Embed Size (px)
Citation preview
FEMTO TOOLS
HIGH-RESOLUTION
NANOINDENTATION
FT-I04FEMTO-INDENTER
Product Brochure
FT-I04 FEMTO-INDENTER
The FT-I04 Femto-Indenter is a high-resolution nanomechanical testing system capable of accurately quantifying the mechanical and tribological properties of materials at the micro- and nanoscale.As the world’s first MEMS-based nanoindenter, the FT-I04 uses the pat-ented FemtoTools Micro-Electro-Mechanical System (MEMS) technology. Leveraging over two decades of innovations, this nanoindenter features unmatched resolution, repeatability and dynamic stability.The FT-I04 Femto-Indenter is optimized for the mechanical testing of metals, ceramics, thin films and coatings, as well as more compliant microstructures such as metamaterials. Furthermore, the FT-I04 is modular and can extend its capabilities to accommodate the versatile requirements of various research fields.Typical applications include the quantification of hardness and elastic modulus as a function of indentation depth using the integrated continu-ous stiffness measurement (CSM) mode, as well as the high-resolution mapping of mechanical properties. Furthermore, optional modules en-able scratch and wear testing, high-resolution scanning probe micros-copy (SPM) imaging and high temperature testing (coming soon).With unmatched noise floors down to 500 pN in force (guaranteed real world values) and 50 pm in displacement (guaranteed real world values) and comparatively large ranges of 200 mN and 20 µm, the Femto-Indent-er enables the comprehensive study of mechanical behavior of materials with an unprecedented accuracy and repeatability.
APPLICATION OVERVIEW
NANOINDENTATION SCRATCH TESTING PROPERTY MAPPING
WEAR TESTING SPM IMAGING
1 FT-I04 Femto-indenter
4
1
2
3
Measurement head (interchangeable) consisting of:
• Long-range positioner for the fast and accurate approach of the nanoindentation tip to the sample surface over a range of 40 mm with a position sensing resolution of 1 nm
• Piezo-scanner for the high-resolution, position-controlled nanomechanical testing of the material properties of the sample. It features a range of 20 µm and a guaranteed noise floor smaller than 50 pm
• FT-S Micro-Force Sensing Probe (interchangeable) with various tip geometry and materials options, enabling the measurement of forces up to 200 mN (FT-S200’000) and down to 500 pN (guaranteed noise floor of the FT-S200)
2-axis sample stage for the accurate positioning of the sample under either the microscope or the nanoindenter head. The stage provides a travel range of 130 x 130 mm and features a closed-loop position control with a noise floor of 1 nm
Interchangeable sample tray for up to 6 samples and 1 reference fused silica specimen
High-stiffness granite measurement frame
High-resolution, top-down optical microscope with coaxial illumination for the observation of the sample and the easy selection of the indentation locations
Enclosure for acoustic shielding and environmental control
SYSTEM COMPONENTS
4
3
2
OVERVIEW
1
5
6
56
2Overview
High-resolution nanoindentation with an unmatched repeatability to detect even smallest variation in hardness and modulus
Displacement sensing range of 20 µm with a guaranteed noise floor of less than 50 pm (in fine mode) and up to 40 mm with a 1 nm noise floor (in coarse mode), covering 9 orders of magnitude
Stiffest nanoindenter on the market with the highest dynamic range featuring load cells with a resonance frequency up to 50 kHz and a data acquisition rate of 96 kHz
Interchangeable force sensing probes with various tip geometries and materials enabling force-sensing from 500 pN to 200 mN in both tension and compression, covering 9 or-ders of magnitude
Intrinsic position-controlled measurements, enabling the direct recording and quantifica-tion of fast plasticity and fracture events (optionally, force-controlled measurements are possible as well)
FEATURES
SPM imaging of surfaces, scratches and residual indents enabling the quantification of surface damage and deformation such as pile-up or sink-in (coming soon)
Integrated procedures for fast and accurate calibration of the nanoindenter tip geometry (area function calibration) from ultra-shallow depths to conventional nanoindentations
FT-I04 FEMTO-INDENTER
High-resolution nano-scratch, nano-wear and nanofriction measurement using the op-tional Scratch Testing Module in combination with the 2-axis Microforce Sensing Probe
Extensive data analysis tools for the plotting of data, its analysis using customizable fits and functions, and the extraction and visualization of material properties
3 FT-I04 Femto-indenter
FEATURES MEMS-BASED MICROFORCE-SENSING PROBE
MEMS-BASED NANOINDENTATIONThe FT-I04 Femto-Indenter is a high-resolution nanoindenter based on Micro-Electro-Mechanical System (MEMS) technology.
