ULTRA NANOINDENTATION TESTER (UNHT) · 2012-11-21 · //// UNHT : TECHNICAL FEATURES V.01.2009 - 9 / 30 - //// Applications The Ultra Nanoindentation Tester is an instrument module

CSM Technical Features //// ULTRA NANOINDENTATION TESTER (UNHT)

//// UNHT : TECHNICAL FEATURES V.01.2009 - 2 / 30 -

//// Table of contents

//// Table of contents ................................................................................................... 2

//// Introduction............................................................................................................ 4

//// Key Features ........................................................................................................ 5

> ULTRA HIGH RESOLUTION AND VERY LOW NOISE FLOOR ....................................................................... 5 > ACTIVE TOP REFERENCING.................................................................................................................. 5 > THERMAL DRIFT FREE ......................................................................................................................... 5 > TWO INDEPENDENT DEPTH AND LOAD SENSORS ................................................................................... 5 > COMPLIANT TO ISO 14577 AND ASTM E2546.................................................................................... 5 > PERFECT POSITIONING SYNCHRONIZATION........................................................................................... 5

//// Measurement Principles ........................................................................................ 6

//// Advantages of the Active Top Referencing............................................................ 6

//// Ultra Nanoindentation Head Assembly.................................................................. 7

> SCHEMATIC DESCRIPTION ................................................................................................................... 7

//// Applications ........................................................................................................... 9

> POP-IN EFFECTS................................................................................................................................. 9 > CREEP PHENOMENA AND DEPTH STABILITY......................................................................................... 10 > INDENTATION ON ULTRA SOFT GEL ..................................................................................................... 11

//// Ultra Nanoindentation Head Specifications ......................................................... 12

> Load application / measurement ............................................................................................... 12 > Displacement measurement...................................................................................................... 12 > Typical measurement time......................................................................................................... 12 > Indentation performances.......................................................................................................... 12

//// Platform Specifications ........................................................................................ 13

> POSITIONING ACCURACY ................................................................................................................... 13 > ACOUSTIC ENCLOSURE..................................................................................................................... 14

//// Indentation Software V4.0 ................................................................................... 15

> FULL SOFTWARE PACKAGE FOR DATA ACQUISITION AND ANALYSIS INCLUDING ...................................... 15 > Complete measurements modes............................................................................................... 15 > Data analysis ............................................................................................................................. 15 > Mechanical properties results.................................................................................................... 15 > Possible additional analysis for specific material properties ..................................................... 15

> GENERAL FEATURES (WINDOWS SOFTWARE) .................................................................................... 16 > Positioning control ..................................................................................................................... 16 > Automated calibration procedures............................................................................................. 16 > Data acquisition ......................................................................................................................... 17 > Data analysis ............................................................................................................................. 17 > Measurement report .................................................................................................................. 18

> MEASUREMENT MODES ..................................................................................................................... 18 > Simple Indentation: .................................................................................................................... 19 > Multicycles with constant load: .................................................................................................. 19 > Multicycles with progressive load: ............................................................................................. 19


> Continuous Multi Cycle (CMCTM)............................................................................................... 19 > Dynamic Mechanical Analysis (DMA)........................................................................................ 20 > Sinus mode................................................................................................................................ 20 > Matrix (with the same indentation settings) ............................................................................... 21 > Visual Matrix (all indentations with free settings) ...................................................................... 21 > User defined matrix (all indentations with free settings)............................................................ 22 > User defined profile.................................................................................................................... 22 > Martens hardness ...................................................................................................................... 23 > Plastic and elastic parts of the indentation work ....................................................................... 24 > Data and measurement analysis ............................................................................................... 25 > Statistical mode: ........................................................................................................................ 25

//// Video Software V4.0............................................................................................ 26

> GENERAL FEATURES......................................................................................................................... 26 > MULTI FOCUS IMAGE (ONLY WITH Z AXIS AUTOMATION)....................................................................... 27

//// Microscope .......................................................................................................... 28

//// CCD Camera ....................................................................................................... 28

//// Optional AFM (Atomic Force Microscope) ........................................................... 29

> AFM FEATURES................................................................................................................................ 29

//// Contact Us........................................................................................................... 30


