Optics11 Piuma Nanoindenter User Manual
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Optics11 Piuma Nanoindenter User Manual

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USER MANUAL
PIUMA NANOINDENTER

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  • Page 1 USER MANUAL PIUMA NANOINDENTER...
  • Page 2 VISITING ADRESS Optics11 VU University Campus W&N Building room O-236 De Boelelaan 1081 1081 HV Amsterdam The Netherlands SHIPPING ADRESS Optics11 De Boelelaan 1081 1081 HV Amsterdam The Netherlands COMPANY INFORMATION Optics11 B.V. KvK/CC: 52469417 VAT: NL850459734B01 Amsterdam, NL optics11.com...

  • Page 3: Table Of Contents

    CONTENTS Revision history Safety Introduction Installation Preparing the setup for measurement Using the Piuma Nanoindenter Optimizing instrument stability and sample mounting Working principle of the Piuma Nanoindenter instrument Description of the Piuma software The OP1550 interferometer FAQ & troubleshoot...

  • Page 4: Revision History

    Version 2.3 Update March 29, 2017 Jakob Pyszkowski Version 2.4 Update May 16, 2017 Jakob Pyszkowski Version 2.5 Update July 18, 2017 Jakob Pyszkowski Version 2.6 Update June 20, 2018 Kevin Bielawski Version 2.7 Update November 7, 2018 Jakob Pyszkowski optics11.com...

  • Page 5: Safety

    SAFETY The OP1550 interferometer, part of the Piuma Nanoindenter, is equipped with a class 1M laser. The laser light is coupled out via a fiber connector on the front panel and has a terminator on the back panel. Do not view directly into the beam with optical instruments.

  • Page 6: Introduction

    Optics11. Details of the installation of the Piuma Nanoindenter are provided in Chapter 1. Chapter 2 describes the preparation of the Piuma Nanoindenter for experiments. How to perform a measurement is described in detail in Chapter 3. Chapter 4 describes the optimization of sample preparation and measurement conditions.

  • Page 7: Installation

    OP1550 interferometer, (3) the Piuma controller, (4) the PC running the Piuma Nanoindenter software suite and (5) the Optics11 optical nanoindentation probes. Figure 2: Picture of the Piuma Nanoindenter, showing the Piuma indenter head (far left), OP1550 interferometer, Piuma controller and the PC.
  • Page 8 The Optics11 OP1550 interferometer operates independently of the other components and can be switched on and off at any time. The Piuma controller box powers the Piuma indenter head and communicates with the software running on the PC and should not be switched off before exiting the Piuma nanoindentation software suite.
  • Page 9 ‘Piezo’ input at the back of the controller. The OP1550 readout is connected to controller box using one BNC and one USB cable. The BNC cable connects the ‘Output’ at the front of the OP1550 with the ‘Input’ on the back of controller box and the second USB cable connects the ‘USB’ output on the back of the OP1550 to the second ‘HUB’...