While typical nanoindentation systems feature force sensing technologies based on precision-machined and as-sembled components, FemtoTools is using semiconductor fabrication technology to monolithically machine the entire force sensor out of single crystalline silicon wafers. This ap-proach enables the fabrication of much smaller structures, making the de-sign of load cells with high sensitivity, resolution and repeatability possible, overcoming the limitations of more traditional technologies. Furthermore, the small size of the MEMS sensing ele-ment results in a mass that is orders of magnitude lower than that of load cells using conventional technologies. In combination with the high stiffness of silicon flexures, the FemtoTools FT-S Microforce Sensing Probes provide a high natural frequency (up to 50 kHz) and the related ability to measure fast events or to conduct fatigue or cyclic tests at higher frequencies.
1-Axis Microforce Sensing Probe
2-Axis Microforce Sensing Probe
1-Axis Microforce Sensing Probe with integrated tip heater
4MEMS-Based Nanoindentation
APPLICATION EXAMPLES
To study the variations of mechanical properties in different specimens, over heterogeneous microstructures or at interfaces, the Femto-Indenter features a sample stage combining a range of 130 x 130 mm with a 1 nm position noise floor that enables precise and repeatable targeting of specific locations. It also enables the automated mapping of mechani-cal properties over large areas with high-resolution. The included Femto-Tools Software Suite provides exten-sive data analysis and visualization tools, with profiles, statistics and color maps of all measured and de-rived properties.
PROPERTY MAPPING
NANOINDENTATIONThe Femto-Indenter enables the meas-urement of hardness, modulus, creep, relaxation and fracture toughness for a wide range of materials, from bulk metals and ceramics to hydrogels, thin films, hard coatings. This is done by in-strumented indentation of a sharp tip with a known or calibrated shape into a material, while recording the force required to penetrate to a given depth.The Femto-Indenter features standard indentation (ISO 14577) and automated procedures for quick tip shape calibra-tion. The integrated continuous stiff-ness measurement (CSM) mode ena-bles the measurement of mechanical properties as a function of the inden-tation depth. It benefits from a depth sensing noise floor of 50 pm. As an example for the outstanding data qual-ity and stability, the results from 100 indents into quartz glass are shown on the right. (The full data set without data selection is shown.) Featuring intrinsic position control, the Femto-Indenter enables the quan-tification of fast stress drops, tran-sients and high speed events with a quality that is not possible with force-controlled systems.
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
00 300 600 900 1200Contact depth hc (nm)
25
100
Redu
ced
Mod
ulus
(GPa
)
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 300 600 900 1200Contact depth hc (nm)
10
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)2.5
-2.5
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
Hard
ness
(GPa
)
Forc
e (m
N)
0
40
80
120
160
200
Displacement (nm)0 400 800 1200
300 µm
300
µm
300 µm
300
µm
300 µm
300
µm
300 µm
300
µm
0
100
200
300
400
500
600
700
800
01
00
00
20
00
03
00
00
40
00
05
00
00
60
00
07
00
00
80
00
09
00
00
10
00
00
11
00
00
12
00
00
13
00
00
14
00
00
15
00
00
16
00
00
17
00
00
18
00
00
19
00
00
20
00
00
21
00
00
22
00
00
23
00
00
24
00
00
25
00
00
26
00
00
27
00
00
28
00
00
29
00
00
30
00
00
Co
un
t
Reduced Modulus (MPa)
0
50
100
150
200
250
300
350
0
500
1000
1500
2000
2500
3000
3500
4000
4500
5000
5500
6000
6500
7000
7500
8000
8500
9000
9500
1000
0
1050
0
1100
0
1150
0
1200
0
Coun
t
Hardness (MPa)
15 200 400 600 800
300
100
00 3 6 9 12
Hardness (GPa)
200
Coun
t
15 200 400 600 800
600
200
00 100 200
