gl an introduction to nanomechanical...
TRANSCRIPT
MEASURING NANOTECHNOLOGY
MICROMATERIALS
An Introduction to Nanomechanical testing
NanoindentationNanoscratch/nanowear
On bio-Materials and other samples
Dr Krish Narain, Micro Materials Ltd., Wrexham
Bringing nanomechanicalmeasurements into the real-world
MEASURING NANOTECHNOLOGY
MICROMATERIALS
Why do we need nanoindentation?
• Coatings are getting more complex• Mechanical properties are critical• If we can understand them then we can
engineer better materials• Yield, cost and performance benefits
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• The NanoTest investigates properties on coatings from 5nm to 200 microns
• Provides hardness and toughness data of many types
• Automated running for multiple analysis• Looks at materials under working
conditions• Single, multiple layer or bulk properties
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Key advantages for biomaterials testing
• The NanoTest system is based around a pendulum (see next slides for more details) which gives these key advantages for testing biomaterials…
• Nanoindentation testing with ultra-low thermal drift (typically 0.005 nm/s or less)
• Nanoscratch testing without bending springs• Nanoscale impact/fatigue testing (no other
instrument can do this)
Bringing nanomechanicalmeasurements into the real-world
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MICROMATERIALS
Founded 1988, based in Wales• Application labs in UK, USA, Germany, Japan• Worldwide support network: LOT Oriel in Europe...
Aim: to become the world leader in the development andmanufacture of nanomechanical testing equipment
Pioneering and progressive approach:-• First commercial nano-impact tester for measuringtoughness and fatigue resistance
• First commercial high temperature nanomechanical testing stage
Micro Materials –Innovation track record
Bringing nanomechanical measurements into the real-world
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To use the NanoTest system..
1) Nanoindentation module to obtain accurate hardness (H) and reduced modulus (Er) values for the coating
2) Scanning module to obtain critical load in scratch test
3) Nano-impact module to assess fracture resistance and durability under dynamic loading
4) High temperature stage to assess coating performance at elevated temperatures (to 750 degrees C)
NanoTest nanomechanical test capability
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Optimised performanceof thin film/coating system
Road-map for development of advanced materials
Mechanical propertiesHardnessStiffnessFracture toughnessLoad support
Tribological propertiesFrictionAdhesionResistance to•Abrasive Wear•Sliding Wear•Brittle fracture•Fatigue wear•Dynamic Loading•Corrosion
Design-in reliability
…at the nanoscaleDurable product= Satisfied customer!
NanoindentationNano-scratchNano-impact
High temp testing
Lab tests at development stage
Test under industrially relevant conditions
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Nanoindentation principle
loading
unloading
• force, displacement and time are recorded throughout indentation of sample by a diamond probe
Scanning = transverse sample movement during loadingImpact = sample oscillation at constant load
Beyond nanoindentation…
• No other technique provides quantitative information about both the elastic and plasticproperties of thin films and small volumes
Indentation curve
coatingcoating
substratesubstrate
MEASURING NANOTECHNOLOGY
MICROMATERIALS Viscoelastic Effects during Indentation
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ep d
ispl
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nm)
Hold time (s)
Steel
Aluminum
Polyester
Epoxy
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Depth (nm)
Hold time = 100 sec
Data: Courtesy Dr Raman Singh, SUNY Stonybrook
Creep effects as a function ofloading rate
Creep at constant load
MEASURING NANOTECHNOLOGY
MICROMATERIALS ISO standards – ISO 15477
4 mandatory user calibrations are needed:• Load• Depth• Diamond area function• Frame compliance
For example without DAF – you can measure Martens hardness – but this is only applicable to Micro Hardness measurements according to ISO standards
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The NanoTest pendulum Advantages of the pendulum include…• large samples possible• calibrated contact load• high temperature stage• sample oscillation (impact)• options such as pin-on-disk wear testing and 2D levelling stage• symmetrical indents• scratching inhigh stiffnessdirection
Bringing nanomechanicalmeasurements into the real-world
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a flexiblenanomechanicalproperty testing centre...
