application - Need to mass produce UNCD coated parts • Benefits: - Improved wear resistance and corrosion resistance of UNCD coated parts - 20% energy savings of 236 trillion Btu by 2020 in pump applications primarily due to reduced friction losses • FY05 Activities: - Commission and optimize 11-inch IPLAS system (up from 6-inch system) - Demonstrate UNCD coating of multiple seals simultaneously - Demonstrate benefits of UNCD coatings on gas seals - Verify tribological benefits of UNCD coated seals - Perform long-term pump tests 2 Pioneering Science and Technology Project Participants – Laboratory-led project • Argonne National Laboratory - Energy Systems: - Jeff Elam, John Hryn (Project POC), Joe Libera - Energy Technology: - Ali Erdemir, Andriy Kovalchenko - Materials Science: - Orlando Auciello, John Carlisle, Dieter Gruen, Mike Pellin, Alex Zinovev • Industry Partners: - Advanced Diamond Technologies, Inc. (ADT) - Neil Kane (Industry POC) - John Crane, Inc. - IPLAS Innovative Plasma Systems - Morgan Advanced Ceramics - Northwestern University - University of Illinois at Chicago 3 Pioneering Science and Technology Barriers Pathways Critical Metrics – – 1) Uniform nucleation and Understand plasma Develop seeding protocol growth of UNCD deposition and surface to produce uniform 1) smooth films seeding requirements, UNCD films 2) good adhesion UNCD characterization (COMPLETED) and testing 2) Scale – up UNCD Commission 11-inch Multiple seals coated with deposition process plasma system UNCD simultaneously 3) Limited seal testing Use industrial facilities and Perform successful pilot facilities expand lab capabilities test (data indicate energy savings) 4) Commercialization of Launch company (ADT) Sign toll-processing UNCD technology agreement 4 Pioneering Science and Technology Ultrananocrystalline Diamond (UNCD) Properties TEM 0.5 nm • Hardness 97 GPa - • Elastic Modulus - 970 GPa 3-5 nm • Fracture Strength - 5 GPa AFM • Grain Size - 2 - 5 nm • RMS Roughness - 0.5 - 1 µ-inch • Friction Coefficient - 0.03 200 nm 5 Pioneering Science and Technology UNCD for Multipurpose Mechanical Pump Seals UNCD Coating 6 Pioneering Science and Technology • UNCD to reduce friction and eliminate wear Technical Barrier #1: Uniform nucleation and growth of UNCD • Seeding to achieve smooth UNCD films • Seeding to achieve excellent adhesion of UNCD to SiC Seal 7 Pioneering Science and Technology UNCD – Example of Poor Seeding Sample: Unseeded CVD SiC • Low nucleation density – discontinuous coating 8 Pioneering Science and Technology UNCD – Example of Excellent Seeding Sample: Mechanically Seeded α-SiC • High nucleation density - dense, continuous, smooth film 9 Pioneering Science and Technology Simultaneous UNCD and Carbon Nanofiber (CNF) Growth SEM and TEM Following UNCD Treatment EDAX Elemental Analysis al gn i ax S d Fe Kα E 0.4% 0 1000 2000 3000 4000 5000 6000 7000 8000 Iron Energy (eV) SEM, TEM shows CNF with iron particle catalyst • Trace Fe Contamination Catalyzes CNF Growth 10 Pioneering Science and Technology • Developed Screening Process for Iron UNCD Coating of Smooth 2” OD α-SiC Seals 5 BefJCo9r4 e Coating 0 -5 -10 -15 ) s e -20 ch in -25 o Ra=0.6±0.1 µinch SEM of Uncoated Seal icr -30 M 5 ( t JC94 h After UNCD 0 ig e H -5 -10 -15 -20 -25 Ra=0.7±0.1 µinch -30 11 Pioneering Science and Technology • UNCD is smooth, no roughness change from UNCD coating UNCD Coating of Rough 1” OD α-SiC Seals Before Coating 20 10 ) s e 0 ch in -10 SEM of Uncoated Seal o icr -20 M ( -30 t h ig -40 e H -50 Ra=8±1 µinch -60 0 0.02 0.04 0.06 0.08 0.1 0.12 Distance (Inches) 12 Pioneering Science and Technology • Rough initial surface for 