NT-MDT NTEGRA Therma User manual

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: [email protected]
Technical Support: [email protected]
NT-MDT Co., building 1,
Zelenograd, 1244, Moscow, Russia
Tel.: [phone]--
Fax: [phone]

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. 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
basic SPM techniques. “Fundamentals of Scanning Probe Microscopy” by V.L. Mironov
gives a good introduction to the subject. This book is available on the Internet,
http://www.ntmdt.com/manuals.
Feedback
Should you have any questions, which are not explained in the manuals, please contact the
Service Department of the company ([e-mail]) and our engineers will give you
comprehensive answers. Alternatively, you can contact our staff on-line using the ask-on-
line service (http://www.ntmdt.com/online).

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.
−SPM Software Reference Manual – is the description of the control program
interface functions, all commands and functions of the menu and, also a description of
the Image Analysis module and the Macro Language “Nova PowerScript”.
−Control Electronics. Reference Manual – is the guide to SPM controller,
Thermocontroller and Signal Access module.
Some equipment, which is described in the manuals, may not be included into your
delivery set. Read the specification of your contract for more information.
The manuals are updated regularly. Their latest versions can be found in the site of the
company, in the section “Customer support” (http://www.ntmdt.com/support).

NTEGRATherma Probe NanoLaboratory. Instruction Manual
NTEGRA Therma Probe NanoLaboratory.
Instruction Manual
Table of Contents
1. SYSTEM DESIGN ................................................................................................................................... 5
1.1. VT THERMAL EXCHANGEABLE MOUNT............................................................................................ 6
1.2. REGISTRATION HEAD ..................................................................................................................... 12
2. BASIC SAFETY MEASURES .............................................................................................................. 13
3. OPERATING CONDITIONS ............................................................................................................... 15
4. STORAGE AND TRANSPORT INSTRUCTIONS ............................................................................ 16
5. SETUP AND INSTALLATION ............................................................................................................ 17
5.1. INTERFACE BOARD INSTALLATION ................................................................................................. 17
5.2. SOFTWARE INSTALLATION.............................................................................................................. 17
5.3. INSTALLATION OF THE VT THERMAL EXCHANGEABLE MOUNT ..................................................... 18
5.4. CABLE CONNECTIONS..................................................................................................................... 23
5.5. POWERING SEQUENCE .................................................................................................................... 24
6. PREPARATION FOR OPERATION .................................................................................................. 26
6.1. SAMPLE INSTALLATION .................................................................................................................. 26
6.2. PROBE INSTALLATION .................................................................................................................... 27
6.3. REGISTRATION HEAD INSTALLATION ............................................................................................. 29
6.4. PREPARATION OF THE OPTICAL VIEWING SYSTEM FOR OPERATION ............................................... 30
6.5. ADJUSTMENT OF THE OPTICAL SYSTEM FOR DETECTING CANTILEVER DEFLECTIONS ................... 31
6.6. SELECTING REGION TO SCAN ......................................................................................................... 32
7. PERFORMING MEASUREMENTS ................................................................................................... 36
7.1. CONTACT AFM .............................................................................................................................. 36
7.1.1. Landing the Sample to the Probe..................................................................................... 36
7.1.2. Setting “Feedback Gain” Factor Working Level ............................................................ 39
7.1.3. Changing the Temperature of the Sample ....................................................................... 39
7.1.4. Setting the Scanning Parameters and Scanning .............................................................. 41
7.1.5. Finishing the Measurements............................................................................................ 41
7.2. SEMICONTACT AFM....................................................................................................................... 42
7.2.1. Setting the Piezodriver Working Frequency.................................................................... 42
7.2.2. Landing the Sample to the Probe..................................................................................... 43
7.2.3. Changing the Temperature of the Sample ....................................................................... 46
7.2.4. Setting the Scanning Parameters and Scanning .............................................................. 48
7.2.5. Finishing the Measurements............................................................................................ 48