Reduced Modulus (GPa)
400
Coun
t
300
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
00 300 600 900 1200Contact depth hc (nm)
25
100
Redu
ced
Mod
ulus
(GPa
)
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 300 600 900 1200Contact depth hc (nm)
10
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
Hard
ness
(GPa
)
Forc
e (m
N)
0
40
80
120
160
200
Displacement (nm)0 400 800 1200
15 200 400 600 800Re
duce
d M
odul
us (G
Pa)
150
125
70
50
00 300 600 900 1200Contact depth hc (nm)
25
100
Redu
ced
Mod
ulus
(GPa
)15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 300 600 900 1200Contact depth hc (nm)
10
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5Ha
rdne
ss (G
Pa)
Forc
e (m
N)
0
40
80
120
160
200
Displacement (nm)0 400 800 1200
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
00 300 600 900 1200Contact depth hc (nm)
25
100
Redu
ced
Mod
ulus
(GPa
)
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 300 600 900 1200Contact depth hc (nm)
10
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
Hard
ness
(GPa
)
Forc
e (m
N)
0
40
80
120
160
200
Displacement (nm)0 400 800 1200
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
00 300 600 900 1200Contact depth hc (nm)
25
100
Redu
ced
Mod
ulus
(GPa
)
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 300 600 900 1200Contact depth hc (nm)
10
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
15 200 400 600 800
5
0
-50 300 600 900 1200Contact depth hc (nm)
Rela
tive
Erro
r (%
)
2.5
-2.5
Hard
ness
(GPa
)
Forc
e (m
N)
0
40
80
120
160
200
Displacement (nm)0 400 800 1200
0
100
200
300
400
500
600
700
800
01
00
00
20
00
03
00
00
40
00
05
00
00
60
00
07
00
00
80
00
09
00
00
10
00
00
11
00
00
12
00
00
13
00
00
14
00
00
15
00
00
16
00
00
17
00
00
18
00
00
19
00
00
20
00
00
21
00
00
22
00
00
23
00
00
24
00
00
25
00
00
26
00
00
27
00
00
28
00
00
29
00
00
30
00
00
Co
un
t
Reduced Modulus (MPa)
0
50
100
150
200
250
300
350
0
500
1000
1500
2000
2500
3000
3500
4000
4500
5000
5500
6000
6500
7000
7500
8000
8500
9000
9500
1000
0
1050
0
1100
0
1150
0
1200
0
Coun
t
Hardness (MPa)
15 200 400 600 800
300
100
00 3 6 9 12
Hardness (GPa)
200
Coun
t
15 200 400 600 800
600
200
00 100 200
Reduced Modulus (GPa)
400
Coun
t
300
5 FT-I04 Femto-indenter
HIGH-SENSITIVITY PROPERTY MAPPING
300 µm
900
µm
300 µm
900
µm
Young’s Modulus Hardness
300 µm
900
µm
300 µm
900
µm15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
300
275
225
200
150175 200 225 250
Contact depth hc (nm)
175
250
Redu
ced
Mod
ulus
(GPa
)
3%
CSM Measurement Data EBSD Map
1
2
21
The most important application of na-noindentation is the measurement and the mapping of properties, such as the hardness and the elastic modulus. Therefore, the most important fea-tures of a nanoindenter are its ability to detect small changes in these prop-erties as well as the spacial resolu-tion at which these properties can be measured.
The FT-I04 Femto-Indenter features two key advantages related to its MEMS-based core technology: high re-peatability and ultra-low noise floors in both force and displacement sensing. As illustrated by the data of hardness and modulus measurements on fused silica (left page), the Femto-Indenter showcases an unprecedented repeat-ability. As a direct consequence, this precision enables to detect ultra-small variations in hardness and modulus values.
To demonstrate this capability of the Femto-Indenter, results from CSM nanoindentation measurements on a single phase alloy (austenitic Nickel-based alloy 690) are presented here. The Femto-Indenter enables to meas-ure not only the hardness and modulus of fine particles from soft dirt residues (H=500 MPa) to hard carbide precipi-tates at grain boundaries (H=15 GPa). More remarkably, it can measure small variations in modulus (3%) corre-sponding to changes in crystal orienta-tion. This can be qualitatively compared to the EBSD map (taken from a differ-ent location on the same sample).
