Teer Coatings Ltd. A New High Rate Magnetron ---Characteristics & Applications D.G. Teer Teer Coatings Ltd., UK www.teercoatings.co.uk 1 Background N S N Closed magnetic field system Target S S N N S S Magnetron Sample holder N S N • TCL coatings are deposited using patented Close Field Unbalanced Magnetron Sputter Ion Plating (CFUBMSIP) system www.teercoatings.co.uk 2 Background System for coating up to 432 drills (∅ 10 mm) per run www.teercoatings.co.uk 3 New high power density magnetron Target size 380 X 175 mm Magnetic field above the target stronger than for a conventional magnetron Optimised water cooling system Typical rectangular magnetrons manufactured by TCL www.teercoatings.co.uk 4 Experimental configuration Closed magnetic field OES viewport N S S N N S Counterpart magnetron Flat ring jig/ sample holder www.teercoatings.co.uk High power magnetron Vacuum chamber Ti, Al or Cu target 5 Experimental condition • Ar flow: 4 – 70 sccm ⇒ pressure variation 0.075 – 5.2 Pa • “Advanced Energy” MDX-II DC power generators with max output 15 kW • I-V reading from generator panel set in current regulation mode • OES measurements by EP200 Verity Instrument monochromator in manual mode, FWHM > 1 nm. • During deposition sample holder revolved at 4 rpm • Deposition substrate to target distance 150 mm www.teercoatings.co.uk 6 I-V characteristics (Al, Cu and Ti) 550 Gas - Ar p = 0.24 Pa 500 V (V) 450 400 350 CM-Cu HPM-Cu 300 CM-Al HPM-Al 250 CM-Ti HMP-Ti 200 0 www.teercoatings.co.uk 15 30 45 I (A) 60 75 90 7 I-V characteristics (Ti target) 500 Target material - Ti Gas - Ar+N2 450 p (Pa) 0.30 V (V) 400 0.17 350 300 250 200 0 10 20 30 40 50 I (A) www.teercoatings.co.uk 8 I-V characteristics (Al target) 550 Target material - Al Gas - Ar 500 p (Pa) V (V) 450 0.09 0.17 400 0.30 350 0.7 0.30 300 250 200 0 10 20 30 40 50 I (A) www.teercoatings.co.uk 9 Ion current to the -50V biased substrate 4.5 4 p=0.30 Pa 3.5 Ijig (A) 3 2.5 HPM-Ti 2 HPM-Al 1.5 CM-Al 1 0.5 0 0 2 4 6 8 10 12 14 16 Pmag (kW) www.teercoatings.co.uk 10 Deposition of TiN coating Deposition conditions • 2 opposing unbalanced HPMs •12.5 kW at each target • Sample rotation at 4 rpm • OEM controlled introduction of N2 • 50 min deposition time www.teercoatings.co.uk Coating characteristics: • Total thickness 3.36 μm • Deposition rate 4 μm/h ⇒ 4 times higher than from CMs • Hardness – 33 GPa • Good scratch result 11 Deposition of Cu coating Deposition conditions: • Single unbalanced HPM without closed field Coating characteristics: • Total thickness 8.0 μm • Deposition rate ≈ 30 μm/h • 28 kW at the Cu target • Sample rotation at 4 rpm • Deposition time 16 min www.teercoatings.co.uk 12 Graphit-iCTM coatings Graphit-iCTM (a-C) Sputtered a-C doped with Cr Dense amorphous structure Very low friction (<0.1 in dry sliding) Very low specific wear rate (<6x10-17 m3.N-1.m-1) High load bearing capacity (>2.5GPa) Electrically conducting Current commercial applications Automotive components, machinery & Tools, decorative & electrical applications Development of Graphit-iC coatings Increase deposition rate (e.g. fuel cell application) www.teercoatings.co.uk 13 Deposition Equipment Two magnetrons of the new design used in place of conventional magnetrons Cr C C Cr (Target size 380 x 175 mm) www.teercoatings.co.uk 14 Graphit-iCTM coating procedure A three step process is ued for the deposition of Graphit-iCTM • ion cleaning • deposition of a thin metallic chromium layer • deposition of the C / Cr layer 1.8 μm 0.2 μm www.teercoatings.co.uk 15 Magnetron Characteristics Current-voltage curve for conventional and high power magnetrons 700 650 Voltage / V 600 550 500 450 HPM1 400 HPM2 Conventional design 350 300 0 1 2 3 4 5 6 7 8 9 10 Current / A www.teercoatings.co.uk 16 Magnetron Characteristics Current-Power graph for target 380mm x 175mm 