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NT-MDT NTEGRA Therma Instruction Manual

Probe nanolaboratory configuration with variable temperature assembly for thermal measurements
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NTEGRA Therma
Probe NanoLaboratory
Configuration with Variable
Temperature Assembly for Thermal
Measurements (SFT03NTF+SCC09NTF)
Instruction Manual
16 October 2009
Copyright © NT-MDT
Web Page:
http://www.ntmdt.com
General Information:
spm@ntmdt.ru
Technical Support:
support@ntmdt.ru
NT-MDT Co., building 1 ,
Zelenograd, 1244 , Moscow, Russia
Tel.: +7-499-735- -
Fax: +7-499-735-64-10

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  • Page 1 Configuration with Variable Temperature Assembly for Thermal Measurements (SFT03NTF+SCC09NTF) Instruction Manual 16 October 2009 Copyright © NT-MDT Web Page: http://www.ntmdt.com General Information: spm@ntmdt.ru Technical Support: support@ntmdt.ru NT-MDT Co., building 1 , Zelenograd, 1244 , Moscow, Russia Tel.: +7-499-735- - 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 measuring head (Fig. 1), laser sources. Fig.
  • 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 Therma Probe NanoLaboratory. Instruction Manual NTEGRA Therma Probe NanoLaboratory. Instruction Manual Table of Contents 1. SYSTEM DESIGN ........................... 5 1.1..................... 6 THERMAL XCHANGEABLE OUNT 1.2........................12 EGISTRATION 2. BASIC SAFETY MEASURES ......................13 3. OPERATING CONDITIONS ....................... 15 4.

  • Page 5: System Design

    − SPM controller; − thermocontroller; − computer. A general view of NTEGRA Therma for variable temperature thermal measurements is given in Fig. 1-1. Fig. 1-1. NTEGRA Therma 1 – base unit, 2 – optical viewing system; 3 – vibration isolation system;...

  • Page 6: Vt Thermal Exchangeable Mount

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual The desing of Ntegra Therma main units is discussed in the books «Performing Measurements» and «Control Electronics». The features of configuration for wide-range temperature measurements are described below. Specifications Parameter Value Temperature range from -30°C up to +80°C Stability of temperature maintenance 0.005°C typically...
  • Page 7 Chapter 1. System Design The main parts of the VT thermal exchangeable mount include the temperature chamber, the heat exchanger, the scanner and the approach mechanism. The temperature chamber is made of copper, thus the temperature variation within the chamber does not exceed one degree after the working temperature has been settled. All other metal parts of the thermal scanner that have strong effect on the thermal drift are made of invar.
  • Page 8 NTEGRA Therma Probe NanoLaboratory. Instruction Manual Fig. 1-4. Temperature chamber 1 – sample holder; 2 – supporting ring; 3 – clamps; 4 – Peltier modules; 5 – Peltier modules heat exchanger Peltier modules 4 maintain working temperature of the chamber during measurements.
  • Page 9 Chapter 1. System Design Configuration А Configuration В Fig. 1-5. Connecting the liquid temperature control system Port 3, 4 (Fig. 1-5) are connected with the cooling system of the Peltier modules. Port 2 and port 1 are attached to the scanner heat exchanger. When using configuration А, the hoses of the liquid temperature control system should be connected to ports 3 and 4.
  • Page 10 NTEGRA Therma Probe NanoLaboratory. Instruction Manual Approach mechanism The design of the approach and scanning mechanisms is shown in Fig. 1-6. Fig. 1-6. Approach mechanism 1 – sample holder; 2 – rod; 3 – beam; 4 – substrate with a sample; 5 – hollow lever;...
  • Page 11 Chapter 1. System Design Approach When engaging the sample, approach mechanism lever 11 is moving upwards pushing the rod. Thus spring 10 is compressing. The beam is raising sample holder 1. During withdrawal lever 11 is moving downwards, the spring is releasing lowering rod 2 and the beam is pulling the sample holder downwards.

