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NT-MDT NTEGRA Spectra Instruction Manual

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  • Page 1 NTEGRA platform NTEGRA Spectra Instruction Manual SNOM Measuring Head www.ntmdt-si.com...
  • Page 3 NTEGRA Spectra Probe NanoLaboratory SNOM Measuring Head Instruction Manual 2010 - 2018, Copyright © NT-MDT SI NT-MDT Spectrum Instruments Proezd 4922, 4/3 Zelenograd, Moscow 124460, Russia Tel.: + 7 (499) 110-2050 www.ntmdt-si.com...
  • Page 5 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 7 User’s documentation set The following manuals are included into the user’s documentation set: - Instruction Manual – is the guidance on 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 depending on the delivery set of the instrument.

  • Page 9: Table Of Contents

    Table of Contents NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Table of Contents 1. BASIC INFORMATION ......................... 2 1.1............................2 VERVIEW 1.2......................... 2 RINCIPLE OF PERATION 1.3.............................. 4 ESIGN 1.3.1. Optical Measuring Head ....................5 1.3.2.

  • Page 10: Basic Information

    SNOM measuring head used with the NTEGRA Spectra PNL (Upright configuration) operates in the optical scheme of the Transmission Illumination Mode, which is used for transparent or semitransparent samples. For details on design and operation of the PNL, refer to manual NTEGRA Spectra Probe NanoLaboratory (Upright Configuration with Renishaw Spectrometer)
  • Page 11 Chapter 1. Basic Information Fig. 1-1. Transmission Illumination Mode The primary laser beam is focused by the objective on the probe aperture. The sample surface stays as close to the probe as to be in the near field of the aperture. Radiation emitted by the aperture and scattered by the sample is collected with the optical system and directed to the PMT detector.

  • Page 12: Design

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 1.3. Design Fig. 1-2 shows the delivery set of the SNOM measuring head: − Optical measuring head; − Probe holder. Fig. 1-2. SNOM measuring head 1 – measuring head; 2 – probe holder Fig.

  • Page 13: Optical Measuring Head

    Chapter 1. Basic Information Fig. 1-3. Parts of the SNOM module 1 – replaceable panel; 2 – optical tube; 3 – positioning device; 4 – laser beam delivery system KineFlex;5 – PMT module; 6 – hollow sample holder; 7 – set of substrates; 8 – fixing screws 1.3.1.
  • Page 14 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Basic parts of the measuring head are shown in Fig. 1-5. Fig. 1-5. Measuring head 1, 2 – screws for XY probe adjusting; 3, 4 – photodiode mirror adjusting screws; 5 –screw for fine focusing of the lens; 6, 7 –screws for XY lens adjusting;...
  • Page 15 Chapter 1. Basic Information provides a wide spectral range (400 <λ < 800 nm for the laser with λ =830 nm) thus allowing for observing the sample through the optical microscope and for optical exciting the sample surface. High sensitivity of the detection system is due to a special design of the laser formation system.
  • Page 16 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual a) triangular cantilever b) triangular cantilever Fig. 1-6. AFM probe 1 – chip; 2 – cantilever; 3 – tip (sensitive element) The aperture probe tip is a hollow pyramid with a hole at its apex that serves as aperture (Fig.

  • Page 17: Optical Tube

    Chapter 1. Basic Information Fig. 1-9. Fastening magnet for mounting the aperture probe The aperture probe holder is placed in the mount of the measuring head and then secured with the spring stop 1 (see Fig. 1-10). The screws 2 and 3 serve to move the probe holder for adjusting the optical cantilever deflection detection system.
  • Page 18 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Fig. 1-11. Optical tube Diagram of the optical tube is shown in Fig. 1-12. For measurements, the sample surface is located in the focal plane of the lens 1. The reflecting prism 2 redirects the laser beam to the objective for delivering radiation to the tube or to the laser beam delivery system for collecting the transmitted radiation.