//// Introduction For the past twenty years, CSM Instruments and its mother company CSEM (Swiss Center for Electronics and Microtechnology) have been an active part of the development of nano mechanical testing instruments for surface and coatings characterization. The CSM Nanoindentation tools are now at the forefront of the technology for characterization of materials at the nanometer scale. Most significantly, CSM’s combination of high-performance depth-instrumented indentation in an integrated Platform configuration along with an AFM or confocal microscope commonly makes it the most useful nano hardness testing tool available for a laboratory. The instrument’s unique referencing design allows for a number of beneficial features, including an open and accessible configuration, a continuous differential depth measurement, a greater thermal stability, and a fast indentation cycle. Combined with the automation abilities of the Open and Compact Platforms, the unique referencing design of the CSM Nanoindentation Tester provides great improvements to laboratory productivity and throughput. The CSM Ultra Nanoindentation Tester (UNHT) has been used for a very wide range of applications. It represents a very efficient automated method of determining the hardness and elastic modulus values on precise positions on a sample surface. A variety of sample configurations and types of materials can be analyzed. The instrument has been used to quantitatively characterize the properties of hard coatings, single or multi-layer films, bulk soft materials, polymer film systems, and multi-phase alloys. Automotive topcoats, semiconductor wafers, IC bonding pads and wires, optical sensors, battery separation films, components for aerospace applications, amongst many other devices, have been investigated. This State-of-the-Art Nanoindentation instrument, is based on the principle of using an axis of measurement and an axis of reference, each one having its own actuator and its own sensors of depth and force. It is therefore possible to carry out active referencing of the surface of the sample.

The UNHT is equipped with a thorough, easy-to-use software package that allows the user to perform Nanoindentation tests in a wide variety of testing modes, including simple loading, multi-cycle loading (increasing or constant loads), dynamic mechanical analysis, automated matrices, and location-pinpointed testing.

Figure 1. Localized nanoindent


//// Key Features The Ultra Nanoindentation Tester corresponds to a high resolution Nanoindentation system with extreme accuracy and extremely low thermal drift. It makes it especially suited for applications such as polymeric materials, very thin layers and soft tissues. Its range of load can be wide but it is better suited for low loads (< 10 mN) where measurements on the corresponding applications can bring tremendous information.

> Ultra high resolution and very low noise floor Depth resolution: 0.0003 nm, noise floor ≈ 0.03 nm* Force resolution: 1 nN, noise floor ≈ 0.1 N*

> Active top referencing The reference is removable and could be of different shapes (balls…). The reference has its own Piezo actuator and load sensor and is applying a very well controlled (servo loop) shallow load on the sample (as low as mN) > Thermal drift free The head is constructed out of ZeroDur® glass and the electronics has a drift rate of ≈ 1ppm/°C

> Two independent depth and load sensors (Ultra high resolution capacitive sensors)

True depth and load control modes Real direct measurement of depth and load

> Compliant to ISO 14577 and ASTM E2546 CSM Instruments produces instruments and measurements that conform perfectly to ISO and ASTM standards.

> Perfect positioning synchronization The Ultra Nanoindentation Tester is perfectly “positionally synchronized” with a high quality optical video microscope and/or an optional Atomic Force Microscope (AFM). The combination of the Ultra Nanoindentation Tester head, the optical microscope and the AFM objective provides great flexibility and ease-of-use, as well as accurate three-dimensional imaging at the nanometer scale.


//// Measurement Principles

The sample is moved by the vertical table in order to touch the reference. The servo loop of the reference is then activated with the selected contact load (as low as mN).

The indenter approach is performed (piezo actuator) and the contact is detected with the

indenter load sensor.

The indentation cycle is run using the piezo actuator (in servo loop mode) to generate the load and both the depth sensor and the load sensor to measure the penetration depth and the normal load.

//// Advantages of the Active Top Referencing

The big advantage of the top referencing is that the indenter displacement is measured differentially to the reference already in contact with the sample.

