measuring nanotechnology an introduction to...

MEASURING NANOTECHNOLOGY

MICROMATERIALS

An Introduction to Nanomechanical testing –

Bringing it into the real world

NanoindentationNanoscratch/nanowear

High temperatureImpact/Fatigue testing

Dr Krish Narain, Micro Materials Ltd., Wrexham29th July 2004

Bringing nanomechanicalmeasurements into the real-world


MICROMATERIALS

Outline• Introduction to Micro Materials, nanomechanical

testing and the NanoTest system• Nanoindentation• Nanoscratch testing• High temperature testing• Nano fatigue and impact testing• Conclusions• Sources of further information



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 and manufacture 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


MICROMATERIALS

Micro Materials is based in Wrexham

Where is Wrexham?It is in Wales, to the west of

England.What is Wales famous for?Sheep, coal-mines (now all

shut), leeks and rugby - and the NanoTest


MICROMATERIALS

Micro Materials Technology:• Nanoindentation • Nano-scratch and nano-wear testing (Nanotribology)

• Nano-impact testing*• Contact fatigue testing*• Dynamic hardness testing*

• High temperature nano-scale testing*

* = Micro Materials techniques - patents pending

Nanomechanical testing = nanoscale testing of the mechanical and tribological properties of materials

Micro Materials –Test techniques


MICROMATERIALS

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


MICROMATERIALS

Source: British Library on-line database. Keyword search on “nanoindentation”.

As devices become smaller, and coatings become thinner…..

mechanical and tribological properties are becoming more important…

hence nanoindentation has become more important…

The rise of nanotechnology


MICROMATERIALS 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


MICROMATERIALS Viscoelastic Effects during Indentation

0

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ep d

ispl

acem

ent (

nm)

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Aluminum

Polyester

Epoxy

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(mN

)Depth (nm)

Hold time = 100 sec

Data: Courtesy Dr Raman Singh, SUNY Stonybrook

Creep effects as a function ofloading rate

Creep at constant load


MICROMATERIALS

Variation in loading curve and creep with loading rate

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disp

lace

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t (nm

)

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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…


MICROMATERIALS

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



MICROMATERIALS

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


MICROMATERIALS

Indenter characteristics• Low compliance• True depth sensing• Low thermal drift (without need to

use rings)• High stability• High sensitivity to indent<10nm

reguarly• No interferometer for calibrations• Scheduling ability - for AUTOrun• Ease of Use• Good vibration isolation• Capture raw data• Scratch in stiff direction of indenter

• Expandable and upgradeable• Uniform loading on all sides of indenter

– don’t want to balance springs or be subject to piezo errors

• Frame, load, depth and diamond area calibrations.

• Uniform frame compliance vs load• Load resolution <50nN• Max depth 200 micron (with high load

option• Option to auto load cal between

indents • Full analysis software• Break-out points as standard


MICROMATERIALS

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)


MICROMATERIALS

Stainless steel plasma-carburized at 450 deg C

Elastic modulusHardness

• Good correlation between H and E• Large areas with slightly different properties• Original microstructure of steel responsible

Elastic recovery

NanoTest software -Mapping Mechanical Properties


MICROMATERIALS

nickel plating

Al pad

passivation layerSi wafer

Quantitative measurement of themechanical properties of thin films

Aim: determine the hardness and modulus of top layer in IC bond pad without substrate influence

Technique Applied ForceSPM nN-µNNanoTest 10 µN-500 mNMicroTest 100 mN - 20 NHardness N-kN

Comparison of load ranges

Indentation: Case study

In collaboration with Wolfson School of Mechanical and Manufacturing Engineering, Loughborough Uni, UK


MICROMATERIALS

Depth-profiling with the load-partial unload technique

1 quick-and-easy experiment at a single point:20-cycle load-partial-unloadDepth controlled 50-1000 nm

Comes as standard with basic Indentation module

• produces rapid and quantified variation in hardness and modulus with depth

constanthardness

decreasinghardness

coating coating + substrate

Hardness

Elastic modulus

Modulus: extrapolation to zero-depth

1/10 film thickness


MICROMATERIALS

Aim: to determine the mechanical properties of thin plasma polymers on aluminium

Plasma polymerisation forms polymer networks where the cross-link density depends on deposition conditions

Can we use nanoindentation to optimise the deposition parameters?