  • Page 10: Preparing The Setup For Measurement

    2. OP1550 interferometer 3. Controller box The controller box automatically powers the Piuma Nanoindenter head and the LED illumination in the indenter head will turn on. After initialization, the interferometer will show a live measurement signal on the LCD screen.
  • Page 11 This action initiates the homing of the X-Y stage of the Piuma Nanoindenter: The stage will move to the front-left corner, set the current ‘X’ and ‘Y’ coordinates to ‘0’ and subsequently move to the last coordinate set in the matrix scan parameters. After this, the system state will switch to ‘ready’, as indicated in the status bar in the home screen.
  • Page 12 Figure 5: Probe and fiber wire inside the box (left), probe mounting to the indenter (right). After powering the Piuma Nanoindenter system and running the software, open the indentation probe box. Carefully take first the probe out of the box in such a way that the probe can be clicked in the Piuma indenter head in one go.
  • Page 13 Figure 6: Connecting the fiber to the OP1550, a notch (red circle) indicates the preferred orientation Next, remove the tape and green safety cap from the optical fiber connector and connect it to the ‘Sensor’ input of the OP1550 interferometer (Figure 6). The fiber connector is a FC/APC type connector, which has a preferred orientation, indicated by the notch on the fiber connector and a groove in the OP1550 connector.
  • Page 14 For this procedure a value of 4000nm for the calibration depth is set by default. You can can change this value in the ‘Options’ menu, shown in the figure 7, right before peforming measurements with higher indentation depths (<5000nm). optics11.com...
  • Page 15 Setting the correct indenter head and corresponding XYZ stage values The correct indenter head, here the Piuma, has to be selected in the ‘Advanced’ tab in the ‘Options’ menu (Figure 8, left). Since the XYZ stage travel values of the Piuma and Chiaro are differing, you need to update the right values corresponding to the preferred indenter head.
  • Page 16 DMA tab of the configure ‘Profile’ menu (Figure 10, left). Then click on ‘Calibration’ in the Chiaro Software Menu to enter the calibration menu (Figure 9). Press ‘Scan OP1550 Wavelength’ to start the optical calibration (Figure 10, right). You can observe the wavelength scan process, after closing the calibration window (Figure 11). optics11.com...
  • Page 17 Figure 9: Set ‘Displacement control’ for automatic optical signal calibration. Figure 10: DMA mode switch in profile configuration menu (left), ‘Scan OP1550 Wavelength’ for automatic optical signal calibration (right). Principle: The OP1550’s internal laser will tune its wavelength rapidly from ~1565nm to ~1525nm to create an interference pattern on the photodiode.
  • Page 18 Since the density of a liquid usually decreases with temperature, it is not surprising that the speed of light in a liquid will normally increase as the temperature increases. Thus, the index of refraction normally decreases as the temperature increases for a liquid. optics11.com...
  • Page 19 2.4 Calibrating the probe geometrical factor Optical Geometrical Measurement calibration factor After performing the optical calibration, the linearization of the interferometer and calibration of the cantilever arm, also called geometrical factor, needs to be performed. Those two steps are accomplished in one calibration procedure. During the signal linearization, the nonlinear response due to cantilever bending is transformed to a linear signal, using the unity circle as a linearization tool.
  • Page 20 In order to get into contact with the stiff surface, the Piuma Nanoindenter features an automated find-surface approach. This approach uses a coarse-fine stepping routine, combining the motorized Z stage and the indentation piezo.
  • Page 21 After the procedure is finished, the program will ask you whether to use the newly calculated factor or retain the old one. Figure 15: Message to confirm calibration value. By pressing ‘Use new’ the software automatically saves the new ‘Calibration factor’ in the probe configuration menu.

  • Page 22: Using The Piuma Nanoindenter

    3. USING THE PIUMA NANOINDENTER This section describes the use of the Piuma Nanoindenter after having prepared the instrument for a measurement (Chapter 2). Optical Geometrical Measurement calibration factor 3.1 Stage controls The motorized stages of the Piuma can be manually positioned in X, Y and Z directions, each having a travel of 12000 mm.
  • Page 23 3.3 The Find surface procedure The Piuma Nanoindenter features an automated find-surface approach. This approach uses a coarse-fine stepping routine, combining the motorized Z stage and the indentation piezo.
  • Page 24 Approaching the sample surface by 1-2 mm with the manual stage, using eyesight and/or the on-board camera. Safely using the ‘Find surface’ function of the Piuma Nanoindenter software. Approaching the sample using the manual stage To approach the sample and perform the experiment with the sample in focus, move the probe completely up using the ‘Z up’...
  • Page 25 Always verify the state of the cantilever by looking at the interferometer screen during finding the surface (see Chapter 7.1). 3.4 Modes of operation The Piuma Nanoindenter is able to operate in three different modes: • Piezo displacement control: D-mode •...
  • Page 26 (µm) and time (s) variables can be customized. A maximum segment number of 12 can be defined, by default the segment number is set to 5 (Figure 21). Figure 20: Mode selection optics11.com...
  • Page 27 Figure 21: Configure displacement, load and indentation profile P-mode The P-mode of operation allows you to set a specific load, which can be kept constant over a certain time interval. For this, the probe needs to be in contact with the sample. A velocity limited approach of sample surface sensing monitors the threshold of 10 nm cantilever bending when touching the surface.
  • Page 28 (s) divided by default in three segments (Figure 21). 3.5 Dynamic mechanical analysis - DMA The Piuma Nanoindenter features, beside the quasi static operation, a dynamic operational mode. This DMA mode allows mechanical oscillations in all three modes of operation while indenting in a sample and can be switched ‘On’...
  • Page 29 3.6 Saving measurement Each series of experiments, independent of operational modes, can be saved in a dedicated folder. To set up this folder, click the saving button in the ‘Experiment’ part of the home screen and create a folder in the browser dialog in the desired location (Figure 23). Afterwards, navigate to this folder and click ‘Select folder’.
  • Page 30 X and Y directions (dX, dY), starting location (Start X, Start Y), number of indentations per point (# Indent) and how often the scan is repeated (# Scans). In order to use the current XY position as the starting position of the scan, just click ‘Use XY’ in the ‘Scan controls’. optics11.com...
  • Page 31 Once the parameters have been set, the scan is initiated by pressing the ‘Start scan’ button. Before continuing to a new point, including the first indentation of a matrix scan, the probe moves up to a safe transportation height and subsequently moves to the indentation location. After reaching this location, the find-surface procedure is initiated.
  • Page 32 (P ), maximum displacement (D ) and (Eff.) Young’s Modulus. Figure 26: Typical indentation file showing the 37 header lines and the start of the five data columns describing the indentation curve. optics11.com...