  • Page 12: Registration Head

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 1.2. Registration Head The main parts of the registration head design are presented in Fig. 1-7. The system for detecting the cantilever deflections and the piezodriver are inside the head. a) general view b) bottom view 1 –...

  • Page 13: 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. - Do not connect additional devices to the instrument without prior advice from an authorized person from NT-MDT.
  • Page 14 NTEGRA Therma Probe NanoLaboratory. 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 (Fig. 2-2), laser sources.

  • Page 15: Operating Conditions

    Chapter 3. Operating Conditions 3. Operating Conditions To provide for the normal operation of the device, it is recommended to observe the following conditions: - environment temperature: 20 ±5˚C; - temperature drift less than 1˚C per hour; - relative humidity less than 80%;...

  • Page 16: Storage And Transport Instructions

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 4. Storage and Transport Instructions Storage Instructions The instruments should be stored packaged in clean and dry premises with low ambient temperature variations: - Acceptable temperature inside the premises is plus (20 ± 10) °C;...

  • Page 17: Setup And Installation

    Chapter 5. Setup and Installation 5. Setup and Installation 5.1. Interface Board Installation Normally the control PC is supplied with the pre-installed interface board. If the control PC is supplied separately, the interface board can be installed by either a certified installation engineer or by the customer.

  • Page 18: Installation Of The Vt Thermal Exchangeable Mount

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 5.3. Installation of the VT Thermal Exchangeable Mount Remove the exchangeable mount. To do this: 1. Loosen retaining screw 1 (see Fig. 5-1). Fig. 5-1 1 – retaining screw; 2 – approach knob; 3 – exchangeable mount fixing screws 2.
  • Page 19 Chapter 5. Setup and Installation Install the VT thermal exchangeable mount. Proceed as follows: 1. Insert the VT thermal mount in the aperture (Fig. 5-3) of the base unit. The guides (see pos. 1 in Fig. 5-4) of the VT thermal mount shall fall into corresponding holes 2 of the base unit.
  • Page 20 NTEGRA Therma Probe NanoLaboratory. Instruction Manual 2. Use the three screws (see pos. 2 in Fig. 5-6) to fix the VT thermal mount to the base unit. Fig. 5-6. The VT thermal mount fixed in the base unit 1 – retaining screw, 2 – VT thermal exchangeable mount fixing screws 3.
  • Page 21 Chapter 5. Setup and Installation Fig. 5-8. Adapter 1, 2 – short tubes to be connected to the temperature mount; 3, 4 – long tubes to be fitted to the liquid-cooling system 6. Remove the round cap to the left of the exchangeble mount. 7.
  • Page 22 NTEGRA Therma Probe NanoLaboratory. Instruction Manual 9. Connect the temperature stage to the liquid-cooling (temperature control) system. Depending on the design of the temperature-stabilization system two configurations are available (Fig. 5-11): a. Configuration А - for a liquid-cooling system without precision stabilization: Connect the inlet and the outlet of the liquid temperature control system with ports 3 and 4.

  • Page 23: Cable Connections

    Chapter 5. Setup and Installation 5.4. Cable Connections Connect separate instrument units according to the diagram given in Fig. 5-12. All connections are made according to the labels on the plugs. ATTENTION! Before connecting of disconnecting any parts of the instrument power off the controllers.

  • Page 24: Powering Sequence

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 5.5. Powering Sequence Switching on 1. Turn the computer on. 2. Start up the program using one of the options below: − By clicking the program icon available from the computer desktop; − By launching the file NOVA.exe available from the program folder.
  • Page 25 Chapter 5. Setup and Installation Completion 1. Disable the feedback loop (button 2. Switch off the SPM controller and the thermocontroller. 3. Switch off the temperature control unit. 4. Turn the vibration protection system off. 5. Close the control program.

  • Page 26: Preparation For Operation

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 6. Preparation for Operation Preparation and operation procedures for NTEGRA Therma include the following basic operations: 1. Sample Installation (see i. on page 26). 2. Probe Installation (see i. on page 27). 3. Registration Head Installation (see i.

