Center for Tribology, Inc. COMPREHENSIVE MATERIALS TESTING FOR MECHANICAL AND TRIBOLOGICAL PROPERTIES

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1 C ET R Center for Tribology, Inc. COMPREHENSIVE MATERIALS TESTING FOR MECHANICAL AND TRIBOLOGICAL PROPERTIES Micro/Nano Indentation Micro/Nano Scratch Wear Friction Lubrication Environmental Multi-Axis Fatigue Strain/Deformation UMT Series Testers On One Precision Platform with Easily-Interchangeable Modules UNMT-1 UNIVERSAL NANO & MICRO TESTER UMT-2 UNIVERSAL MICRO MATERIALS TESTER UMT-3 UNIVERSAL MACRO MATERIALS TESTER

2 UNIVERSAL NANO+MICRO+MACRO MATERIALS TESTER (UMT) APPLICATIONS HARDWARE Automotive, Aerospace Microelectronics Electric Contacts Metals, Ceramics Bio Materials, Medical MEMS, Optics Flexible & Hard Media Composite Materials Lubricants, Additives Thin Films, Coatings Polymers, Elastomers Paper, Fabric FUNCTIONAL TESTING SCRATCH WEAR adhesion delamination hardness INDENTATION Yyoung s modulus storage modulus hardness ADHESION FATIGUE LUBRICITY pull-up stiction scratch multi-axis tension compression torsion hydrodynamics mixed boundary rotary linear reciprocating abrasive fretting galling seizure static dynamic stick-slip elasticity plasticity creep FRICTION STRAIN ENVIRONMENTAL temperature humidity vacuum gases Lower Specimen X Y Translation Horizontal & Vertical Rotation Fast Oscillations Vacuum Chamber Thermal Control Humidity Control The Universal Nano+Micro+Macro Tester platform comes in three main configurations: UNMT-1 for comprehensive nano and micro mechanical tests of thin films and nano-structured materials, with a load range of 1 N to 10 N, UMT-2 for comprehensive micro- mechanical tests of coatings and materials, with a load range of 1 mn to 200 N, UMT-3 for comprehensive macro- mechanical tests of lubricants, metal and ceramic materials, with a load range of 0.1 N to 1 kn. Data Monitor Recording Real-Time Scope Mode Programmable Filtering WORLD LEADERS IN MATERIALS & TRIBOLOGY TEST INSTRUMENTATION Upper Specimen X Y Z Translation Rotation SOFTWARE Motion Control Programmable Velocities & Positions Forces & Torques Synchronized Motions Data Acquisition 16 Sensor Inputs 16 Bit Resolution 100 khz Data Rate Parameters Monitored X,Y, Z Forces X, Y, Z, Positions X, Y, Z Torques Wear Depth & Rate, Deformations Acoustic Emission Temperature Humidity Electrical Capacitance Electrical Resistance Optical Images, Digital Video Data Presentation Data Analysis Data Statistics Charts Format Conversions

3 T E STS C C ET ET R R SCRATCH-RESISTANCE SCRATCH-ADHESION SCRATCH-HARDNESS SCRATCH-TOUGHNESS Applications Optical coatings Semiconductor layers Flat panel LCD and plazma displays Wear-resistant coatings Corrosion-resistant coatings Decorative coatings and paints Data storage media overcoats Cutting tools coatings Automotive varnishes and finishes Pharma tablets and pills UNIVERSAL MATERIALS TESTERS UNMT-1AND UMT-2 MICRO-SCRATCH MODULE QUANTITATIVE COATING ADHESION, SCRATCH-RESISTANCE AND SCRATCH-HARDNESS Technical Highlights Loading system: uniquely precise active-feedback servo-control for normal force, maintained either constant or increasing (in steps or gradually) Scratch tools: Rockwell and Vickers indenters Diamond stylus, m Tungsten carbide, sapphire, steel balls, mm Steel needles, mm Patented micro-blades, mm Maximum normal load: 200N Normal load minimum resolution: 1 N Multiple sensors: Acoustic emission: high-frequency up to 5.5 MHz Friction coefficient Electrical contact or surface resistance: mohms-mohms Capacitance for depth monitoring Digital optical microscope for micro-imaging: 550X CCD Camera: video and still images Atomic force microscope for nano-imaging: contact and semi/non-contact modes Sample shapes: any, including irregular Sample sizes: from microns up to 150 mm Sample stages: linear or rotary, Multi-scratch: Position resolution < 1 m automatic mode UNMT-1 with optical microscope and AFM Patented micro-blade (left) and holder (right) CENTER FOR TRIBOLOGY, INC.