  • Page 19: Laser Beam Delivery System

    Chapter 1. Basic Information The screws 1, 2, and 3 provide displacement of the optical tube in the ranges of 11 mm for corresponding degrees of freedom. The supporting bracket 4 is screwed on the replaceable panel of the base unit thus fixing the positioning device.

  • Page 20: Photomultiplier Module

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 1.3.4. Photomultiplier Module Photomultiplier module (PMT module) (Fig. 1-16) serves for converting optical radiation acquired from the sample into electrical signals. Fig. 1-16. PMT module  ATTENTION! The photomultiplier is highly sensitive to light. Never illuminate the PMT (even when it is off) with high intensity to prevent its damage or degradation.

  • Page 21: Basic Safety Measures

    − Ground the instrument before operation! − Do not disassemble any part of the device. Disassembling of the product is permitted only to persons certified by NT-MDT Spectrum Instruments. − Do not connect additional devices to the instrument without prior advice from an authorized person from NT-MDT Spectrum Instruments.
  • Page 22 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 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 23: Operating Conditions

    Chapter 1. Basic Information 1.5. Operating Conditions To provide for the normal operation of the device, it is recommended to observe the following conditions: − (25 ± 10) °C; environment temperature: − temperature drift less than 1 °C per hour; −...

  • Page 24: Storage And Transport Instructions

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual − the measuring unit of the instrument (the base unit with the measuring head) should be placed on a separate table away from computers and monitors, to eliminate electromagnetic interference; −...

  • Page 25: Assembling Of The Snom Module

    Chapter 2. Assembling of the SNOM Module 2. Assembling of the SNOM Module Before assembly, the PNL should be prepared for operation and interconnections of all electromechanical parts are done. Make sure that the controllers, the spectral unit< and the laser source are off. Assembly of the SNOM module and its installation on the base unit of the PNL include the following procedures: 1.

  • Page 26: Mounting The Optical Tube

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual M4×16 screws (pos. 2 in Fig. 2-2) with Allen key wo fix the panel on the exchangeable mount. Fig. 2-2. Replaceable panel mounted on the base unit 1 – screws for fastening to the base unit; 2 – screws for fastening to the exchangeable mount This completes mounting the replaceable panel on the base unit.
  • Page 27 Chapter 2. Assembling of the SNOM Module Approach knob Fig. 2-5. Approach knob of the base unit c. Connect the scanner to the base unit: - When using a scanner with sensors, connect the scanner slot to the SCAN+SENSOR located on the base unit. - When using a scanner without sensors you may connect the scanner SCANNER SCAN+SENSOR...
  • Page 28 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 3. Mount the positioning device with the optical tube on the base unit as follows: a. Loosen nuts of the guide pins 1 (Fig. 2-7). Fig. 2-7. Positioning device 1 – nuts for fastening the guide pins; 2 – guide pins;...

  • Page 29: Mounting The Laser Beam Delivery System

    Chapter 2. Assembling of the SNOM Module Fig. 2-9. Optical tube mounted on the base unit 1 – X movement screw; 2 – Y movement screw 4. Tighten two nuts of the guide pins (pos. 1 in Fig. 2-7) with hexagonal box wrench. Fixing the guide pins enables the positioning device to take its initial state if it is remounted on the base unit.
  • Page 30 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Fastening screws Input Fig. 2-10. LBDS socket mounted Input 2. Secure the socket by screwing two fastening screws with Allen key 1.5 mm (Fig. 2-10). 3. Close the laser source exit shutter if it is open.