6Application Examples
APPLICATION EXAMPLES
SCRATCH TESTING
SHALLOW INDENTATION
0 10 50Contact depth hc (nm)
20 30 4015
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
0
25
100
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 10 50
Contact depth hc (nm)
10
15
10
0
-10Rela
tive
Erro
r (%
)
5
-5
15 200 400 600 800
10
0
-10Rela
tive
Erro
r (%
)
5
-5
Hard
ness
(GPa
)
Forc
e (m
N)0
4
8
12
20
28
Displacement (nm)0 6 10 12
20 30 40
0 10 50Contact depth hc (nm)
20 30 40 0 10 50Contact depth hc (nm)
20 30 40
16
24
842
15 200 400 600 8000 5 10 15 20Position (µm)
0
-200
-100
-400
Prof
ile (n
m)
-300
15 200 400 600 8000 5 10 15 20Position (µm)
4
40
0
Norm
al
Forc
e (m
N)
2
Late
ral
Forc
e (m
N)
2
The Femto-Indenter can be upgraded with a Scratch Testing Module to en-able nano-scratch and nano-wear testing, as well as SPM imaging. The di-amond tip of a 2-Axis Microforce Sens-ing Probe is pushed across the sample surface while applying a ramping or constant normal load at a given speed. Scratch testing yields quantitative in-sights into tribological properties and failure mechanisms at the nanoscale, including thin film adhesion, friction coefficient and scratch or wear resist-ance of materials. Furthermore, high-resolution SPM imaging can be used for topography imaging before and after scratch, wear or nanoindenta-tion testing. It provides direct visuali-zation of pre-test surface roughness and post-test surface deformation or damage.
The Femto-Indenter enables a large va-riety of tests with a force range of 200 mN and a displacement range of 20 µm. The patented FemtoTools MEMS-based force sensors provide sub-nanonew-ton noise floor, which is combined with sub-nanometer noise floor of the fine positioning stage. The Femto-Indenter is therefore the ultimate nanoindenter for repeatable, high-resolution in-dentations at low loads and shallow depths. It enables the quantitative characterization of properties at the nanoscale, with applications in thin films, nanocomposites and nanostruc-tures. Moreover, intrinsic position con-trol enables to characterize load dis-continuities linked to dislocation events using nanoindentation at low loads. Typically, the indention follows a Hertz-ian curve at low loads until the nuclea-tion of dislocations and their interac-tions with point defects trigger fast stress drops. The direct quantification of stress drop amplitudes enables to measure activation volumes and ener-gies relevant to nanoscale plastic de-formation mechanisms.
15 200 400 600 8000 5 10 15 20Position (µm)
0
-200
-100
-400
Prof
ile (n
m)
-300
15 200 400 600 8000 5 10 15 20Position (µm)
4
40
0
Norm
al
Forc
e (m
N)
2
Late
ral
Forc
e (m
N)2
15 200 400 600 8000 5 10 15 20Position (µm)
0
-200
-100
-400
Prof
ile (n
m)
-300
15 200 400 600 8000 5 10 15 20Position (µm)
4
40
0
Norm
al
Forc
e (m
N)
2
Late
ral
Forc
e (m
N)
2
20 µm
20 µ
m0 10 50
Contact depth hc (nm)20 30 4015
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
0
25
100
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 10 50
Contact depth hc (nm)
10
15
10
0
-10Rela
tive
Erro
r (%
)
5
-5
15 200 400 600 800
10
0
-10Rela
tive
Erro
r (%
)
5
-5Ha
rdne
ss (G
Pa)
Forc
e (m
N)
0
4
8
12
20
28
Displacement (nm)0 6 10 12
20 30 40
0 10 50Contact depth hc (nm)
20 30 40 0 10 50Contact depth hc (nm)
20 30 40
16
24
842
0 10 50Contact depth hc (nm)
20 30 4015
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
0
25
100
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 10 50
Contact depth hc (nm)
10
15
10
0
-10Rela
tive
Erro
r (%
)
5
-5
15 200 400 600 800
10
0
-10Rela
tive
Erro
r (%
)
5
-5
Hard
ness
(GPa
)
Forc
e (m
N)
0
4
8
12
20
28
Displacement (nm)0 6 10 12
