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NT-MDT NTEGRA Solaris Probe NanoLaboratory Instruction Manual

Configuration based on inverted optical microscope olympus x-71
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NTEGRA Solaris
Probe NanoLaboratory
(configuration based on inverted optical
microscope Olympus X-71)
Instruction Manual
2012
Copyright © "NT-MDT"
Web Page:
http://www.ntmdt.com
General Information:
spm@ntmdt.ru
Technical Support:
support@ntmdt.ru
NT-MDT Co., building 100,
Zelenograd, 124482, Moscow, Russia
Tel.: +7-499-735-77-77
Fax: +7-499-735-64-10

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  • Page 1 NTEGRA Solaris Probe NanoLaboratory (configuration based on inverted optical microscope Olympus X-71) Instruction Manual 2012 Copyright © “NT-MDT” Web Page: http://www.ntmdt.com General Information: spm@ntmdt.ru Technical Support: support@ntmdt.ru NT-MDT Co., building 100, Zelenograd, 124482, Moscow, Russia Tel.: +7-499-735-77-77 Fax: +7-499-735-64-10...
  • Page 2 Read me First! Observe safety measures for operation with devices containing sources of laser radiation. Do not stare into the beam. A label warning about the presence of laser radiation is attached to the laser sources (Fig. 1). Fig. 1 Before you start working with the instrument, get acquainted with the basic safety measures and the operation conditions for the instrument! If you are a beginner in scanning probe microscopy, we recommend you to familiarize with...
  • Page 3 User’s documentation set The following manuals are included into the user‟s documentation set: Instruction Manual – is the guidance for the preparation of the instrument and other ● equipment for operation on various techniques of Scanning Probe Microscopy. The contents of the user‟s documentation set may differ in dependence on the delivery set of the instrument.

  • Page 4: Table Of Contents

    NTEGRA Solaris Probe NanoLaboratory NTEGRA Solaris Probe NanoLaboratory Table of Contents 1. BASIC INFORMATION ......................... 5 1.1. NTEGRA S ....................5 URPOSE OF THE OLARIS 1.2....................6 ESCRIPTION OF OMPONENTS 1.2.1. Inverted Optical Microscope Olympus IX71 ................. 7 1.2.2. NTEGRA Base Unit ....................... 8 1.2.3.

  • Page 5: Basic Information

    Chapter 1. Basic Information 1. Basic Information 1.1. Purpose of the NTEGRA Solaris The NTEGRA Solaris PNL is a specialized SPM measurement system built on the NTEGRA platform. A SNOM measuring head lies in the basis of this system. SNOM techniques are used to study near-surface optical characteristics (including luminescent and spectral) of various objects with resolution much greater than the diffraction limit.

  • Page 6: Description Of Main Components

    NTEGRA Solaris Probe NanoLaboratory 1.2. Description of Main Components Main components of the NTEGRA Solaris PNL The following parts are included in the basis configuration of the NTEGRA Solaris PNL: 1. Inverted Optical Microscope Olympus IX71 (item. 1.2.1 on page 7).

  • Page 7: Inverted Optical Microscope Olympus Ix71

    Chapter 1. Basic Information Investigation of optical characteristics with resolution better than the diffraction limit is performed with a SNOM scanning measuring head equipped with an optical fiber probe. The probing beam is coupled into the probe by means of a laser module. An optical viewing system is employed both to select an area of the sample for investigation and to control the approach of the probe to the sample.

  • Page 8: Ntegra Base Unit

    NTEGRA Solaris Probe NanoLaboratory 1.2.2. NTEGRA Base Unit The NTEGRA base unit is used to install the scanning mount on it. In addition, the measuring head and the scanning mount are connected to the controller by means of this unit.

  • Page 9: Xy Scanning Exchangeable Mount

    Chapter 1. Basic Information Connectors for connecting the base unit with the controllers of the control system: CONTROLLER 1 – for connecting the SPM controller; CONTROLLER 2 – for connecting the SPM controller; CONTROLLER T – for connecting the thermo-controller. NOTE.
  • Page 10 NTEGRA Solaris Probe NanoLaboratory The objective is placed into the inside “cup” 9 of the scanning mount, which is a part of the approach system. Coarse focus of the objective on the area of interest is adjusted by means of the approach system of the base unit. Fine focus of the objective is adjusted by means of the Z-scanner of the scanning mount.