The indenter motion is always relative to any movement of the sample or thermal drift of the

body, which, with a static system, would cause error due to elasticity of the sample or compliance of the supporting framework, or temperature fluctuations

Allows a shorter approach distance and time when compared to a non-reference system

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//// Ultra Nanoindentation Head Assembly > Schematic description

Figure 2. Schematic design of the Ultra Nanoindentation head FN : Normal Force (FN Indenter and FN Reference) C1: Indenter’s Load cell capacitive sensor C2: Reference’s Load cell capacitive sensor C3: Penetration depth differential capacitive sensor


Abstract of the patent : The invention concerns a measuring head using a measuring axis and a reference axis having, each, their own actuating means (A1, A2) and their own displacement measuring means (C1 to C3) and applied force measuring means (C1, K1, C2, K2). The indentation measurement can therefore be performed relative to a reference whereof the application force on the sample (E) is accurately controlled. The independent control of the axis of reference enables any disturbance of the sample and/or of the measuring instrument itself, for example, resulting from a temperature variation, to be prevented.


//// Applications The Ultra Nanoindentation Tester is an instrument module designed to pick up and record variations of penetration depth at a sub-nanometer accuracy. At the same time, the high resolution force and depth measurements are contingent to a high stability of the different signals. Indeed, many instruments could display a high resolution but the stability of the different signals is in fact the key factor of an effective and reliable Nanoindentation measurement.

Thanks to the high stability of the depth and force measurements, the Ultra Nanoindentation Tester provides new insights in materials phenomena like pop-in and creep. > Pop-in effects Nanoscale variations of depth could occur during a Nanoindentation test (unloading or/and loading curve). While some instruments have noise values in the range of 1 or 2 nm, these small instantaneous variations of depths could be lost in the general noise of the instrument. The Ultra Nanoindentation Tester is able to accurately display these small variations of depth (from 1 to 3 nm).

Figure 3. Pop-in effect (2 mN maximum load)

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> Creep phenomena and depth stability Thermal drift is common in nano-range instrumentation. Creep phenomenon is showing the same effect on the penetration depth, as the measured depth can increase for a constant applied load. It is therefore important to have a perfect depth stability of the instrument.

Constant depth at a constant load (raw data showing the true depth stability)

Figure 4a. Fused silica sample: 2 mN max load with a pause of 60 seconds at max load

Creep phenomenon (increasing depth at a constant load)

Figure 4b. Copper sample: 5 mN max load with a pause of 60 seconds at max load

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> Indentation on ultra soft gel The Nanoindentation test shown below demonstrates the incredible stability of the UNHT head for a small force and a high penetration depth: an indent of 22 um depth is accurately measured with an applied load of only 100 uN ! In that case, it is possible to measure the value of this extremely small elastic modulus: 171 kPa. The load vs. depth curve is shown together with the curves of load and depth vs. time. The load stability of the signal for high depths and small loads is clearly seen.

Figure 5a. Force vs Depth

Figure 5b. Force and Depth vs time


//// Ultra Nanoindentation Head Specifications > Load application / measurement

Piezo actuator/capacitive sensor Load range 0 – 50 mN (optional 100 mN)

- fine range: 10 mN - standard range: 50 mN

Load resolution : 1 nN, noise floor ≈ 0.1 N* (rms) Minimum usable load : 25 N Maximum load : 50 mN (100 mN with high load option) Minimum contact force : 0.1 N* ( = noise floor ≈ 0.1 N) Contact force hold time : unlimited

> Displacement measurement

Differential capacitive sensor Displacement resolution 0.0003 nm, noise floor ≈ 0.03 nm* (rms) Thermal drift (raw and uncorrected data) : ≈ 0.5 nm/min (= 0.008 nm/sec) Maximum indentation depth :

- fine range: 10 m - standard range: 100 m

Maximum indenter travel range : 100 m

Usable load range for Ultra Nanoindentation Tester: from 0.025 mN to 50 mN in maximum load of indentation

Maximum depth: 100 μm

Figure 6. Schematic of a typical depth-instrumented indentation curve

> Typical measurement time

Less than 5 minutes including first measurement on a new sample No thermal stabilization is required after loading of a new sample

> Indentation performances

Loading rate: from 0 to 1000 mN/min Usable load: from 0.01 to 50 mN (up to 100 mN with the maximum 100 mN option)

* This value is obtained in a noise free lab. It is highly environment dependent.

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//// Platform Specifications CSM Instruments proposes two platforms of measurements: Compact Platform (CPX) and Open Platform (OPX) (please see Figure 5 for pictures of the platforms). The descriptions of the platforms are also available on a separate brochure.