Chapter 1. System Design
1. System Design
The NTEGRA Therma research system for variable temperature thermal measurements
includes the following basic parts and units:
-base unit;
-variable temperature thermal measurements assembly (VT thermal assembly):
−registration head;
−VT thermal exchangeable mount;
-protective hood;
-optical viewing system;
-vibration isolation system;
-liquid temperature control unit;
-control system:
−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;
4 – registration head; 5 – VT thermal exchangeable mount
5

NTEGRATherma 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
better than 0.001°C
Thermal drift on XY ≤15 nm/°C
Thermal drift on Z ≤10 nm/°C
Scan range 10x10x6 μm
XY linearity error 0.2% peak-to-peak/2
Z linearity error 1% peak-to-peak/2
RMS X, Y sensor noise in 300 Hz band ≤0.03 nm
RMS Z sensor noise in 1 kHz band ≤0.05 nm
RMS noise on Z in 1 kHz band <0.025 nm
Maximum sample size ∅14x1 mm
1.1. VT thermal Exchangeable Mount
A general view of the VT thermal exchangeable mount is given in Fig. 1-2. The
exchangeable mount provides both low temporal drift in the temperature range from -30°С
to +80°Сand small temperature drift after the temperature of the cell has been changed.
Fig. 1-2. VT thermal exchangeable mount
1 – temperature chamber; 2 –heat exchanger of scanner; 3 – outlets for liquid cooling
system; 4 – registration head seats
6

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.
Moreover, lower thermal conductivity of invar ensures thermal insulation of the scanner:
when the temperature chamber is heated up to 200°C the scanner piezotube is practically at
a room temperature, thus reducing the scanner thermal drift and temperature variations of
piezoceramic properties. The scanner contains capacitance sensors enabling exact control
over its position along all coordinate axes.
The inlet and outlet ports 3 are used to plug the heat exchanger to a liquid-cooling system
in order to stabilize the temperature of the exchangeable mount.
The scanner heat exchanger stabilizes the temperature of the scanner and other design
elements for which the temperature is required to stay constant while that of the
temperature chamber, the base unit and the environment is changed.
The cover of the temperature chamber is fixed by four clamps.
The probe is mounted on the cover (Fig. 1-3). Since the piezodriver is removed to the
registration head, the oscillations are transmitted to the cantilever through the cover using a
driving rod (see i. 1.2 “Registration Head” on page 12).
Fig. 1-3. Probe mount
1 – probe; 2 – spring clamp
The sample holder (see item 1 in Fig. 1-4) is in the center of the temperature chamber. The
sample is glued to a substrate which is installed on the sample stage and fixed on it by a
magnetic clamp.
7

NTEGRATherma 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.
The temperature sensor is inside the temperature chamber housing.
Supporting ring 2 is a part of the sample XY-positioning system.
When positioning the sample the holder descends below the edge of the supporting ring.
The substrate is retained by the supporting ring. The scanner moves in the XY-plane and
then lifts up. The holder fixes the substrate and then returns to the initial position.
Liquid temperature control system
The liquid temperature control system fulfills two main functions:
-Heat application/abstraction for maintaining temperature of the inoperative surfaces of
the Peltier modules;
-Scanner temperature stabilization (when used together with the temperature control
unit which maintains the fluid temperature stable up to about 0.01С).
Ports 3 are intended for connecting the thermal exchangeable mount with the temperature
control unit (Fig. 1-2).
Depending on the design of the liquid temperature control system two configurations are
available (Fig. 1-5):
-Configuration А– for a liquid-cooling system without precision stabilization.
-Configuration В– for a liquid temperature control which maintains the fluid
temperature stable up to about 0.01°С.
8

Chapter 1. System Design
Configuration АConfiguration 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. As a result, the liquid circulates only through the cooling
system of the Peltier modules.
When configuration B is used, the outlet of the liquid temperature control system should be
connected to port 2, and port 4 should be attached to the inlet of the system. Port 1,
connected to the port 3. Thus, the coolant is first fed to the scanner heat exchanger and
then to the cooling system of the Peltier modules.
9