  • Page 11: Snom Measuring Head

    Chapter 1. Basic Information 1.2.4. SNOM Measuring Head The SNOM measuring head (Fig. 1-5) is used for both measurements of surface topography of the sample and for measurements of its near-surface optical properties. Oscillation amplitude and phase of the probe can also be registered during these measurements.
  • Page 12 NTEGRA Solaris Probe NanoLaboratory Fig. 1-6. Probe holder assembly 1 – probe holder; 2 – spring clips; 3 – bottom part of the scanner; 4 – protective case; 5 – optical fiber input orifice Movements of the scanner in the XY plane are controlled by means of the capacitance sensors (Fig.

  • Page 13: Optical Fiber Probe

    Chapter 1. Basic Information Technical specifications of the SNOM measuring head Scanning range in the XY plane 100x100 μm; ShFM resolution: in the XY plane <20 nm; ● in the Z direction <0.1 nm; ● SNOM resolution in the XY plane <100 nm; Number of pixels up to 1024x1024;...

  • Page 14: Laser Module

    NTEGRA Solaris Probe NanoLaboratory Optical fiber probe technical specifications Optical fiber type single-mode; Accepted wavelengths 480†550, 600†680, 780†1050 nm; Fiber length 2 m; Fiber transmission coefficient, K †10 Output aperture diameter ~100 nm; Radius curvature of the tip ~100 nm;...

  • Page 15: Photomultiplier Modules

    Chapter 1. Basic Information Positioning stage: Translation resolution 1 μm, along X, Y, Z; ● Travel 4 mm, along X, Y, Z. ● NOTE. The laser module assembly can vary. It can be equipped with different lasers: gas, solid-state, with different power characteristics and operating wavelengths (see data sheets).
  • Page 16 NTEGRA Solaris Probe NanoLaboratory ATTENTION! Photomultiplier is a photosensitive device. To avoid permanent damage and earlier degradation, do not expose it to high intensity radiation even if it is not connected. Open the shutter only for measurements. Avoid overloading the photomultiplier.

  • Page 17: Spm Controller

    Chapter 1. Basic Information 1.2.8. SPM Controller The SPM controller provides control of the probe measurement system. Its main functions are: Processing signals received from measuring heads; ● Conversion of signals generated by the computer control program Nova; ● Generating signals for scanners and probe; ●...

  • Page 18: Optical Viewing System

    NTEGRA Solaris Probe NanoLaboratory 1.2.10. Optical Viewing System The video viewing system is intended to perform visual control over the following processes: selection of an area of the sample for measurement; ● approach of the probe to the sample; ●...
  • Page 19 Chapter 1. Basic Information Due to the modular design of the system, the instrument can be configured to operate in different scanning modes: Scanning by probe; ● Scanning by sample. ● During scanning-by-probe the sample does not move, while the scanner of the measuring head performs the procedure.
  • Page 20 Fig. 1-13. Block diagram of the NTEGRA Solaris PNL...
  • Page 21 Chapter 1. Basic Information Transmission Mode The Transmission Mode (Fig. 1-14) is used for measurements on transparent and semitransparent samples. The probe approaches the sample from the top. The optical radiation, which is transmitted through the sample, contains the information on properties of the sample and it is collected by the objective and, then, directed to the photo-detector.
  • Page 22 NTEGRA Solaris Probe NanoLaboratory Reflection Mode The Reflection Mode (Fig. 1-15); is used for measurements on non-transparent samples. The probe approaches the sample from the top. The optical radiation, which is scattered on the surface the sample, contains the information on properties of the sample surface. It is diverted to the objective by a mirror and is then directed to the photo-detector of the optical system.