  • Page 33: Optimizing Instrument Stability And Sample Mounting

    Preferably this bench is not shared with other vibrating machines such as vortexes, pumps, or large fans. Optionally the Piuma Nanoindenter can be mounted on top of a third-party stabilization platform, such as an air table or spring table.
  • Page 34 Laminar flow cabinet The Piuma Nanoindenter can also be used inside a Figure 27: Side-view of Piuma Nanoindenter. laminar flow cabinet. For optimal stability, only put the Piuma indenter head in the laminar flow cabinet on a sturdy surface and set up the peripherals outside the flow cabinet.
  • Page 35 selecting the appropriate cantilever stiffness, tip size and indentation settings. For example, when working with samples that have a porous surface, selecting a tip diameter that is either much smaller or larger than the average pore size avoids having the tip trapped in the sample. Sample immobilization Next to a stable sample, it is important to immobilize the sample to eliminate lateral and height drift during and between indentations.
  • Page 36 The ‘Probe suitability’ indicator in the bottom-right corner of the software indicates the suitability of the probe in use. Please see the probe selection guide for more information on selecting the appropriate probes for your experiments. optics11.com...
  • Page 37 Suitable probe tip size Choosing an appropriate tip size is related to the structure of the sample and the kind of experiment one wishes to perform. When measuring the global elasticity of a sample, a larger tip would be more suitable, since the applied and recorded force of each indentation would effectively average over a larger area than for a small tip.

  • Page 38: Working Principle Of The Piuma Nanoindenter Instrument

    5.1 Principle of operation The Piuma Nanoindenter uses proprietary optical probes in combination with the Optics11’s OP1550 interferometer, to precisely detect sample deformation by detecting cantilever bending. The Piuma’s unique probes are at the heart of what makes the Piuma instrument so easy to operate and provide unparalleled precision at the same time.
  • Page 39 The optical probes used in the Piuma Nanoindenter are manufactured in Amsterdam, and consist of an optical connector, an optical fiber, a probe holder and an indentation probe, all in one piece. The cantilever stiffness and tip size of the probe is calibrated at Optics11 and the values are provided on the probe’s container.
  • Page 40 Figure 33: Schematic picture of probe (left) and picture of probe mounted in the Piuma Nanoindenter. 5.2 The measurement and calculation of the Young’s modulus The determination of the Young’s modulus relies of the measurement of load-indentation curves, which subsequently can be analysed by different material models. For elastoplastic materials, the Oliver&Pharr model...
  • Page 41 Figure 34: Typical load-displacement curve of an indentation (left). The ‘unloading’ curve is used to derive the Young's modulus, by applying the Oliver and Pharr method. Schematic imprint of made by a spherical indenter after loading and unloading cycle (right). ∗...
  • Page 42 If the amplitude of the input oscillation is small enough, the measurements can be considered within the material linear viscoelastic region (LVR). Within the LVR, the response is assumed to be independent of the input amplitude and sinusoidal with the same input frequency and a phase lag, optics11.com...
  • Page 43 ��. The phase lag is 0° for a purely elastic material, 90° for a purely viscous material, and in-between 0° and 90° for a viscoelastic material. After gather the frequency-dependent storage and loss moduli, they can be fit to lumped parameter rheological models to derive material viscoelastic constants.