20 30 40
0 10 50Contact depth hc (nm)
20 30 40 0 10 50Contact depth hc (nm)
20 30 40
16
24
842
0 10 50Contact depth hc (nm)
20 30 4015
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
0
25
100
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 10 50
Contact depth hc (nm)
10
15
10
0
-10Rela
tive
Erro
r (%
)
5
-5
15 200 400 600 800
10
0
-10Rela
tive
Erro
r (%
)
5
-5
Hard
ness
(GPa
)
Forc
e (m
N)
0
4
8
12
20
28
Displacement (nm)0 6 10 12
20 30 40
0 10 50Contact depth hc (nm)
20 30 40 0 10 50Contact depth hc (nm)
20 30 40
16
24
842
0 10 50Contact depth hc (nm)
20 30 4015
Redu
ced
Mod
ulus
(GPa
)
150
125
70
50
0
25
100
15 200 400 600 800
Redu
ced
Mod
ulus
(GPa
)
20
15
5
00 10 50
Contact depth hc (nm)
10
15
10
0
-10Rela
tive
Erro
r (%
)
5
-5
15 200 400 600 800
10
0
-10Rela
tive
Erro
r (%
)
5
-5
Hard
ness
(GPa
)
Forc
e (m
N)
0
4
8
12
20
28
Displacement (nm)0 6 10 12
20 30 40
0 10 50Contact depth hc (nm)
20 30 40 0 10 50Contact depth hc (nm)
20 30 40
16
24
842
7 FT-I04 Femto-indenter
8Application Examples
ACCESSORIES
The FemtoTools FT-S Microforce Sens-ing Probes are sensors capable of measuring forces from sub-nanone-wtons to 200 millinewtons along the sensor’s probe axis. Both compression and tension forces can be measured. Single SI-traceable pre-calibration for each probe in combination with an out-standing long-term stability guaran-tees significantly higher measurement accuracy than other force sensing systems in this force range. Special-ized versions are also available, includ-ing 2-Axis Microforce Sensing Probes or Tip Heating.The FT-S Microforce Sensing Probes are available with a wide variety of tip materials and geometries including diamond Berkovich, cube corner, flat punch, wedge, conical and more.
FT-S MICROFORCE SENSING PROBES
FT-S200 +/- 200 µN 0.5 nN
FT-S20’000 +/- 20’000 µN 50 nN
FT-S200’000 +/- 200’000 µN 500 nN
FT-S2’000 +/- 2’000 µN 5 nN
Model Range Noise Floor(10Hz)
SCRATCH TESTING MODULE HIGH TEMPERATURE MODULE
FT-S20’000-2Axis +/- 20’000 µN 100 nN
+/- 20’000 µN 100 nN
The Scratch Testing Module (coming soon) consists of an exchangeable sample stage with an integrated piezoscan-ner. This enables the in-plane movement of the sample while simultaneously applying a normal force. Combined with the FemtoTools 2-Axis Microforce Sensing Probe, this mod-ule enables nanoindentation, nano-scratch and nano-wear testing, as well as SPM imaging of surface roughness, high-aspect ratio features and residual scratches or indents.
The High Temperature Module (coming soon) enables heat-ing of specimens. In combination with the FemtoTools Tip Heating Sensors, it makes isotherm nanomechanical testing of samples at various temperatures possible. It enables not only the measurement of materials properties evolution as a function of temperature, but also the quantitative study of thermally-induced changes in plastic deformation and frac-ture mechanisms at the nanoscale.
9 FT-I04 Femto-indenter
MEASUREMENT HEAD
Force
Sampling frequency 96 kHz
Noise floor (10 Hz) down to 500 pN
Digital resolution down to 0.5 pN
Range up to 200 mN
SAMPLE STAGE
TECHNICAL
SPECIFICATIONS
Measurement principle position controlled
Position
Fine noise floor (10 Hz) 50 pm
Coarse noise floor (10 Hz) 1 nm
Fine range 20 µm
Coarse range 40 mm
Sampling frequency 96 kHz
Digital resolution 0.05 pm
Range 130 x 130 mm
Noise floor (10 Hz) 1 nm
MICROSCOPE
Camera 5 megapixel CMOS sensor
Objective lens options 5x, 10x, 20x, 50x, 100x
Coaxial illumination LED, Adjustable
Focus motorized
10Accessories & Technical Specifications
FemtoTools AGFurtbachstrasse 48107 Buchs / ZHSwitzerland
T +41 44 844 44 25F +41 44 844 44 27
www.femtotools.com
FEMTO TOOLS