  • Page 23: Safety Measures

    ● Do not disassemble any part of the device. Disassembling of the product is permitted ● only to persons certified by NT-MDT. Do not connect additional devices to the instrument without prior advice from an ● authorized person from NT-MDT.
  • Page 24 NTEGRA Solaris Probe NanoLaboratory Laser Observe safety measures for operation with devices containing sources of laser ● radiation. Do not stare into the beam. A label warning about the presence of laser radiation is attached to the measuring head. Labels are different for different wavelength and output power of laser (Fig.

  • Page 25: Operating Conditions

    Chapter 1. Basic Information 1.5. Operating Conditions NTEGRA Solaris is a high precision optical instrument. Therefore high requirements are made on the premises, power supply system and the optical table quality during installation. Also the room for the installation should be darkened and a source of low power scattered light should be available in addition to the main light source (top light).
  • Page 26 NTEGRA Solaris Probe NanoLaboratory the table intended for installation of the instrument measuring unit must be stable and, ● whenever possible, massive; to provide solid stability against vibrations, SPM modules should be placed on self- ● leveling floor with marble covering alongside bearing components of the building (pillows, beams etc.);...

  • Page 27: Storage And Transport Instructions

    Chapter 1. Basic Information 1.6. Storage and Transport Instructions Packaging of the equipment should be performed indoors in a ventilated room at ● ambient temperature of 15° С – 40 °С and relative humidity at most 80 % with no corrosive agent in the atmosphere.

  • Page 28: First Time Installation

    NTEGRA Solaris Probe NanoLaboratory 2. First Time Installation 2.1. Assembly of Main Modules Assembly of main modules requires the following steps: 1. Loosen the approach lever fastening screw 3 located in the base unit (Fig. 2-1). Fig. 2-1. Base unit 1a –...
  • Page 29 Chapter 2. First Time Installation 4. Winding the lever drive knob 1a (Fig. 2-1) clockwise, insert the end of the approach lever 2 into the hole 3 (Fig. 2-3) in the inside “cup”. Fig. 2-3. Bottom part of the scanning mount 1 –...
  • Page 30 NTEGRA Solaris Probe NanoLaboratory Fig. 2-5. The base unit with the scanning mount installed on the Olympus IX71 microscope 8. Set up the optical viewing system. The more detailed description of the optical viewing system is provided in the manual “Performing Measurements” (see Appendix).
  • Page 31 Chapter 2. First Time Installation Fig. 2-6. Spring stops b. Screw the objective into the inside “cup” of the scanning mount (Fig. 2-7). Fig. 2-7. Installation of the objective into the scanning mount c. Set the sample holder in the XY positioner of the scanning mount (Fig. 2-8). Fig.

  • Page 32: Installation Of Interconnections Between Parts Of The Instrument

    NTEGRA Solaris Probe NanoLaboratory 10. Set the assembled instrument on the vibration isolation table. Assembly of main modules is completed. 2.2. Installation of Interconnections between Parts of the Instrument ATTENTION! Switch controller before connecting/disconnecting cables. Disconnecting or connecting cables while the instrument is operating may cause damage to electronic circuits.

  • Page 33: Preparation Of The Ntegra Solaris Pnl For Operation

    Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation 3. Preparation of the NTEGRA Solaris PNL for Operation 3.1. Main Steps of Preparation for Operation Preparation of the instrument for operation in dependence of the choice of the optical measurement scheme requires the following procedural steps: 1.
  • Page 34 NTEGRA Solaris Probe NanoLaboratory Fig. 3-1. Block-diagram of interconnections between the electro-mechanical parts for scanning-by-sample Configuring the system to operate in the “scanning-by-sample” mode requires the following procedural steps: 1. Connect the cable SCANNER of the scanning mount 1 (Fig. 3-2) to the connector SCAN+SENSOR located on the base unit.
  • Page 35 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation 2. Connect the cable of the Z-scanner of the scanning mount to the controller (see Fig. 3-1). 3. Connect the cable SCANNER, 2, of the measuring head to the top of the cable SCANNER, 1, of the scanning mount.