(a) Compact Platform (b) Open Platform

Figure 7. Indentation and/or Scratch CSM modules can be mounted on one of two platforms, depending on how many modules will be required. The Compact Platform (a) can accommodate 2 modules, whereas the Open Platform (b) can accommodate 3 modules total. A full video microscope comes standard on either platform. Displacement tables

OPX Range CPX Range Standard Resolution

High Resolution (optional)

X 245 mm 120 mm 0.25 µm 0.1 µm Y 120 mm 20 mm 0.25 µm 0.1 µm Z 30 mm 30 mm 10 nm -

Maximum sample size X, Y and Z

Compact Platform: 230 x 580 x 120 mm Open Platform: 250 x 480 x 120 mm

Usable areas of analysis X and Y

Compact Platform : 70 x 20 mm Open Platform : 195 x 120 mm

System Dimensions (with anti-vibration table)

Compact Platform: 600 x 600 mm, 1200 mm height Open Platform : 900 x 600 mm, 1200 mm height Total weight: ~ 150 kg

The usable areas of analysis indicate the areas of possible automated analysis in the X&Y directions. This area will also vary with the other modules installed (Scratch, AFM and/or ConScan).

> Positioning accuracy

Standard resolution of X&Y tables: 0.25 m per axis Repositioning accuracy of standard tables: 1 m per axis

For the high resolution tables, please ask CSM Instruments for more details. All table movements (X, Y, Z) can be controlled with Joystick.

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> Acoustic Enclosure Acoustic enclosure is highly recommended to prevent disturbances from human voices or other neighbouring machines. Acoustic Enclosure attenuation average for frequencies between 100 – 10 000 Hz : - 50 dB. The frequency resonance of the Ultra Nanoindentation head is around 130 Hz.

Figure 8. Open Platform in Acoustic Enclosure with Ultra Nanoindentation Tester


//// Indentation Software V4.0 The new software, V4, for Scratch and Indentation has been developed with completely new features in order to help our customers use our instruments more efficiently and accurately. (The enhanced application standards and the obvious traceability of those are an entire part of our new development.)

> Full software package for data acquisition and analysis including > Complete measurements modes

Complete control of indentation parameters (loading/unloading rate, maximum load, pauses, loading modes, …)

Real time display of force and depth data during acquisition, with the possibility to initiate an instantaneous user controlled unloading during the experiment

Fully user definable indentation modes (single/multi cycles, linear and square root loading ramps, unlimited hold time, user-defined load profiles)

Powerful indentation modes including CMCTM (Continuous Multi Cycle) and large area mapping

System setting programmable for every single indent in a multi-indent experiment. Fully customized user access rights management Integration of the indenter tip calibration curve Automated positioning correlation between indentation and imaging analysis Full integration of AFM and Video imaging into the indenter control software

(with AFM option only) MultiFocus Imaging, MultiFocus produce a picture with a perfect depth of field.

> Data analysis

Powerful and fully integrated statistical module (data and graphical tools) Automatic measurement report generator, unlimited templates and test protocols Logging of all operations executed on the instrument Multi language support Data export in ASCII format top open files in Excel and Text software

> Mechanical properties results

Automatic calculation of Hardness(HIT), Elastic Modulus (EIT) and Creep (CIT), Relaxation (RIT) and Recalculated Vickers (Hv)

Plastic and elastic parts of the indentation work Display of all indentation data results : maximum depth, contact depth, residual depth,

projected contact area, stiffness (according to depth-instrumented indentation theories) Display of Hardness and Elastic Modulus vs. Depth Multiple models for hardness and elastic modulus evaluation Standard evaluation according to ISO 14577 and ASTM E2546

> Possible additional analysis for specific material properties

Analysis of fracture toughness, creep and stress-strain behaviour Analysis of plastic-elastic energy work ALSO INCLUDED: Material deformation modelling software

(additional modelling software based on elastic contact mode: Hertz theory)


> General Features (Windows Software) > Positioning control X-Y-Z Position control for sample positioning and motion between measurements

Sample positioning with industrial joystick, keyboard, mouse, table crosshairs, or vectors. > Automated calibration procedures

UNHT – Optical distance Optical – AFM distance (or Optical - ConScan objective)


Automated indenter calibration (with frame compliance included)

All the data are presented in a clear and very understandable format on the screen

> Data acquisition Continuous real time data acquisition of load (FN) and displacement (DZ) signals during an indentation.