8 Power / kW 7 6 5 4 HPM1 3 HPM2 2 Conventional 1 0 0 2 4 6 8 10 12 14 Current/ A www.teercoatings.co.uk 17 Ion currents at substrate holder Magnetron Design C Target */ A Cr Target **/A Bias /V Ion current recorded /A Conventional 3.5 0.25 60 0.46 HPM 9.0 0.40 60 1.25 HPM 12.0 0.54 60 1.65 * applied to each of two carbon targets * *applied to one of two chromium targets ¾ Ion current is significantly increased by the higher powers www.teercoatings.co.uk 18 Deposition Rates C target power / kW Graphit-iC Layer thickness / µm Graphit-iC Graphit-iC/ / hrs µm/hr Conventional 2.2 - 2.4 1.8 - 2.0 4 0.45 - 0.5 HPM 5.0 - 5.2 1.8 - 1.9 2 0.9 – 0.95 HPM 6.7 - 7.1 2.4/2.5 2 1.2 /1.35 Magnetron Design Deposition time Deposition rate Summary • Power input increased by up to 3 times. • Deposition rates increased by 2 to 2.7 times depending on the chosen target power www.teercoatings.co.uk 19 Coating Properties 3.5A (2.2 kW) 9A (5.1 kW) 12A (6.9 kW) Surface Quality – Optical microscope Adhesion – Indentations from 150kgf Rockwell Test VDI 3198/1991 Hardness – Fischerscope H100 (testing load 50mN) 1769 kgmm-2 www.teercoatings.co.uk 1519 – 1729 kgmm-2 1554 kgmm-2 20 Tribological properties - Wear 3.5A (2.2 kW) 9A (5.1 kW) 12A (6.9 kW) Specific Wear rates in m3/Nm ( 80N POD test in air against WC/Co ) 2.1 x10 -17 Pin-on-disc wear tracks 2.8 x10 -17 2.9 x10 -17 Taper sections through wear tracks (produced by ball crater technique) Summary : Specific wear rate comparable at low and high deposition rates. www.teercoatings.co.uk 21 HPM at Different Powers Graphit-iC coatings produced at different target currents Magnetron Design C Target */ A Cr Target **/A Specific Wear Rate 80N POD / m3N-1m-1 Stable Friction Coefficient Conventional 3.5 0.25 2.1 x10-17 0.07 HPM 2.5 0.18 2.7 x10-17 0.07 HPM 5.0 0.25 3.3 x10-17 0.08 HPM 9.0 0.40 2.8 x10-17 0.08 HPM 12.0 0.54 2.9 x 10-17 0.09 * applied to each of two carbon targets ** applied to one of two chromium targets ¾ The new magnetron can be operated at low powers if required for temperature sensitive materials – e.g. bearing steels. www.teercoatings.co.uk 22 TEM results on Graphit-iC coating Cr interface layer Cr/C superlattice layers ~3 nm www.teercoatings.co.uk 23 TEM results on Graphit-iC coating 102 (006) a-C phase with (006) basal plane crystalline cluster perpendicular to the surface www.teercoatings.co.uk 24 Conclusions (1) ¾ High power density magnetron with 665 cm2 industrial size sputter target has been designed and successfully tested ¾ Stable operation of HPM with Cu & Ti targets up to 30 kW (80 W/cm2) and with Al target up to 15 kW (40 W/cm2) was demonstrated ¾ Current-voltage characteristics exhibit large increase in current with little or no increase in voltage, indicating high efficiency of plasma confinement above the target ¾ Deposition experiments demonstrate substantial increase of deposition rate, proving possibility of cost effective processes based on HPMs. www.teercoatings.co.uk 25 Conclusions (2) ¾ Target power was increased by up to 3 times ¾ Low voltage operation deposition rates were increased by up to 2.7 times ¾ No detrimental effects were observed on the coating hardness or coating tribological properties at fast deposition rates ¾ No significant increase in surface defects was observed ¾ The high power magnetron design can also be used successfully at lower powers for temperature sensitive substrates www.teercoatings.co.uk 26 Acknowledgements Thanks to: Dr. A. Grouppa who did most of the development work on the High Rate Magnetron and to Sue Field for her work on the Graphit-iC coatings www.teercoatings.co.uk 27 Teer Coatings Ltd. www.teercoatings.co.uk West Stone House, Berry Hill Ind. Estate, Droitwich, Worcestershire, WR9 9AS. U.K. www.teercoatings.co.uk 28
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