Collaborative research between MML and Corrosion and Protection Centre, University of Manchester Institute of Science and Technology (UMIST), UK.


MICROMATERIALS

Low power

Higher power

The mechanical properties of thin, soft coatings can only be tested by nano-scale materials testing (nanoindentation, Nanotribology, nano-impact)

Plasma-polymerised Coatings


MICROMATERIALS

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…


MICROMATERIALSMEASURING NANOTECHNOLOGY

MICROMATERIALS

• Deposited at 100 WHardness = 0.7 GPaModulus = 10 GPa

• Deposited at 25 WHardness = 0.4 GPaModulus = 15 GPa

Nanoindentation revealed clear differences in mechanical properties with coating deposition conditions…

(compare - polyester with 50 % crystallinity has H ~ 0.28 GPa, Modulus ~ 3.5 GPa – so plasma-polymers are harder and stiffer than highly crystalline thermoplastics)

• nanoindentation provides quantitative hardness and elastic modulus values and shows how coating properties can be optimised

“Nanoindentation testing of plasma-polymerised hexane films”B.D. Beake (MML), S. Zheng (MML), Morgan Alexander (UMIST)

Journal of Materials Science vol. 37 (2002) in press.

Plasma-polymerised Coatings


MICROMATERIALS

0

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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


MICROMATERIALS

Coil

Ceramic

Capacitor plates Indenter

MicroTest pendulum


MICROMATERIALS

MT 10 micron indentations into Al


MICROMATERIALS

MicroTest 20 micron indentations into AlNote consistent values of reduced modulus at 10 and 20 µιχρο


MICROMATERIALS

MicroTest 6.4N indentations into WReduced modulus lit value = 320 GPaIs equivalent to lit value of Young’s modulus of 410Despite poor sample quality (see loading curves) still v. accurate


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


MICROMATERIALS

• Two main types of scanning experiment providing different information….

• Single ramped load scratches– at a critical load (Lc) failure occurs – this can be a measure of adhesion strength

• Constant load multi-pass scratches- resistance to sliding/abrasive wear

Scanning module: Nanoscratch testing


MICROMATERIALS

Ramped load scratch test1. Low load scan2. Ramped scratch3. Final low load scan

• On-load deformation• Off-load deformation• Critical load• Friction forces• Acoustic Emission• Optical Microscopy

Nanoscratch/Nanotribology

Key advantages of the NanoTest for nano-scratch testing…

• Scratching occurs in high stiffness direction for pivot• Direct calibration of tangential (frictional) forces possible


MICROMATERIALS

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


MICROMATERIALS Micro-scratch testing

Substrate temperature effects on the microhardness and adhesion of diamond-like thin films, E Martinez, MC Polo, E Pascual and J Esteve, Diamond and Related Materials 8 (1999) 563-566.

Critical load is a function of 1) deposition conditions2) coating thickness…


MICROMATERIALS

Load ramp used in multi-pass scratch test…

5 x 400 mN scratches then final topography scan at 0.2 mN

Nanowear testing

Nanowear testing of ceramic composites

Scans 1-5

Scan 6


MICROMATERIALS

• Clear differences in nano-/micro- scale wear resistance between different ceramic composites• Correlates to nanoindentation hardness

Zirconia/Mullite Alumina/Zirconia Zirconia/Alumina

~1 µm wear depth ~2 µm wear depth ~3 µm wear depth

Nanowear testing

Nanowear testing of ceramic composites


MICROMATERIALS

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.