1” seals Roughness Measurements of Rough 1” OD Seals Following UNCD Coating 12 Before Coating ) h c After UNCD n i 10 o r c i M ( s 8 oughnes 6 age R er v A 4 48 49 50 51 52 53 54 Seal Number 13 Pioneering Science and Technology • No roughness change from UNCD Coatings Adhesion Measurements Using Fracture Analysis 3 1 2 Conformal UNCD coating over Fracture of UNCD-SiC interface observed after Seal face and beveled edge diamond saw cutting (1). However, fracture also observed along SiC grains (2) and UNCD film (3) 14 Pioneering Science and Technology • Strong adhesion of UNCD Coating to SiC Surface UNCD Coating of 5” Gas Seals • Improved coating technology required for • Segment of 5” 5” gas seals seal was coated • Coating must preserve in existing small- precisely engineered area plasma taper system Outside Edge Inside Edge UNCD SiC 10 microns 10 microns 15 Pioneering Science and Technology • UNCD Maintains Critical Tolerance Across Face of 5” Gas Seal Technical Barrier #2: Scale – up UNCD deposition process IPLAS 11” Microwave Plasma CVD System • First unit of its kind in the world • Will enable batch-coating of multiple 2” seals • Will enable coating of intact 5” seals 16 Pioneering Science and Technology • Work is underway to install and commission this system Technical Barrier #3: Limited seal testing facilities • Building Test Pump Loop at Argonne for Measuring Seal Friction and Wear • Installed Surface Profiler at Argonne • Friction and Wear Analysis at John Crane Testing Facilities 17 Pioneering Science and Technology Hot Water Test of UNCD-Coated Seals at John Crane • 2” OD Seal • 100 Hours • Very aggressive test of materials properties • Mimics harsh conditions in chemical process pump • 100 hour test simulates 2 years of extreme use 18 Pioneering Science and Technology Hot Water Test of UNCD-Coated Seals Uncoated UNCD-Coated graphite SiC graphite SiC blistering wear debris No wear! h 0 pt e 0 D Wear 0 Distance (inch) 0.3 0 0.3 19 Pioneering Science and Technology • Failure of uncoated seal, no detectable wear for UNCD-coated seal Friction Measurements of UNCD Coated 2” SiC Seal Low Initial Roughness Uncoated Uncoated SiC Seal UNCD coated SiC seal que r o T UNCD Face Load • Significantly Reduced Friction for Smooth Seal Surface 20 Pioneering Science and Technology Friction Measurements of UNCD Coated 1” SiC Seal High Initial Roughness Low RPM Uncoated t n e i c i UNCD f f Uncoated on Coe JC48 i t c i r F 0 102 0 304 0 50 Time (Minutes) • Marginally Reduced Friction for Rough Seal Surface 21 Pioneering Science and Technology Current Study: Effect of Roughness on UNCD Friction Technical Barrier #4: Commercialization of UNCD technology Advanced Diamond Technologies • Advanced Diamond Technologies - Argonne-initiated start-up company - Exclusive license in UNCD application - Company officially launched in 2003 - Business plan established - Toll processor for seal manufacturers - Agreements in principle reached with partners 22 Pioneering Science and Technology Future Work Leading to Commercialization • FY05 - Understand effect of initial substrate roughness on UNCD friction - Commission and optimize 11-inch IPLAS system (up from 6-inch system) - Demonstrate UNCD coating of multiple 2” seals simultaneously - Demonstrate benefits of UNCD coatings on gas seals - Verify tribological benefits of UNCD coated seals - Perform long-term pump tests • FY06-07 - Pilot tests (field tests): 2" seals, 5" seals - Automation of UNCD deposition process • FY07 - Commercialization (sign toll-processing agreements) - Final report 23 Pioneering Science and Technology .
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