4 MICRO-SCRATCH APPLICATIONS Scratch-Adhesion Test The technique involves generating a controlled scratch with a scratching tip under a precisely controlled progressive load. At a certain critical load the coating starts to fail. The critical loads are detected precisely with multiple sensors and then are used to quantify the adhesive properties of film-substrate combinations. Z-carriage Normal load Strain-gauge sensor ECR Moving stage Coating sample Micro-blade holder Diamond tip CoF = Fx/Fz Fz Linearly increasing load Fx Substrate Coating Below is an example for a thin DLC coating on a magnetic disk. The critical load of scratching was detected at 4 sec, when ER dropped and AE increased (though friction did not react due to its averaging nature). For about 30 sec ER continued to drop and AE continued to increase. Then at 34 sec the final critical load of coating breakthrough was detected when ER dropped to zero, AE peaked, COF stepped up. ER, kohm Fx, g COF AE, volt Fz, g Scratch-Hardness Test Scratch-hardness test is performed with diamond stylus per ASTM G171-03, under precisely controlled constant load. The scratch hardness: HSp = k* Fz / W 2 Where k- constant; Fz - applied load; W - scratch width. When k is unknown, the scratch hardness can be determined by comparison of the scratch width on the sample and on a reference material. AE sensor is used to monitor the high-frequency signal generated during scratching and indicating the intensity of material fracture. A polished fused quartz (with the hardness of 9.5 GPa) was used as the reference material for the scratch-hardness calculations. Examples of COF and AE data as a function of time for comparison of two materials are plotted below. Reference An example of scratch 3-D nano-imaging and width measurement with integrated AFM is shown below. A digital micro-image of a thick polymer coating tested similarly (load increased from right to left) shows three areas of the test track divided by two critical loads: from deformation (on the right) to microscratching (center) to delamination (on the left) 3-D nano-image of the scratch CETR, INC DELL AVE, CAMPBELL, CA PHONE FAX INFO@CETR.COM

5 C EE T R LEADERS IN TRIBOLOGY TEST INSTRUMENTATION AND SERVICES NANO ANALYSER METROLOGY FOR COMPREHENSIVE NANO-MECHANICAL EVALUATION OF THIN FILMS A NON DESTRUCTIVE TECHNIQUE TO EVALUATE YOUNG S MODULUS OF THIN FILM NANO-HARDNESS NANO-SCRATCHING NANO- IMAGING Technical Highlights Non-destructive measurement of Young s modulus for thin and ultra-thin films. Nano-scratching at ultra-shallow depths. Simultaneous nano-mapping of surfaces for nanotopography and nano-mechanical properties. Nano imaging of specimen for precise nano-positioning on its target area and nano-imaging of shallow nanoscratches. After sample insertion, it takes order of magnitude less time for measurements than conventional nanoindenters. Applications Thin film coatings MEMS, NEMS Semiconductor wafers and devices Data storage media Metals, Ceramics, Polymers Super Hard materials Nanoanalyser Specifications X-Y stage Micro-positioning Max Travel: 75mm Resolution: 0.5µm X-Y stage Nano-positioning Max Travel: 50/100microns Resolution: 10 nm Hardness Measurement Maximum indentor load: 10 g. Range of measured values: GPa Young s Modulus Measurement Range of measured values : GPa Nano Imaging Resolution in XY plane:10 nm Resolution in Z plane: 1 nm Nano Analyser is a Fast and Robust Metrology Tool Destructive indents Indent after plastic deformation Indent within Elastic Limit of material Center for Tribology, Inc Dell Avenue, Campbell, CA 95008, USA Phone: 408/ Fax: 408/ sales@cetr.com Nano Image comparing Young s Modulus measurement results with different techniques