  • Page 36: Installation Of The Probe Into The Measuring Head

    NTEGRA Solaris Probe NanoLaboratory 3.3. Installation of the Probe into the Measuring Head ATTENTION! The probe tip is extremely fragile. Avoid any physical contact with it to prevent damage to the probe. The probes are supplied packaged in plastic boxes (Fig. 3-4) (one box contains two probes).
  • Page 37 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation 2. Open the box with probes (Fig. 3-6). Take the roll of one of the optical fibers, do not remove the probe itself. Roll the fiber out carefully; do not bend it too much. Fig.
  • Page 38 NTEGRA Solaris Probe NanoLaboratory Fig. 3-9 Fig. 3-10 6. Holding the probe near the holder in the measuring head, pull the fiber through the head. Insert the probe under the spring clips (Fig. 3-11). Fig. 3-11. 1 – contact areas of the probe; 2 – spring clips; 3 – holder...

  • Page 39: Assembly Of The Laser Module

    Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation 3.4. Assembly of the Laser Module Main components of the laser module are shown in Fig. 3-12: Fig. 3-12. Laser module 1 – laser; 2 – objective; 3 – fiber mounting stage; 4 – magnetic fasteners; 5 –...
  • Page 40 NTEGRA Solaris Probe NanoLaboratory Switching the laser on 1. Connect the laser with the power supply: Connect the power supply cable to the connector 220V of the power supply ● module; Connect the laser cable to the connector TO LASER HEAD of the power supply ●...
  • Page 41 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation Alignment of the system laser-objective 1. Set a white screen at the back of the positioning stage perpendicular to the laser beam (Fig. 3-17). 2. The center of laser projection spot on the screen should be straight above the guide groove of the positioning stage (Fig.

  • Page 42: Preparation And Installation Of The Optical Fiber In The Laser Module

    NTEGRA Solaris Probe NanoLaboratory Installation of the fiber mounting stage 1. To install the fiber mounting stage, turn the stage fastening screws so that their cut-off flanges face each other (Fig. 3-20). Fig. 3-20 Fig. 3-21 2. Set the fiber mounting stage on the movable part of the positioning stage (Fig. 3-21).
  • Page 43 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation To load the optical fiber into the laser module, perform the following steps: 1. Take off the magnetic fasteners from the fiber mounting stage 2 (Fig. 3-24). 2. Load the fiber into the groove of the fiber mounting stage so that its end comes out from the edge of the mounting stage by 3†4 mm (Fig.

  • Page 44: Loading The Sample

    NTEGRA Solaris Probe NanoLaboratory 3.6. Loading the Sample To load the sample, perform the following steps: 1. Prepare the sample for measurement. To do that, place the sample on a substrate and (if necessary) fix it. 2. Place the substrate on the sample stage 1 of the scanning mount (Fig. 3-26).
  • Page 45 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation Fig. 3-27. Measuring head seated on the scanning mount 1 – measuring head positioning screws; 2 – micrometer screws of the XY positioning device 2. In the case of measurements on the transmission mode, get the probe into the field of vision of the scanning mount objective by using the measuring head positioning screws 1 (Fig.

  • Page 46: Assembly Of Optical Scheme For Transmission Mode

    NTEGRA Solaris Probe NanoLaboratory 3.8. Assembly of Optical Scheme for Transmission Mode Optical measurements on transparent samples are performed using the transmission mode. An overall view of the transmission mode is shown in Fig. 3-28. NOTE. The objective should be installed into the scanning mount before installation of the sample and preparations for operating on the “transmission mode”...
  • Page 47 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation The preparation procedure for operation on the “transmission mode” optical scheme requires the following steps: 1. Switch the optical path selector 6 (Fig. 3-29) to the position “only port” (pictogram NOTE.
  • Page 48 NTEGRA Solaris Probe NanoLaboratory ATTENTION! Close the shutter of the photomultiplier module before installing it. 6. Switch the controller off (if it has been on). Connect the photomultiplier module with the connector EXTENSION of the controller. 7. Switch the selector of the microscope optical path (Fig. 3-30) into the position “trinocular”...