Normal force FN sampling rate : > 5000 points/s Displacement DZ sampling rate :> 5000 points/s DZ and FN filtering : 10 points/s

> Data analysis Analysis of NHT measurement files using modified W.C. Oliver and G.M. Pharr calculation method Reference: - J. Mater Res., Vol. 7, No. 3, Mar 1992

- J. Mater Res., Vol. 7, No. 6, Mar 1992 - Thin Solid Films, 308-309 (1997) 297-303 - Journal of materials research Vol. 19, No. 1, Jan 2004 Other methods: Tangent method, Martens Hardness

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> Measurement report

In the same file, you can put all the indentation curves corresponding to a single sample. Pictures and comments can also be included to provide a more comprehensive analysis

A complete synthetic report for a set of measurements can be

automatically generated

> Measurement modes

New measurement type - Standard - Advanced - Constant Multicycle - Progressive Multicycle - CMC (Continuous Multicycle) - Sinus (with option installed) - Line - Simple matrix - Advanced matrix - User defined profile Use of a protocol A previous measurement type can be launched.

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During the measurement process, an on screen real time monitoring of the indentation curves is displayed

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> Simple Indentation: - Maximum depth or maximal load - Loading rate - Pause - Unloading rate - Linear or quadratic loading > Multicycles with constant load:

- Maximum loading depth or force - Minimum unloading depth or force - Number of cycles - Loading rate - Pause - Unloading rate > Multicycles with progressive load:

- First maximum loading depth or force - Minimum unloading depth or force - Number of cycles - Loading rate - Pause - Unloading rate > Continuous Multi Cycle (CMCTM)

- First minimum load - Maximum load - Choose the unloading % - Time to max load - Pause - Time to unload - Number of cycles After the CMC measurements, the graphs of Hardness and Young’s Modulus vs Penetration Depth can be directly analyzed.

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> Dynamic Mechanical Analysis (DMA)

- Maximum load - Loading and Unloading rate - Pause - Sinus Frequency - Sinus Amplitude The Dynamic Mechanical Analysis uses sine wave loading curves to obtain a more complete analysis of the mechanical properties of viscoelastic materials. This method allows for a continuous acquisition of Hardness, Elastic modulus, Storage and Loss Modulus data as a function of indentation depth. > Sinus mode

Sinus amplitude Sinus frequency

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> Matrix (with the same indentation settings)

Series of indentations with defined X and Y distances between each indentation One indentation setting Possibility to store the matrix setup for future use

> Visual Matrix (all indentations with free settings)

Series of indentations selected optically, You select the Indentation positioning with the computer mouse directly on the PC screen. User defined indentation settings for each indentation

Before Indentation testing After Indentation testing

Indents


> User defined matrix (all indentations with free settings)

Series of indentations selected optically, You select the Indentation positioning with the computer mouse directly on the PC screen. User defined indentation settings for each indentation

> User defined profile

Indentations with user defined profile Possibility to store the user defined profile setup for future use quadratic or linear loading


> Martens hardness

Indentation using a quadratic loading profile (Norm DIN 50359-1) Possibility to store the user defined profile setup for future use


> Plastic and elastic parts of the indentation work The mechanical work Wtotal indicated during the indentation procedure is only partly consumed as plastic deformation work Wplast. During the removal of the test force the remaining part is set free as work of the elastic reverse deformation Welast. According to the definition of the mechanical work as W = Fdh both parts appear as different areas in Figure bellow.


> Data and measurement analysis

Various analysis methods (according to norm ISO 14577): Oliver and Pharr, Tangent,

Martens, Sinus modes Continuous determination of hardness and elastic modulus:

Hardness, Elastic Modulus and Stiffness vs. Penetration Depth

> Statistical mode: Average, standard deviation, min, max, median, number of measurements per sample

Exportable data and statistics in text files (for Excel, …)


//// Video Software V4.0 > General features Instruments are delivered with a video microscope. Objectives are available from x5 to x 100 Nikon objectives.