  • Page 27: Probe Installation

    Chapter 6. Preparation for Operation 4. Install the substrate with a sample on the sample stage using tweezers (see Fig. 6-2). Use invar substrates supplied with the instrument. Substrates are secured on the sample stage by the magnetic clamp. ATTENTION! When applying the sample-heating feature use only invar substrates.
  • Page 28 NTEGRA Therma Probe NanoLaboratory. Instruction Manual 4. Place the probe to the holder (cover) and move it to touch the sidewall stops (Fig. 6-4). sidewall stops Fig. 6-4. Probe installation 5. Grip the spring clamp with tweezers near its top arm (Fig. 6-5), slightly raise it and move to fix the probe.

  • Page 29: Registration Head Installation

    Chapter 6. Preparation for Operation 6.3. Registration Head Installation 1. Install the registration head with its supports resting on the seats of the VT thermal mount (Fig. 6-9). The head shall firmly rest on the three supports without rocking. Measuring head cables holder Fig.

  • Page 30: Preparation Of The Optical Viewing System For Operation

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 6.4. Preparation of the Optical Viewing System for Operation To adjust the optical viewing system, proceed as follows: 1. Loosen the screws on rack 1 (see Fig. 6-10) and pull bar 2 upwards on 40-50 mm. If the bar was accidentally lifted more than 70 mm, lower it so that the alignment pin sets in the guide groove on the bar.

  • Page 31: Adjustment Of The Optical System For Detecting Cantilever Deflections

    Chapter 6. Preparation for Operation 6.5. Adjustment of the Optical System for Detecting Cantilever Deflections To adjust the optical system perform the following procedures: 1. Run the control program. ATTENTION! When working with the thermal scanner the program shall be started first and then the thermocontroller shall be switched on. 2.

  • Page 32: Selecting Region To Scan

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual Fig. 6-12 5. Use the laser positioning screws to obtain maximum Laser signal. 6. Turning the positioning photodiode screws adjust the values of the DFL and LF signals close to zero. 7. Re-adjust the Laser signal. The value of the Laser signal shall be around 5÷10 nA.
  • Page 33 Chapter 6. Preparation for Operation To move the sample proceed as follows: 1. Open the Approach window. With the thermocontroller powered on, the thermal approach panel appears in the right part of the control panel in the Approach window (Fig. 6-14). Fig.
  • Page 34 NTEGRA Therma Probe NanoLaboratory. Instruction Manual The following parameters can be specified in this window: X Movement – sample displacement along the X-axis; Y Movement – sample displacement along the Y-axis; Up/Down Movement –sample displacement along the Z-axis. 8. In the Up/Down Movement input box enter the value of Way.
  • Page 35 Chapter 6. Preparation for Operation c. The stepper motor raises the sample holder. The substrate fixes in the new position (Fig. 6-17 c). d. The piezotube deflects in the opposite direction (Fig. 6-17 d). e. Then the cycle repeats until the sample has moved on the specified distance. Fig.

  • Page 36: Performing Measurements

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 7. Performing Measurements 7.1. Contact AFM The measurements by the AFM-techniques are discussed in detail in the book “Performing measurements” Part 3, Chapter 2, Section “Constant Force Mode”. Hence, only a sequence of main operations and a detailed description of the stages which differ from the standard procedure are given here.
  • Page 37 Chapter 7. Performing Measurements 2. Click the button on the thermal approach panel to turn on the approach mode (see Fig. 7-2). 3. Set the parameters of thermal approach (see Fig. 7-2). Fig. 7-2. Thermal approach panel During the initial approach it is recommended to set the following values: −...
  • Page 38 NTEGRA Therma Probe NanoLaboratory. Instruction Manual 6. Click the OK button to save the modifications. 7. Turn on the software oscilloscope by selecting the Height signal for registration. 8. Start the approach procedure by clicking the Landing button. Using the oscilloscope graph make sure that during each approach cycle the scanner piezotube has enough time to extract and retract to its full scan range on Z (Fig.