  • Page 44: Description Of The Piuma Software

    6. DESCRIPTION OF THE PIUMA SOFTWARE This chapter describes the Piuma Nanoindenter software suite, which is used to perform the indentation experiments. The Piuma software is pre-installed on the Piuma PC and runs by double- clicking the Piuma icon on the desktop. In case of freshly installing the Piuma software on another PC, please contact Optics11 for a detailed instruction.
  • Page 45 Experiment name and save location In the top-left of the Piuma software suite the experiment name and save location of each experiment series can be defined. In order to select a path for saving the experiment series, click on the File button. A pop-up will emerge, displaying a windows explorer window where a folder can be created or selected.
  • Page 46 The ‘dX before scan’ field enables a step in X-direction each time after finding the surface. The ‘Adhesion mode’ enables the pull-off of the cantilever from the surface in case of adhesion. It does this by moving up a certain optics11.com...
  • Page 47 amount of µm, holding there for a certain amount of time, and moving the same distance down again, starting after the software detected the surface automatically. 6.2 Results Indentation results The indentation results section describes the results derived from the latest indentation. The parameters displayed here are slope, maximum force applied, the effective Young’s Modulus and the bulk Young’s Modulus using the pre-configured Poisson’s ratio (Figure 41).
  • Page 48 This tab displays a live feed of both the optical cantilever signal as well as the video camera on board of the Piuma Nanoindenter. An image of the video feed can be saved to the hard disc by clicking ‘Save image’. The image can be magnified on the screen by clicking ‘Magnify’. The LED top lighting can be switched on (default) or off with the ‘LED light’...
  • Page 49 Figure 43: Load-displacement tab showing load- and unloading curve in P-mode. Time data tab This tab shows two graphs: The top graph contains probe displacement, cantilever bending indentation depth as a function of time. Following the displacement (Piezo) curve down, at some point the cantilever starts bending.
  • Page 50 Young’s Modulus per coordinate. This map can be showed in 2D or 3D, and the minimum and maximum Z-axis values can be manually adjusted (Figure 45, 46). The ‘Show Young’s’ button allows to convert the effective Young’s Modulus to the bulk Young’s Modulus using the preconfigured Poisson’s ratio. optics11.com...
  • Page 51 Figure 45: Young's Modulus tab, showing a 10x10 2D plot. Figure 46: Young’s Modulus plot showing a 10x10 3D plot.
  • Page 52 This menu allows to set a custom displacement, load and indentation profile. The maximum displacement or indentation depth is 20 µm and the maximum duration of one segment is 60 seconds. Therefore, the maximum load results from: �� = 20µ�� ∗ ������������ ���������������� In total up to 12 segments can be defined. optics11.com...
  • Page 53 Figure 48: Configure indentation menu. Configure probe menu This menu allows inserting of all the probe-specific parameters that are used in the software to convert voltages to force and Young’s Modulus. In case a wrong stiffness or tip radius is entered, the accuracy of the force, load and Young’s Modulus estimate will be compromised.
  • Page 54 In case the Hertzian model is selected, the ‘% of Pmax’ field controls the part of the curve to be fitted, expressed in a percentage of the maximum load in the loading part of the optics11.com...
  • Page 55 Maintenance menu The maintenance panel is protected by a password, as any change in these settings may compromise the performance of the Piuma Nanoindenter. Please note that changing parameters in the maintenance menu can cause unexpected behavior and potentially break the hardware on the Piuma. Use caution when changing parameters.
  • Page 56 Additionally, different settings for the PID settings on displacement, load, and indent control can be set from the General tab. It is recommended to only change these settings if you have experience with tuning PID controllers. Changing the parameters could result in unstable operation of the system and cause the controller to break. optics11.com...

  • Page 57: The Op1550 Interferometer

    7. THE OP1550 INTERFEROMETER The interferometer operates as stand-alone device and can be switched on or off any time the Piuma Nanoindenter system is in stand-by. The OP1550 interferometer contains a tunable laser source, modulation options, a high-speed photodiode and data acquisition electronics.
  • Page 58 (Figure 54). When calibrating the geometrical factor, the probe must be in contact with a stiff surface, otherwise the calibration fails. If the probe is not in contact after the find surface procedure, you can manually move the Z-stage in 1µm-steps down to bring the probe into contact. optics11.com...
  • Page 59 Figure 54: Datapoint changing its position after the tip is getting in contact with a surface: probe out of contact (a), noise caused by probe moving during automated find surface procedure or by manually moving the Z-stage (b), probe in contact with surface resulting in datapoint position change (c).
  • Page 60 In the ‘Maintenance’ menu the modulation phase shift and the lock-in amplification can be adjusted to certain parameters. The default settings are 80.0 degree for the ‘DDS Phase shift’ and 10.0 V for the ‘Lock-in gain’ and should not be changed. optics11.com...

  • Page 61: Faq & Troubleshoot

    8. FAQ & TROUBLESHOOT Q1: The automated find-surface function fails to detect the surface automatically. A1: The Piuma looks for a voltage difference when using the find-surface function. In case any problems occur with the find-surface function, please verify the signal amplitude on the OP1550 is sufficient (absolute values 3-7 V minimum, or an amplitude of 4V or higher).
  • Page 62 Figure 56: Example of contamination that compromises cantilever bending. Flowchart - Calibration Most issues that occur while measuring with the Piuma Nanoindenter are related to the calibration of the instrument. A troubleshooting flowchart is presented on the next page to guide you through possible issues and solutions, to ensure a safe calibration of the Piuma Nanoindenter and therefore a correct functionality of the instrument.
  • Page 64 For troubleshooting, support or questions, while working with the Piuma Nanoindenter, please contact Optics11 at: Tel.: +31 20 5987917 E-mail: info@optics11.com Office hours are between 8h and 18h, CET. optics11.com...

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