6 C C ET ET R R UNIVERSAL NANO+MICRO MATERIALS TESTER UNMT-1 NANO-INDENTATION MODULE NH-1 Applications Thin films, coatings MEMS, NEMS, Bio-MEMS Semiconductor wafers and devices Data storage media Biomaterials Polymers, Elastomers Metals, Ceramics NANO & MICRO TESTS YOUNG S MODULUS HARDNESS STIFFNESS TENSION COMPRESSION ADHESION FATIGUE CREEP Side optical microscope view of Berkovich tip approaching the surface (includes tip reflection) Nanohead NH-1 and Sample on Rotary Stage Technical Highlights Nano-indentation module includes nano-head NH-1, programable controller NC-1 and vision system with computerized optical microscope NM-1 Nano-indentation module can be easily attached to tester UNMT-1 via fast-exchange fixture or used as a stand-alone instrument Metrology fully corresponds to the ISO14577 standard on instrumented nano-indentation Load and penetration depth are continuously monitored and independently controlled Proprietary contact surface approach, drift and machine compliance compensation algorithms Hands-free electronics and intuitive control software, easily programable indentation cycles Integrated computerized optical microscope with in-situ side and top-down views. Optional AFM for in-line pre/post-test nanoimaging of the indent and indentation area Optional acoustic and thermal enclosure, antivibrational table. CENTER FOR TRIBOLOGY, INC. Script example for multiple loading-unloading cycles Nanohead Specifications Load Maximum Force: 400mN Digital Resolution: 0.1 N Load ranges: ±4mN, ±40mN, ±400mN Displacement Maximum Displacement: 200 µm Digital Resolution: 0.02 nm Displacement ranges: 1µm, 10µm, 100µm, 200µm X and Y stages Z stage Travel: 75 mm x 75 mm 150 mm Digital Resolution: 1 µm 2 µm Rotary stage O Travel: 360 Position Resolution: 0.03 arcsec

7 METROLOGY Nano-head NH-1 and nano-indenter tip are factorycalibrated, the information is conveniently stored. 2 APPLICATIONS Thin metal and ceramic films TiN film on Si wafer: Er= 128GPa and H=16GPa Semiconductor porous films Database of tip area functions Quality control of porous low-k films: sub-surface crack induced excursion Sub-surface air bubble induced inelastic behavior Flexible data storage media AFM image and cross-sections of Berkovich tip The load versus displacement plots are generated automatically. The reduced elastic modulus Er and sample hardness H are calculated according to standard. DLC coating on flexible media: sinking-in behavior, Er = 0.42GPa and H = 0.65GPa. MEMS Devices Stiffness of micro-membrane: Multiple loading-unloading curves on fused quartz 50µN load resulted in 270nm displacement (first segment reflects stiffness of the nanohead) CETR, INC DELL AVE, CAMPBELL, CA PHONE FAX INFO@CETR.COM