2 loading headsNano - 10 µN - 500 mNMicro - 0.1 N - 20 N
3 modulesIndentationScanningImpact
10 options includingHigh temp testingContinuous compliancePin-on-disk wearMicroscopes/AFM3D imaging
NanoTest platform system
Microscope
Transfer stage (indenter/microscope)
MT head
NT head
Stage Assembly+Z
+Y
+X
Repositioning to 0.5 µm
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NanoTest options…
• High Temperature Stage• Automatic 2D levelling stage• High Load Head (20 N)• Micro-scale Pin-on-disk• Continuous Compliance• Humidity Control• Spherical Indentation• Powder Adhesion• Acoustic Emission• High Resolution Microscope• Zoom Microscope• In-situ AFM• Piezo stage Imaging• Open access to signals
NanoTest Options
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How homogeneous is mycoating?An example of nanoindentation as a QA tool
• rapid, automatic schedulingof arrays of indentations - 10,000 pointsper single run - or 100 scratches
Indentation: mapping (1)
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• NanoTest high resolution microscope used to exactly place indents• Osteonal bone is stiffer than interstitial bone
Nanoindentation into osteonal bone…
Nanoindentation of bone
MEASURING NANOTECHNOLOGY
MICROMATERIALS Bone: Nanoindentation creep
Bone is viscoelastic, so to obtain accurate H and E values, the tests need:-
• Slow loading• Long hold period at max. load for creep (180s)• Good thermal drift (as creep recovery can be important)
• Only the NanoTest system has additional software for investigating this creep deformation – which provides additional characterisation information on rate and extent of creep
Creep of osteonalbone fittedto a log function
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Use of Nanoindentation to assess new candidate surface modification technologies for biomedical applications
Data from European project
“Ion Beam Surface Modification of Polymers for Improved Friction and Wear Properties”
Micro Materials Ltd (UK)University of Birmingham (UK)Technical University of Clausthal (Germany))SC Plasmaterm (Romania)Hungarian Academy of Sciences (Hungary)
Wear resistance predicted from H/E ratio correlates to Pin-on-Disk wear testsand Nano-tribology results
Follow-up project – dynamic loading and fatigue
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Variation in loading curve and creep with loading rate
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0.0001 0.001 0.01 0.1
loading rate (mN/s)
disp
lace
men
t (nm
)
after
before
creep
1. After 30s hold period at maximum load depth is the same in very slow and fast tests
2. Only an instrument with negligible thermal drift could perform these tests, with loading rates varying by x300
Loading history on polymer = load then hold for 30 s
No thermal drift correction necessary…
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Nanoindentation of polymer-clay nanocomposites…
• to produce advanced materialswith improved mechanical properties by PEO intercalation between clay layers
• to accurately characterise their nanomechanical properties so synthetic and fabrication methods can be optimised
Ben Beake (MML), Shuaijin Chen, J Barry Hull and Fengge Gao(Polymer Engineering Centre, Nottingham Trent)
2 key aims…
1
2
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Improving polymer performance…
Nanoindentation of PEO/Clay Nanocomposites
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Ben Beake*, Shuaijin Chen J. Barry Hull and Fengge Gao J Nanosci. Nanotech. 2002 vol 2, 73-79.
• Hardness and stiffness of PEO film are dramatically improved by addition of high clay loading
Indentation on melt-synthesised PEO
G-105 clay/solution-synthesised PEO
Pure PEO
PEO/ 20 % clayLow hardness -influenced by creep?