  • Page 49: Assembly Of Optical Scheme For Reflection Mode

    Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation Fig. 3-31 Preparation for operation on the “transmission mode” optical scheme is completed. 3.9. Assembly of Optical Scheme for Reflection Mode Optical measurements on non-transparent samples are performed using the reflection mode.
  • Page 50 NTEGRA Solaris Probe NanoLaboratory Fig. 3-33. Measuring head with the optical attachment During measurements, the attachment diverts the reflected light, which contains the information on properties of the sample, to the built-in optical system. The photo detector, then, acquires this light.
  • Page 51 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation Fig. 3‑35 3. Mount the optical attachment on the measuring head by securing it with fixing screws of the support rods (Fig. 3‑36). Fig. 3‑36 4. Emplace the screw legs (Fig. 3‑37).
  • Page 52 NTEGRA Solaris Probe NanoLaboratory Fig. 3‑37 Preparations for operations on the “reflection mode” optical scheme require the following steps: 1. Watching the probe tip through the orifice 2 (Fig. 3-38), set it at the center of this orifice using the micrometer screws 1.
  • Page 53 Chapter 3. Preparation of the NTEGRA Solaris PNL for Operation 5. Select an area for measurement by moving the sample using the micrometer screws 3 3 (see Fig. 1-4). Control this procedure using the monitor. 6. Take the microscope aside. ATTENTION! Close the shutter of the photomultiplier module before installing it.

  • Page 54: Measurement Procedure

    NTEGRA Solaris Probe NanoLaboratory 4. Measurement Procedure As it has been pointed out in item on page 5, NTEGRA Solaris can perform measurements using several measurement techniques. Those are the Shear Force Microscopy (ShFM) technique and the techniques of Scanning Near-field Optical...

  • Page 55: Loading Scanner Calibration Parameters

    Chapter 4. Measurement Procedure 2. In the Main Parameters panel, select the controller configuration from the drop-down list (Fig. 4‑2): – for the Reflection Mode. Besides, the configuration can be SNOM1 SNOM1 selected for the Transmission mode if the Z-lens will not be used. If is selected, both voltages applied to the PMT on the optical SNOM1 microscope (PMT1) and applied to the PMT on the measuring head...
  • Page 56 NTEGRA Solaris Probe NanoLaboratory Fig. 4-3 This will open a dialog box with a list of par-files contained in the PARFiles folder. 2. Choose the par-file corresponding to the installed scanner. The par-files are named by numbers of the scanners.

  • Page 57: Setting Of The Photomultiplier Module Parameters

    Chapter 4. Measurement Procedure If you prefer the current scanner parameters to load by default at the program start-up save the file as Default.par. Proceed as follows: 1. In the Main menu select the items: → → Settings Calibrations Save Calibrations (Fig.
  • Page 58 NTEGRA Solaris Probe NanoLaboratory 2. To operate with the photomultiplier module, it is required to visualize the laser signal, which is acquired by the photomultiplier module, on the oscilloscope. To do that: a. Switch to the addition operations area by clicking the button located in the top right corner of the Main Window.

  • Page 59: Search For Resonance Frequency

    Chapter 4. Measurement Procedure 4.4. Search for Resonance Frequency Unlike the cantilever type probes, the probes of the quartz resonator type always have fixed resonance frequencies: one is located near 33 kHz and another is near 190 kHz. The optimal operating frequency depends on a number of parameters (individual properties of the probe, properties of the sample, specifics of scanning etc).
  • Page 60 NTEGRA Solaris Probe NanoLaboratory Set the generator output signal phase, , equal to 0; Phase ○ Leave the generator output signal frequency, , with no change (as set Frequency ○ by default). c. On the panel of parameters of the synchronous detector...
  • Page 61 Chapter 4. Measurement Procedure c. On the panel of parameters of the synchronous detector (Fig. 4-10): Lock-In Set cutoff frequency equal to 1 kHz. Low Pass ○ Set the gain coefficient of the synchronous detector equal to 10. Gain ○ Set the DFL signal at the input of the synchronous detector with the gain ○...