Two video cameras (USB2.0) are available: the standard unit with a resolution of 768 x 582 or the optional high resolution (1280x1024) model using a progressive scan sensor with a very high sensitivity. The CSM Video Software is the perfect companion of the CSM Indentation and Scratch Testers for the optimal use of video microscopy:

Real-time video display Crosshair, scales, differential measurement tools Automatic image scaling Objectives available: x5, x20, x50, x100 for magnifications x200, x800, x2000, x4000 respectively Image capture, the picture will automatically be added to Scratch or Indentation image gallery Layer thickness measurement (with the Calotest)

With this software, you can: Capture the picture of an indentation, Measure the distances with the cursors, Show the picture scale, Calculate the radius of a circle (if you have the Calotest, you can also calculate the thickness of the coating).


> Multi Focus Image (only with Z axis automation)

MultiFocus produce a picture with a perfect depth of field. During the video capturing, our platform will move in Z direction in order to take and combine different levels of focused depth into one image. Examples:

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//// Microscope

The measuring head and the microscope are mounted side-by-side and linked by the two X- and Y- translation tables

Video microscope magnification from 200x to 4’000x

Allows a specific sample site to be selected

Modular focusing unit - Stroke 30 mm - Coarse focusing 5.2 mm/rotation - Fine focusing 0.1 mm/rotation - Distance optical axis 141 mm Mounting surface

Objectives available: - 5x Working distance 22.50 mm - 20x Working distance 3.10 mm - 50x Working distance 0.54 mm - 100x Working distance 0.30 mm

Revolving Nosepieces - Nosepiece 4 or 5 objectives

//// CCD Camera Standard Resolution Camera Resolution 768 x 582 (CCIR/PAL) Sensor High Quality 1/2'' SONY CCD sensor with square pixels Scanning Progressive scan Frame Rate Up to 50 fps Mount adapter C-Mount Interface USB 2.0 Power supply Via USB (<1.5W) Size (HxWxD) 34 x 32 x 34.4 mm Weight 75 g


//// Optional AFM (Atomic Force Microscope)

An AFM objective can be mounted together aside the standard optical objectives The AFM head is approached automatically until its cantilever tip contacts the sample surface Cantilever deflection is detected using an optical interferometer The compact AFM head is manufactured by Surface Imaging Systems (SIS)

> AFM features

Scanning unit: Piezotube with integrated fiberoptic sensor plug, sensor for closed-loop X-Y scanner linearization

Scan modes contact, non-contact & friction optional

(see different modes in AFM technical specifications)

Deflection detection Glass fibre interferometer with laser diode

Laser Wave length 780 nm Class 3a Max. Power 5 mW (direct at diode) 500 W (at the fibre end)

Scan range (X, Y) : 40 x 40 m / 80 x 80 m

Vertical scan range (Z) :4 m – 6 m respectively (estimated maximum depths of analysis, experimental observed values can be higher)

Resolution: X, Y, Z < 1 nm

Data acquisition 12 bit DSP board

Scan control Power supply 230V, 50 Hz, 100 VA Security class SK I Security type IP 20 HV (High Voltage) out put for XYZ 150 V HV out put for cantilever actuator 0-60 V


//// Contact Us

//// CSM Instruments SA Rue de la Gare 4 CH-2034 Peseux Switzerland [email protected] T : +41 32 557 56 00 F : +41 32 557 56 10

//// CSM Instruments, Inc. 197 1st Ave, suite 120 Needham, MA-02494 United States [email protected] T : (781) 444-2250 F : (781) 444-2251

//// CSM Instruments Germany Basler Strasse 115 79115 Freiburg Germany [email protected] T : +49 7 61 47 87 150 F : +49 7 61 47 87 100

//// CSM Instruments China 1518 15th floor NCI Tower 12A, Jianguomenwai Ave Chaoyang District, Beijing 100022 China [email protected] T : +86 10 8523 3119 F : +86 10 8523 3001

The content of this document is subject to change without prior notice. Copyright CSM Instruments.

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ULTRA NANOINDENTATION TESTER (UNHT) · 2012-11-21 · //// UNHT : TECHNICAL FEATURES V.01.2009 - 9 / 30 - //// Applications The Ultra Nanoindentation Tester is an instrument module