8 C C ET ET R R UNIVERSAL NANO+MICRO MATERIALS TESTER UNMT-1 ATOMIC FORCE MICROSCOPE (AFM) MODULE NANO-IMAGING TOPOGRAPHY MAGNETIC PROPERTIES Applications NANO-MEASUREMENTS NANO-ROUGHNESS WEAR/SCRATCH/INDENT NANO-MAPPING LATERAL NANO-FRICTION PULL-UP NANO-ADHESION Nano-imaging in mechanical and tribological testing without sample removal: - comparison of surface topography before/after and periodically during tests - periodic nano-imaging (AFM) and continuous micro-imaging (OM) of wear, scratch, crack, indent development, growth and propagation - lateral and adhesion mapping of test surface before/after and periodically during tests AFM Module Integrated in the UNMT-1 with Linear Stages Force measurements in mechanical and tribological testing without sample removal: - comparison of AFM nano-friction and UMT micro/macro-friction on surfaces - comparison of AFM nano-adhesion and UMT micro/macro-adhesion on surfaces Nano Defectoscopy - auto-positioning on surface defects with known coordinates (X&Y or R& ), easily downloadable from optical or stylus macro-characterization instruments, - rotary or linear sample table with sub-micron positioning resolution - failure analysis and quality control on samples up to 6, optional 8 : - optical displays (LCD, LED, Plazma) - optical disks (DVD, CD, PD) - magnetic disks and head wafers - semicon and MEMS wafers Dishing profile in a 50 micron line polished at 55 ml/min slurry flow Dishing profile in a 50 micron line polished at 20 ml/min slurry flow Post-CMP of semiconductor wafers: two 3-D nano-images of dishing profiles on the copper lines Process artifacts of a laser textured hard magnetic disk with 5-mm texture bumps and 2-mm wide scratches. Technical Highlights Commercial advanced atomic force microscope (AFM) Functions: - atomic-force microscopy - phase imaging - magnetic force microscopy - lateral force mapping - adhesion force mapping - contact and semi/non-contact Scanning ranges: 50X50X3 m 85X85X7 m 100X100X9 m Resolution: 0.1 nm Digital high-resolution, wide field-of-view optical microscope (OM) and a color CCD camera - continuous video - still micro-images - micro-positioning of AFM tip Full mechanical and electrical integration into UNMT CETR, INC DELL AVE, CAMPBELL, CA PHONE FAX WWWW.CETR.COM

9 UNMT-1, UMT-2 AND UMT-3 Technical Highlights MULTIPLE TESTS on nano, micro and macro scales: - static and dynamic friction - ultra-low-speed (0.1 micron/s) stick-slip - adhesive, abrasive and scratching wear - pull-off adhesion/ stiction - scratch-adhesion and delamination - indentation, hardness and elastic modulus - multi-cycle, multi-axis fatigue - strain, elasticity, plasticity and creep - compression, tension and torsion - three-point bending pin-on-disk module with o 1000 C chamber disc-on-disc module block-on-ring module MULTIPLE SENSORS for IN-SITU test monitoring: - ultra-precision force sensors of the proprietary technology and patented design (1 N to 1 kn) - 6-D sensors for simultaneous measurements of 3 forces and 3 torques in all X, Y and Z axes - high-frequency acoustic emission sensors of the proprietary design, ultra-sensitive to tiniest cracks and wear - wear and deformation sensors of micro (0.5 micron) and nano (20 nm) resolution - contact and surface electrical resistance (mohms to MOhms) for detection of film failure or buildup - temperature and humidity sensors - integrated vision system for micro-positioning and digital video of the failure dynamics - integrated AFM for periodic nano-imaging of test surfaces, wear tracks, indents and scratches reciprocation module o with 300 C chamber AFM module Precision SERVO-CONTROL of loads, speeds, and positions for uniquely reproducible data and highly productive tests, e.g., repeatable different loads on different specimen areas for multi-test results from single tests MULTIPLE SYNCHRONIZED linear and rotary motions of upper and lower specimens in all X, Y and Z axes, including oscillations (up to 60 Hz), for sophisticated multi-axis tests, e.g., with spiral, zigzag or butterfly scratch/wear tracks MULTIPLE CHAMBERS with computer controlled o temperature (-25 to 1000 C), humidity (10 to 95% RH), -6 vacuum (up to 10 Torr), gases All motion and sensor modules are easily INTERCHANGEABLE within a few minutes CENTER FOR TRIBOLOGY, INC. ST A NDARD I N DUST R I AL nano-indenter TEST SCHEMATICS (EXAMPLES) Pin/Ball-on-Disk Block/Pin-on-Ring Crossed-Cylinders Bearings Valves Connectors Commutators Contact/Wires Screw-in-Nut Pin-in-Chain Shaft-in-Seal Disc/Plate-on-Disc/Plate Indenter-on-Plate 4-Balls ISO/ASTM/DIN Standards Razor-on-Hair Brush-on-Teeth Orthopedic Joints Semicon Wafers Head-on-Disk Cutting Tools Contact Lenses Optical Media/Lenses