  • Page 39: Setting "Feedback Gain" Factor Working Level

    Chapter 7. Performing Measurements 7.1.2. Setting “Feedback Gain” Factor Working Level Для устойчивой работы рекомендуется устанавливать уровень коэффициента усиления не более 0.5÷0.7 от порогового значения, при котором начинается генерация. Регулировка коэффициента усиления производится в поле ввода FB Gain на панели основных параметров. A detailed discussion of the procedure for setting the working level of the feedback gain is given in the book «Performing measurements», Part 3, Chapter 2, Section «Constant Force Technique».
  • Page 40 NTEGRA Therma Probe NanoLaboratory. Instruction Manual 8. Click on the tool bar to start plotting the temperature curve (Fig. 7-16). Fig. 7-6 9. Start the software oscilloscope and select SensorHeight signal for display. Fig. 7-17 and Fig. 7-18 show the temperature curve and SensorHeight variation when cooling the sample from 24°...

  • Page 41: Setting The Scanning Parameters And Scanning

    Chapter 7. Performing Measurements 7.1.4. Setting the Scanning Parameters and Scanning Setting the scan parameters (selection of a SPM-method, choosing scan region and scan speed) and scanning are similar to operation at normal conditions. A detailed description is given in the book (“Performing measurements”), Part 3, Chapter 2, Section «Constant Force Mode».

  • Page 42: Semicontact Afm

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 7.2. Semicontact AFM The measurements by the AFM-techniques are discussed in detail in the book “Performing measurements”, Part 3, Chapter 3, Section “Semicontact Mode”. Hence, only a sequence of main operations and a detailed description of the stages which differ from the standard procedure are given here.

  • Page 43: Landing The Sample To The Probe

    Chapter 7. Performing Measurements Setting Mag Signal Initial Level The resonance amplitude of the Mag signal should be about 10 nA. Setting “Feedback Gain” Factor Working Level The working level of FB Gain shall be about 0.1. NOTE. For detailed description refer to the book “Performing measurements”, Part 3, Chapter 3, Section “Semicontact Mode”.
  • Page 44 NTEGRA Therma Probe NanoLaboratory. Instruction Manual 4. Open the Landing Settings dialog box by clicking the button (Fig. 7-13). Fig. 7-13. Landing Settings dialog box 5. Set the following parameters for the stepper motor (see Fig. 7-13): Forward panel: BackZ = 70;...
  • Page 45 Chapter 7. Performing Measurements Fig. 7-14 Once the landing is finished: - The signal Mag decreases to the level of parameter Set Point, the feedback loop maintains the Z-scanner in the position where the value of Mag is equal to Set Point. Note that this position of the scanner is approximately equal to half of the scanner extension range;...

  • Page 46: Changing The Temperature Of The Sample

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 7.2.3. Changing the Temperature of the Sample 1. Power on the liquid temperature control unit. ATTENTION! Using sample heating/cooling feature without the liquid temperature control system can cause damage to the Peltier modules. 2. Open the Additional Operations region by clicking the button in the upper right corner of the program main window.
  • Page 47 Chapter 7. Performing Measurements 9. Start the software oscilloscope and select SensorHeight signal for display. Fig. 7-17 and Fig. 7-18 show the temperature curve and SensorHeight variation when cooling the sample from 24° С to 14° С. The resulting thermal drift is the difference in the initial and final z-scanner position (SensorHeight signal) divided by the variation of temperature.

  • Page 48: Setting The Scanning Parameters And Scanning

    NTEGRA Therma Probe NanoLaboratory. Instruction Manual 7.2.4. Setting the Scanning Parameters and Scanning Setting the scan parameters (selection of a SPM-method, choosing scan region and scan speed) and scanning are similar to operation at normal conditions. A detailed description is given in the book (“Performing measurements”), Part 3, Chapter 3, Section «...

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