  • Page 31: Preparing For Operation

    Chapter 3. Preparing for Operation 3. Preparing for Operation  ATTENTION! Familiarize with the manual NTEGRA Spectra Probe NanoLaboratory (Upright Configuration) before starting operation with the SNOM measuring head. Preparation of the instrument for operation includes the following operations: 1. Preparing and Installing the Aperture Probe (sect. 3.2 on p. 26).
  • Page 32 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 3. Put the sample on the adhesive tape and carefully press it with tweezers in several places (not touching the area intended for the investigation).  NOTE. After the sample is fixed on the substrate, a noticeable vertical drift of the sample can occur within one hour (due to the slow relaxation of sticky tape).
  • Page 33 Chapter 3. Preparing for Operation Fig. 3-4. Sample holder installed on the scanner This completes installing the sample. Setting the sample height The sample thickness influences the geometrical dimensions of the acquired image. With the same elongation of the scanner tube, a thicker sample will move to a larger distance from the probe in the XY plane (Fig.

  • Page 34: Preparing And Installing The Aperture Probe

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Sample Height 2. In the input field of any of the tabs enter the sample height (Fig. 3-6). - If the substrate is of the same thickness as that of calibration, enter thickness of the sample itself.
  • Page 35 Chapter 3. Preparing for Operation 2. Place the support on a clean smooth surface with its protrusion up. 3. Apply a small amount of glue on the support protrusion. Use epoxy resin or cyanocrylate glue for sticking. 4. Take the probe from the container with the tweezers. Make sure that the working side of the chip with cantilevers is directed to you during the installation.

  • Page 36: Installing The Probe Holder

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 3.3. Installing the Probe Holder To install the probe holder on the measuring head, perform the following steps: 1. Place the measuring head with its bottom up on a plane surface.
  • Page 37 Chapter 3. Preparing for Operation Fig. 3-12 1 – approach knob; 2 – seats of the measuring head 2. Place the screw legs of the measuring head down to the seats 2 of the exchangeable mount (see Fig. 3-13). Observe that the probe tip does not contact with the sample surface or with parts of the microscope.

  • Page 38: Preliminary Approaching And Selecting Scan Area

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 3. Tuck in the head cable into the cable holder. Connect the measuring head to the HEAD socket in the base unit of the instrument. This completes installing the measuring head.

  • Page 39: Primary Adjusting The Detection Channel

    Chapter 3. Preparing for Operation 3.6. Primary Adjusting the Detection Channel Primary adjusting serves for aligning the sample surface with the focal plane of the lens. This procedure needs the sample to approach the probe to distance of 0.5 mm. Proper focus of the lens on the sample surface is required for efficacy of collection and detection of radiation transmitted through the sample.
  • Page 40 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Fig. 3-16. Screws for moving the optical tube 1 – X movement screw; 2 – Y movement screw; 3 – Z movement screw 5. Focus the laser beam on the sample surface by moving the optical tube along Z with the screw 3 (Fig.

  • Page 41: Launching The Control Program

    This completes primary adjusting the detection channel. 3.7. Launching the Control Program Before this procedure, all interconnections of electromechanical units of the instrument are to be done according to the manual NTEGRA Spectra Probe NanoLaboratory (Upright Configuration with Renishaw Spectrometer). ...

  • Page 42: Adjusting The Optical Cantilever Deflection Detection System

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 3.8. Adjusting the Optical Cantilever Deflection Detection System Adjusting the optical cantilever deflection detection system can be performed in one of two ways: − by the spotlight from the illuminator; −...
  • Page 43 Chapter 3. Preparing for Operation the optical viewing system (Fig. 3-21). Here, the bright portion corresponds to the edge of the probe chip while dark areas display the chip surface and the sample surface which are out of focus of the objective. Fig.
  • Page 44 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 5. Focus the objective on the cantilever by turning the screw 3 (Fig. 3-19). Watch quality of the focusing on the monitor of the optical viewing system. 6. Move the probe in the XY plane to a position at which the bottom of the tip is viewed slightly below the center of the monitor (Fig.
  • Page 45 Chapter 3. Preparing for Operation Fig. 3-26. Spot of the detection system laser on the cantilever 9. For fine aiming the laser beam at the end of the cantilever, use adjusting the total signal of the photodiode. With laser positioning screws 1 and 2, move the beam a Laser little against the cantilever and find the position at which the total signal ( ) is at...