MICROMATERIALS

Nanoindentation – mechanical properties (hardness, modulus, creep)Nanoscratch – tribological properties (resistance to abrasive/sliding wear)

Conventional nanoscale testing techniques provide part of the solution…

But…

• All material properties are temperature-dependent• Materials often fail by fatigue not overload


MICROMATERIALS

Nanomechanical testing at high temperatures

• Nanoindentation and nano-scratch testing to 750oC• Thermal drift minimal

Horizontal loading configuration has key advantages for drift-free high temperature testing – heat flows upwards away from electronics


MICROMATERIALS

Reduced modulus solgel coating on Si as function of temperature

66.5

77.5

88.5

99.510

0 50 100 150

depth [nm]

Er [G

Pa]

100CRT

Nanoindentation of solgel coating on Si

4.2 µm solgel coating - spin coated onto Si and cured at 350 deg. C20 µm spheroconical indenter Modulus drops with temperature

Data courtesy of Philips Research, Netherlands


MICROMATERIALS Nanoindentation of Si(111)

At room temperature Si(111) undergoes phase changes…

NanoindentationParameters:-

Loading rate = 1.67 mN/sHold period at maximum load = 5sUnloading rate = 0.56 mN/s

• What happens at higher temperatures?

“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


MICROMATERIALS

High temperature nanoindentation of Si(111): slow unloading

100 deg. C 300 deg. C

200 deg. C29 deg. C


MICROMATERIALS Thermal barrier coatings

• Heterogeneous columnar coating – complex indentation response even at RT

•Probability distribution functions can be used to determine results affected by porosity and natural scatter

• Sapphire indenter mounted in Mo stub was used for 750 degree indentations

• Clear fracturing during loading

• Minimal drift at 90% unloadingJ.R. Nicholls, S.A. Impey, R.G. Wellman, A.G. Dyer (all Cranfield University) and J.F. Smith (Micro Materials), ICMCTF 2003

Nanoindentation of EB-PVD TBC (Zirconia/8wt% yttria) 25, 500 and 750 degrees C

Fracturing during loading

3 curves at 750 deg. C

• Aerospace – critical that the high temperature mechanical properties of TBCs are well understood at the nanoscale


MICROMATERIALS

Reduced Modulus Room Temp. 157.12 ± 12.78 GPa500 C 123.24 ± 14.74 GPa750 C 102.16 ± 15.05 GPa

Youngs Modulus [ GPa ]

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200

-2.0 -1.5 -1.0 -0.5 0.0 0.5 1.0 1.5 2.0

Standard Normal Distribution

Youn

gs M

odul

us [

GPa

]

R.T. (polished)500 C (calculated)750 C (polished)Linear (R.T. (polished))Linear (500 C (calculated))Linear (750 C (polished))

Hardness [ GPa ]

0.0

1.0

2.0

3.0

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5.0

6.0

7.0

8.0

9.0

-2.0 -1.5 -1.0 -0.5 0.0 0.5 1.0 1.5 2.0

Standard Normal Distribution

Hard

ness

[ G

Pa ]

R.T. (polished)500 C (calculated)750 C (polished)

Hardness Room Temp. 5.84 ± 1.04 GPa500 C 4.15 ± 0.74 GPa750 C 2.89 ± 0.49 GPa

• Hardness and modulus of TBCs decrease with temperature…

Thermal barrier coatings


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


MICROMATERIALS

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


MICROMATERIALS

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


MICROMATERIALS

Coating B Coating C

Effect of microstructure on impact performance

small needle-like crystalsaid impact resistance

larger rounded crystalsdo not help impact resistance


MICROMATERIALS

Collaboration with Ito Tecnologia Cerámica, Castellon

Does not fail in impact test Fails quickly in impact test


MICROMATERIALS

Impact testing of ceramic coatings:comparison fracture toughness from SEM

• Hardness and Young’s Modulus did not vary• Scratch testing frustrated by high surface roughness

• Correlation with fracture toughness data from SEM…

• Impact resistant samples had high fracture toughness

• Time-to-failure • Change in Probe Depth

…measures of resistance to brittle fracture

“Micro-impact testing: a new technique for investigating fracture toughness” BD Beake (MML), Maria Jesus Ibanez Garcia (ITC Spain) and JF Smith (MML), Thin Solid Films 398-399 (2001) 438-443.