Very high hardness atHigh clay loadings
Nanoindentation of PEO/Clay Nanocomposites
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020406080
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% G-105 Clay
A B
The variation with clay is striking
when creep data are fitted to d = A ln(Bt + 1)
A determines extent of creepB determines rate of creep
More clay – slows creep processExplains small decrease in hardness at low loading
Influence of creep on hardness…
Good fit tologarithmic creep equation
Nanoindentation of PEO/Clay Nanocomposites
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Depth profiling with the load-partial-unload technique
100 W
25 W
100 W
25 W
20 cycle load-partial-unload experiment – takes 30 mins
Plasma-polymers deposited at 100 W and 25 W power…
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Nanomechanical properties of burnt polyurethane foams in resin
Modulus (GPa) Hardness (MPa) optical image
Nano-mechanical properties of heterogeneous, multi-phase soft samples can be quantitatively mapped
Mapping hardness and modulus
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IPP Repeat Indentations
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(mN
)
Ultra-low load (10 µN) testing of soft samples
• For slow loading excellent thermal stability is necessary
Ultra-low load nanoindentation
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Nanoindentation – mechanical properties (hardness, modulus, creep)
Nanoscratch – tribological properties (resistance to abrasive/sliding wear)
The standard nanoscale mechanical/tribologicaltest techniques are very useful…
But…
• All material properties are temperature-dependent
Room Temperature or real temperature
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NanoTest hot stage …
Dampingplate
Heaterelement
Thermocouple
Power supply +temperature controller
Insulation
Thermal shield
For clarity, separate diamond heater not shown
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At room temperature Si(111) undergoes phase changes…
Nanoindentation Parameters:-
Loading rate = 1.67 mN/sHold period at maximum load = 5sUnloading rate = 0.56 mN/s
“Pop-out” during unloading
Phase changes:-Si-I diamond-type to Si-II β-tin on loading…to Si-XII and Si-III on slow unloading
At slow unloading rate the pop-out only in room temp data
29 deg. C200 deg. C
• Different unloading slopes as test temperatures increases
• Elastic modulus reduced by 27% at 200 degrees C
• No observable “pop-out” at slow unloading rates
• Implications for microelectronics processing/applications
Nanoindentation of Si(111)
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Reduced modulus solgel coating on Si as function of temperature
66.5
77.5
88.5
99.510
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depth [nm]
Er [G
Pa] 100C
RT
20 µm spheroconical indenterRoom temp modulus agrees well with Berkovich dataModulus drops with temperature
Data courtesy Philips Research, Netherlands
Nanoindentation of solgel coatings on Si
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AJ Muir Wood, V Gergely and TW Clyne, Gordon Laboratory, Dept of Materials Science and Technology, University of Cambridge. Proc SPIE 2004 (in press)
The NiTi shows shape memory behaviour above the transition temperature
Nanoindentation testing of NiTi at high temperature
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High temperature friction
Double forcetransducer
Thermalinsulation
Diamond holder
Testprobe
Thermalshield
Fused quartz rod
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Friction coefficient at RT and 200ºC
Influence of Temperature on Friction Coefficient
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Fric
tion
coef
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Roomtemp.
1 mm dia. stainless steel ball + glass substrate
Scan speed 4 µµµµm/s
Normal load 4 mN
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Stiction at 400ºC
Stiction at 400C and a Load of 4 mN
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Stiction at 400C and a Load of 0.4 mN
02468
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1 mm dia. stainless steel ball + glass substrate
Scan speed 4 µµµµm/s
Normal load 4 mN
1 mm dia. stainless steel ball + glass substrate
Scan speed 4 µµµµm/s
Normal load 0.4 mN
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Influence of temperature on adhesion
Adhesion of Stainless Steel to Glass
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1 mm dia. stainless steel ball + glass substrate
MEASURING NANOTECHNOLOGY
MICROMATERIALS Nano-and Micro-scratch test principle
loading
1. Force, displacement, friction, acoustic emission and time are recorded throughout the scratching of a test sample by a diamond probe
2. Can test much thinner coatings and more local scratch behaviour than conventional scratch test
coating substrate
Sample motion during loading makes nano-scratch tests possible…
transverse samplemotion with XYZ stage
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50 µm
100
µm
Precise determination of Critical load (Lc) for film failure • Friction force data• Displacement data• Microscopy
Carbon films on Si as protective overcoats for hard disk, MEMS
Track end
Friction
Depth
Nanoscratching of thin hard ta-C films on Si for MEMS
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MICROMATERIALS
As hydroxyapatite isthe main CalciumPhosphate in bone,it is being considered as a biocompatible coating for artificial joint replacements
NanoTest system has been used to evaluate the abrasive wear resistance of HA coating…
Nanoscratch testing
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MICROMATERIALS
Multi-pass sub-critical load scratch testing
dplast
dtotalExperimental parameters:25 µm Rockwell probescratch load:- ramped to 1 mNtopography load 0.1 mNscan speed 0.5 µm/s Nano-scratching wear of PET film
Repeat scratches over the same wear track reveal gradual wear of oriented polyester [PET] film
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2, 4, 6
1, 3, 5, 7
Nanotribology
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2 different PET samples -clear differences in nano-scratching wearwith processing history...