  • Page 62: Probe Landing

    NTEGRA Solaris Probe NanoLaboratory 4.5. Probe Landing 1. Define value of to be at least 1 (Fig. 4‑12). FB Gain Fig. 4‑12. Main Parameters Panel 2. Verify that the level is 12. Define the value slightly more than the Tune_Fork Set Point level.
  • Page 63 Chapter 4. Measurement Procedure 7. Trigger the landing procedure (button Wait till the end of the landing procedure. A record «…Approach Done» appears in the journal in the right part of the control panel on its completion (Fig. 4-14). Fig. 4-14. Message on the completion of the landing procedure After landing, noise generations might be induced in the feedback loop (Fig.

  • Page 64: Scanning

    NTEGRA Solaris Probe NanoLaboratory 4.6. Scanning 4.6.1. Setting of Scanning Parameters To perform measurements, select a scanning technique appropriate for your specific problem. To read surface topography, use the ShFM method. SNOM methods are used to obtain data on optical properties of the sample. Setting of parameters of scanning depends on the method selected for measurement.
  • Page 65 Chapter 4. Measurement Procedure Fig. 4-18. Dialog box Scan Setup Near-field Optical Microscopy 1. Open the window of scanning parameters (bookmark Scan on the panel of main operations). 2. Select the option SNOM transmission, from the menu Mode (scanning modes) of the panel of scanning parameters (Fig.

  • Page 66: Triggering Of Scanning

    NTEGRA Solaris Probe NanoLaboratory 4. Click the button . A dialog box, (Fig. 4-21), will appear. Set Scan Setup as signals for measurement. Height PMT1_Transmission Fig. 4-21. Dialog box Scan Setup 4.6.2. Triggering of Scanning Switch the selector of the microscope optical path (see Fig. 3-30) into the position “side port”...

  • Page 67: Methods Of Improving Image Quality

    Chapter 4. Measurement Procedure In the case of SNOM scanning, the monitor will display two windows. One of the windows will visualize the signal (Fig. 4-23 a), while the other window will visualize Height (Fig. 4-23 b). Fig. 4-23. Surface image a) ShFM –...

  • Page 68: Saving Of Measurement Results

    NTEGRA Solaris Probe NanoLaboratory Noise generation in the process of scanning It is recommended to set the value of gain coefficient to be 0.5†0.7 of the value FB Gain where the noise generation is beginning to affect the signal . At the same time with taking this measure, the value of scanning velocity should also be reduced to 0.5†0.7 of the...
  • Page 69 Chapter 4. Measurement Procedure b. Double-click in the text box (Fig. 4-25) of the control panel Moving Backward of the tab . Set the value 2†3 mm using the slider. Approach Fig. 4-25 c. Take the probe away from the sample by clicking the button Fast Backward (Fig.

  • Page 70: Maintenance

    NTEGRA Solaris Probe NanoLaboratory 5. Maintenance One-month maintenance for sensors is recommended. If calibration of sensors stays valid for a month, then check calibrations once for 6 months. If settings of either of the sensors are incorrect, perform the following: 1.
  • Page 71 Chapter 5. Maintenance Closed-Loop Fig. 5-1. 6. Adjust the X-scanner in the middle of the scan range by clicking the button and place the slider in the middle of the range (Fig. 5-2); Move X Fig. 5-2 7. Close the XY feedback by clicking the button.
  • Page 72 NTEGRA Solaris Probe NanoLaboratory Fig. 5-3. HV-X signal for the 50-m scanner. Fig. 5-4. HV-X signal for 50-m scanner. Top of Adjustment of the scanner is unnecessary the saw-tooth signal is cutoff. The scanner should be adjusted Adjusting the displacement sensors 1.

  • Page 73: Scanner Calibration

    Chapter 5. Maintenance 2. Check the sensor signal with the oscilloscope signal . The signal should be in X Sensor the range of ±5 V and be of regular triangular shape (Fig. 5-6). X Sensor signal for Fig. 5-6. 50-m scanner at proper adjustment of the sensors Saving the adjustment coefficients To save the calibration results in a par-file, perform the following steps: 1.
  • Page 74 NTEGRA Solaris Probe NanoLaboratory 2. Find the average period of the grating in the ХY-directions using the Image Analysis software. Proceed as follows: a. Switch to the Data tab. The last scan image is displayed in the Frame View and Modification window.

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