  • Page 46: Performing Measurements

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 4. Performing Measurements Initial state Before measurements, components of the instrument should be prepared as follows: 1. Control program is running; 2. Instrument is on; 3. Probe is installed; 4. Sample is installed;...

  • Page 47: Approaching The Sample And Fine Adjusting The Detection Channel

    Chapter 4. Performing Measurements 4.1. Approaching the Sample and Fine Adjusting the Detection Channel Approaching the sample to the probe Perform approaching the sample to the probe according to the procedure of contact AFM. For details, refer to manual NTEGRA Probe NanoLaboratory. Performing measurements, Part 3.

  • Page 48: Adjusting The Delivery Channel

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual 3. Focus the objective on the sample surface by rotating the screw 3 (Fig. 4-1). Watch the surface image on the monitor of the optical viewing system. 4. Open the laser exit shutter. The laser beam will go through the LBDS and the optical tube and come to the sample.
  • Page 49 Chapter 4. Performing Measurements Arranging the optical scheme of the Transmission Collection Mode Output 1. Remove the socket from the radiation feedthrough. To this purpose, press and hold the backing-up screw of the feedthrough with your left had (Fig. 4-3) and pull Output socket with your right hand.
  • Page 50 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Fig. 4-5. Image of the laser spot focused on the sample surface Aligning the laser beam with the focus of the detection system Spectra 1. Go to the tab in the Main window of the Nova program. This runs the auxiliary version of the Nova program.
  • Page 51 Chapter 4. Performing Measurements a. In the drop-down list of the Main Parameters panel, select PMT1 (Fig. 4-7). Fig. 4-7  ATTENTION! When using the PMT module, monitor level of the Ext2 PMT output ( signal) on the oscilloscope. At level >5 V, the PMT may be damaged.
  • Page 52 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual  NOTE. The optimal level (in modulus) of the PMT output for measurements is 1 V. Higher output results not only in direct raise of the noise level RMS but also in heating the PMT module that contributes to noise.
  • Page 53 Chapter 4. Performing Measurements Fig. 4-10. Intensity distribution of the detected signal The dark region in the acquired image corresponds to the light-transmitting region of the optical tube, that is, light coming to this region will be detected by the PMT module.
  • Page 54 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Aligning the probe aperture with the focus of the laser beam 1. Turn the turret to the position M2 (no reflection applied). The laser beam will not illuminate the sample and the image of the sample on the monitor of the optical viewing system will be formed by ambient light.

  • Page 55: Scanning

    Chapter 4. Performing Measurements Tuning the photodiode position With the delivery channel adjusted, align the photodiode as follows: Aiming 1. Switch to the tab with the button in the Main Operations panel. 2. Rotate the photodiode positioning screws 4 and 5 (Fig. 4-12) to place the laser spot position indicator at the center of the photodiode indicator (Fig.
  • Page 56 NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Tuning position of the laser beam 1. In the Auxiliary Operations Area (accessible through the button at the right top of Scheme the Program window), select the tab to open the block scheme.
  • Page 57 Chapter 4. Performing Measurements Fig. 4-16. Arrow indicates position of the maximal intensity of the laser signal 7 With the laser beam aimed at the center of the aperture, the monitor of the optical viewing system will display the distinct image of the laser spot with rays radiating in vertical and in horizontal (Fig.

  • Page 58: Saving Data

    NTEGRA Spectra Probe NanoLaboratory. SNOM Measuring Head. Instruction Manual Scan 2. Switch to the tab by clicking the button in the Main Operations panel to activate scanning-by-sample. Open the scanning parameters window by clicking the button. Select the following detection signals for the forward pass: for ADC#1 –...

  • Page 59: Finishing The Work

    Chapter 4. Performing Measurements 4.5. Finishing the Work 1. Open the feedback loop by releasing the button. 2. Retract the sample from the probe as follows: Approach a. Go to the tab with the button in the Main Operations panel. Moving Backward b.

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