10 UNIVERSAL NANO+MICRO+MACRO MATERIALS TESTER (UMT) Four Types of Drive Modules Lower Linear Fast Reciprocation with Upper Linear Motion Lower Plate: up to 150 mm Lower Cylinder/Wire: 1 µm to 25 mm Reciprocation Frequency: 0.1 to 60 Hz Reciprocation stroke: 50 µm to 25 µm Options: fluid bath, environm. chamber Wear & Fretting Tests Upper Pin/Ball/Block: stationary Multiple Wear Tracks: auto-positioning, distance 0 to 75 mm, resolution 1 µm Cross-Cylinder Tests Upper Cylinder: 0.1 to 25 mm Upper Tensioned Wire/Suture/Fiber: 1µm to 1 mm Narrow Wear Track: stationary upper sample Wide Wear Track: sliding upper sample, to 10 mm/s Multiple Wear Tracks: auto-positioning 0 to 75 mm, resolution 1 µm Engine Tests Upper Piston Ring: stationary Lower Cylinder Liner: reciprocating Lower Rotation (horizontal axis) with Upper Linear or Rotary Motion Lower Ring/Bearing: Rotation: Options: Block-on-Ring Tests Upper Block or Plate: 1 to 150 mm Narrow Wear Track: stationary block/plate Wide Wear Track: sliding block/plate, to 10 mm/s Ball/Pin-on-Ring Tests Upper Ball: 1.5 to 25 mm Upper Pin: 1 to 25 mm, flat, spherical or conical end Single/Multi-Crater Tests Upper Ball or Pin: rotating cw/ccw, speeds 0.1 to 1,000 rpm Positioning on new craters: radial - range 360, resolution 0.5 µm axial - range 75 mm, resolution 1 µm 10 to 80 mm cw/ccw, 0.1 to 5,000 rpm fluid bath, environmental chamber Lower Disc: Rotation: Upper Ball: Upper Pin: Options: Lower Rotation (vertical axis) with Upper Linear or Rotary Motion up to 150 mm (optional 200 mm) cw/ccw at two speed ranges: 0.1 to 5000 rpm or to 50 rpm 1.5 to 25 mm cylinder 1 to 25 mm, flat, spherical or conical end fluid bath, environmental chamber Single-Radius Pin/Ball-on-Disc Tests Upper Pin or Ball: stationary during test, automatic positioning on disc radii 0 to 75 mm, resolution 1 µm Spiral-Wear Pin/Ball-on Disc Tests Upper Pin or Ball: sliding radially on Lower Disc, speeds to 10 mm/s Lower Disc angular speed autoadjusted for constant linear speed Four-Ball Tests Upper Ball: stationary in the center Three Lower Balls: immersed in fluid bath Single/Multi-Crater Tests Upper Pin or Ball: rotating cw/ccw, speeds 0.1 to 1,000 rpm Positioning on new craters: automatic radial positioning, range 75 mm, resolution 1 µm circumferential positioning, range 360, resolution 0.5 µm Disc/Ring-on-Disc Tests Upper Disc or Ring: Stationary or rotating: Lower High-Precision Linear with Upper Linear Motion Lower Plate: up to 150 mm Reciprocation Stroke: 75 mm Positioning Resolution: 1 µm Linear Speed: to 10 mm/s Options: fluid bath, environm. chamber Single/Multiple Indentation Tests Upper Indenter: Rockwell, Vickers, Berkovich Positioning on new indents: automatic, resolution 1 µm Butterfly Wear-Track Tests up to 150 mm cw/ccw, speeds 0.1 to 1,000 rpm Upper Pin: 1 to 25 mm Upper Ball: 1.5 to 25 mm Upper Sliding: synchronous with lower sliding CETR, INC DELL AVE, CAMPBELL, CA PHONE FAX INFO@CETR.COM