Biaxially drawn PET film - 50% crystalline
dplast
dtotal
dplast
dtotal
• extent of ploughing
• differences inelastic recovery (dp/dt)
Uniaxially drawn PET film ~ 30% crystalline
Evaluate slidingwear resistance ofdifferent coatingformulations
Nanotribology
BD Beake (MML) and GJ Leggett (UMIST), Polymer 2002, 43, 319-327.
MEASURING NANOTECHNOLOGY
MICROMATERIALS Evaluation of Dental Composites
Dental composite materials used to be evaluated by standard macroscale test methods – but results were inconsistent
So the NanoTest is being used to rapidly evaluate the abrasion resistance of new improved composite materials
NanoTest wear depth data for repeat scratches on common composites…
The new composites in this study were shown to have betterabrasion resistance than conventional materials
Scr
atch
dep
th
(mic
rons
)
MEASURING NANOTECHNOLOGY
MICROMATERIALS Nano-impact testing
Materials can fail by fatigue not overload so optimisation based on nanoindentation/scratch may be insufficient
for applications where materials are exposed in service and/or in processing to fatigue wear or erosive wear (impact wear)
Dynamic nanomechanical tests (nano-impact and contact fatigue) have been developed by Micro Materials to address this problem
The need for dynamic testing
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Nano-impact testing - simulating fatigue wear and failure
Impact
Sample oscillation
2 different methods…
• High frequency oscillation• High cycle fatigue
• Accurately controlled impacts• Known energy to failure• Wear mechanisms
Pendulum impulse impact
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Impact at high load = Contact fatigue testing
• A and C fracture easily but B and D do not fracture within 500s• Can we correlate with fracture toughness data? • Can we correlate with microstructure?
1N load repetitive contact testing reveals clear differences….
Collaboration with Ito Tecnologia Cerámica, Castellon, Spain
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Unimplanted SiO2 1 x 1016 N cm-2
implanted SiO2
Damage regimes in the impact test:1 = before impact2 = plastic deformation3 = slow crack growth (fatigue)4 = abrupt failure and material removal5 = further slow crack growth
Fracture and fatigue wear by Nano-impact testing
MEMS: nanostructured Si and SiO2
• Fatigue resistance from time-to-failure
• Ion-implantationimproves toughness
BD Beake (MML), J Lu, Q Xue, and T Xu, (all Lanzhou Institute of Chemical Physics) Proc FMC8 2003
1 impact every 4 s in these tests
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MICROMATERIALS Nano-impact mapping of biomaterials
• Initial results suggest the nano-impact test can be used to identify osteopaenia (2-5 times greater risk of osteoporosis in later life)
Grids of impacts to determine differences in toughness/ductility…
Collaboration in progress with Universities of Limerick and Lancaster
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position (microns)
position (microns)
Variation in fatigue properties across finger nail of 42 yr old woman
2500-3000
2000-2500
1500-2000
1000-1500
500-1000
0-500
• No other nanoindentation system has the capability to do nano-impactso no other system can investigate toughness and fatigue at the nanoscale
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Damage mechanism in the impact test: before impact - plastic deformation - slow crack growth (fatigue) - abrupt failure and material removal - further slow crack growth
Fatigue and Fracture Wear of ta-C films
80 nmon Si
60 nmon Si
• time-to-first-failure to rank impact resistance• some plastic deformation of the substrate does occur (depth at failure)
5 nm
on Si
80 nmon Si
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Diamond-like-carbon (DLC) has high hardness and low friction so it is being considered for many applications
But its fatigue properties have not been fully tested –this is particularly important asIt is prone to poor adhesionIt has been considered as an inert coating for biomedical devices
The NanoTest is being used to investigate the toughness and durability of DLC coatings to fatigue wear with the nano-impact facility…
DLC: is it tough enough for your application?