Low depth change = high fracture toughness

Collaboration with Ito Tecnologia Cerámica, Castellon


MICROMATERIALS Time-to-failure

Impact results on thin hard multilayer coatings on glass

• Repetitive impacts at the same position• Sharp probe to induce fracture quickly• Monitor depth vs. time – failures are very clear• Long time to failure = more tough, durable

Short time-to-failure Long time-to-failure


MICROMATERIALS

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


MICROMATERIALS

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


MICROMATERIALS

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?


MICROMATERIALS

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


MICROMATERIALS

Carbon coating on tool steel

• depth vs. time impact plot for multilayered carbon coating at 1mN• long time to failure

Coating failure

Multiple coating failures

DLC coating on tool steel

• depth vs. time impact plot for multilayered DLC coating at 1mN• short time-to-failure

Nano-impact testing reveals fatigue differences on coatings of the same hardness…

Impact – cube corner indenter

• Carbon coating much tougher than DLC


MICROMATERIALS

Mapping variations in high-strain rate deformation

50 200

350

500

650

800

950 50

200Impact depth

(nm)

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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position (microns)

Toughness map for ABS 25wt% rubber

360-400320-360280-320240-280200-240

Applications in Milling Prediction


MICROMATERIALS

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


MICROMATERIALS

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


MICROMATERIALS

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


MICROMATERIALS

Fatigue and Fracture Wear of ta-C films

Procedure developed for analysing fracture behaviour

• Sort initial time to failure in individual tests into ascending order• Plot time to failure vs. probability of the sample failing in that time• Use time for failure probability of 0.5 to rank impact resistance

Fracture resistance of 80 nm ta-C films

00.10.20.30.40.50.60.70.80.9

1

0 50 100 150 200 250 300

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Prob

abili

ty o

f fra

ctur

e Probability of fracturewithin 300 s = 0.9

Probability offracture = 0.5at 75 s

A key advantage ofnano-scaleimpact is thepossibility ofrepeat testing atdifferent locations


MICROMATERIALS

1 mN impact load

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Impact behaviour of coatings on M42 tool steel

5 mN impact load

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Red = 1Blue = 2Green = 3

coating1 – poorcoating 2 – goodCoating 3– good at low load


MICROMATERIALS

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.



MICROMATERIALS Conclusions

• New materials testing techniques – impact/fatigue testing and high temperature nanoindentation testing - have been developed to extend the capability of nanoindentation instruments

• Important since coatings are subjected to fatigue and extremes of temperature in service

• Development of these techniques is a notable advance enabling testing under contact conditions that more closely simulate those in service for the first time

• Test results can therefore be used with greater confidence to optimise the mechanical properties of coatings and surface treatments for specific applications

Bringing nanomechanical measurements into the real-world


MICROMATERIALS Acknowledgements

Further information

• Dr Jim Smith (Micro Materials)• Dr Stephen Goodes (Micro Materials)• Rob Parkinson (NEWI, UK)• Prof John Nicholls and co-workers (Cranfield Uni, UK)• Dr Jinjun Lu and co-workers (LSL, Lanzhou, China)• Dr Nathalie Renevier (Teer (now at UCLAN), UK)• Dr Rego and co-workers (MMU, UK)• Dr Daniel Lau (NTU, Singapore)• Philips Research (Eindhoven, Netherlands)

High temperature testingTCS Associate Rob Parkinson NEWI/Micro [email protected]

Nano-impact testingDr Nigel Jennett – Project Leader on NPL Project MPP2.2 – [email protected]


MICROMATERIALS

www.www.micromaterialsmicromaterials.co..co.ukuk• references• customer profiles• application notes

[email protected]

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