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Impact failure of 550 nmDLC film on Silicon
Nano-impact shows how deposition conditionsinfluence coating performance• Time-to-failure• Failure mechanism
Coating debonding - adhesion failureAbrupt depth change at failure > film thickness
Coating fracture – cohesive failureDepth change at failure less than film thickness
CVD CoatingDepositionRF Power
BD Beake et al, Diamond and Related Materials, 11, 1606, 2002
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Nano-impact can be used to assess the toughness and adhesion of DLC coatings under industrially relevant conditions
DLC suffers from brittlenessDLC suffers from high stressDLC suffers from poor adhesionDLC suffers from poor resistance to fatigue
Nano-impact is a very quick and easy way to optimise DLC performance
Next slide shows typical brittle fracture and debonding of DLC after repetitive contacts (impact)
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Nano-impact can assess DLC performance
1. Under a range of contact conditions (I.e. from light to severe loading) – important since many tests are too gentle
2. Quickly
3. Provides clear-cut time-to-failure data
4. Microscopy confirms failure mode…(see next slide)
5. Can test on actual component
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Hydrogenated DLC (a-C:H) Hydrogen-free DLC (a-C)
50 µµµµm 50 µµµµmRing-cracking
Nano-impact results on commercial DLC
Delamination occurs for the DLC on the left – it is not suitable for severe contact conditions
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Mapping variations in high-strain rate deformation
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position (microns)
position (microns)
Mapping of fatigue properties across crab shell
5000-60004000-50003000-40002000-3000
• Nano-scale ductility of crab shell varies across the shell
• Finer “mesh sizes” can be used to investigate this behaviour at much smaller scale
• At this highly localised scale the ductility varies with distribution of micron/sub-micron sized rubber particles in the ABS matrix
Grids of impacts to determine differences in toughness/ductility…
Collaboration in progress with University of Maryland
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Toughness map for ABS 25wt% rubber
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Applications in Milling Prediction
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Testing the viscoelastic properties of thin films and small volumes requires the ability to access a wide range of strain rates
The NanoTest system has far greater strain rate choice than other systems because
1. Ultra-slow loading, long creep tests etc, are possible due to excellent thermal stability (~0.001-0.01 nm/s)
2. Very high strain rates accessible – use nano-impact
Indentation: viscoelastic materials
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Repetitive impact tests on brittle and ductile materials
• Focus on ability to absorb energy• More plastic deformation = more ductile• Less plastic deformation = less ductile
• Little plastic deformation before failure• Clear fracture event(s)• Time-to-failure characterises impact resistance
Less ductile
More ductile
Impact behaviour:brittle and ductile materials
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Nano-impact of Rubber-modified ABS Polymer
Incorporation of 25 % rubber leads to greater depth change on repetitive impact at the same position
1 impact every 7 s; 5 mN impact force; spherical test probe
Nano-impact – ductile materials
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5 repeat impact tests at each composition
Very reproducible behaviour - error bars are smaller than symbols
Geometric considerations used to convert depth to volume
• Rubber incorporation improves ability to absorb energy on impact by deforming plastically rather than fracturing (improved ductility)
Nano-impact - a new method of ductility testing
Variation in impact-induced plastic deformation with rubber loading
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The technique has considerable potential in evaluating the local fatigue behaviour and ductility of thin polymer films that are not capable of being tested by conventional methods that were designed for bulk samples
Ben Beake, Steve Goodes, Jim Smith and Fengge Gao, J Mater Res (2004) 237-247.
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New innovations
• Liquid cell• In two beta sites
• NanofrettingAbout to got Beta-site
status
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Conclusions
1. Nanoindentation is fast becoming an essential tool in the optimisation of the mechanical and tribological properties of thin coated systems and advanced materials, for applications where hardness and stiffness are important.
2. The pendulum arrangement has key advantages for reliable scratchtesting. Scratching occurs in high stiffness direction for pivot and direct calibration of tangential (frictional) forces are possible.
3. Nano-scratch and nano-wear tests can accurately reveal differences in coating adhesion and wear resistance of coatings and bulk materials. This information can be used to aid materials processing and coating design.
4. Together, the combination of nanoindentation, nanoscratch and nano-impact provides much information on the plastic, elastic, adhesive, fatigue wear and fracture properties of biomaterials
Bringing nanomechanicalmeasurements into the real-world
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www.micromaterials.co.ukwww.micromaterials.co.uk• references• customer profiles• application notes
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