NTEGRATherma 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;
6 – probe; 7 – scanner piezotube; 8 – temperature chamber; 9 – elastic hinge;
10 – restoring spring; 11 – approach mechanism lever; 12 – supporting ring;
13 – membrane; 14 – heat exchanger of scanner
Sample holder 1 is inserted into hollow lever 5 and hold there by friction force. Beam 3
enters a hole in the sample holder and provides its displacement along the Z-axis.
The hollow lever consists of two parts. Its upper part, coupled to the cell by a membrane is
made of copper, while the lower part is from invar. The hollow lever is joined to the
piezotube by an elastic hinge. Such design provides uniform heating of the temperature
chamber and also protects the scanner from overheat.
10

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.
The procedure of automatic sample approach to the probe consists of several cycles.
Within one approach cycle the following operations are completed:
1. The feedback is turned on and the scanner piezotube extracts to the maximum towards
the probe.
2. If interaction between the probe and the sample has not been obtained, the feedback
circuit breaks, the piezotube retracts to the maximum and the stepper motor moves the
sample holder towards the probe at a specified distance.
3. Then the procedure repeats.
If interaction of the probe with a sample is obtained, the step engine makes several steps in
the opposite direction. Mechanical joint between the beam and the sample holder breaks,
and the former is hold at the adjusted height by friction force.
Scanning
The main parts of the scanner include:
-piezotube;
-elastic hinge;
-hollow lever;
-sample holder;
-membrane.
When scanning, the piezotube displacement in the XY-plane is transmitted to the sample
through the hollow lever using the elastic hinge. Membrane 13 joins the lever with the
temperature chamber and provides a center of rotation during scanning. The distance from
the center of the elastic hinge to the membrane is 4 times more than that from the
membrane to the cantilever. Hence, the scan range in the XY-plane decreases by a factor of
four. The piezotube displacement along the Z-axis is transmitted to the sample along the
lever without transformation owing to the membrane deformation.
11

NTEGRATherma 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
1 – laser adjustment screws;
2 – photodiode adjustment screws;
3 – protective overlay; 4 – observation port;
5 – piezodriver
b) bottom view
6 – supports; 7 – piezodriver driving rod
Fig. 1-7. Registration head design
The system for detecting the cantilever deflections consists of a laser, a photodiode,
the system of mirrors, the laser beam and photodiode alignment devices and a preamplifier
board. The system for detecting the cantilever deflections is schematically shown
in Fig. 1-8.
LAZER
12
2
3
4
Fig. 1-8. System for detecting cantilever deflections
1 – laser, 2 – mirror, 3 – photodiode, 4 – probe
To protect the head from heat, a fluoroplastic protective cover is installed in the lower part
of the head (Fig. 1-7). There is an observation port in its upper part.
The piezodriver is in the lower part of the head. The driving rod, that transmits oscillations
to the cantilever in the temperature chamber, is fixed to the piezodriver (see Fig. 1-7 b).
12

Chapter 2. Basic Safety Measures
2. Basic Safety Measures
General 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.
-This instrument contains precision electro-mechanical parts. Therefore protect it from
mechanical shocks.
-Protect the instrument against the influence of extreme temperature and moisture.
-For transport, provide proper packaging for the instrument so as to avoid its damage.
Electronics
-Before operation, set the power switch of the SPM controller to the position
corresponding to value of the local electrical power line (this is only done with the
controller being off!).
-Switch the SPM controller off before connecting/disconnecting its cable connectors.
Disconnecting or connecting the cable connectors during operations may cause damage
to the electronic circuit and disable the instrument. A warning label is attached to the
SPM controller of the instrument (Fig. 2-1).
Fig. 2-1
13

NTEGRATherma 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.
Fig. 2-2
Scanner
-Do not apply to the scanner forces bigger than it is necessary for installation of a probe
or a substrate with a sample. Avoid impacts on the scanner and its lateral displacement.
Remember that thickness of the scanner walls makes only 0.5 mm.
14

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%;
-atmospheric pressure 760 ±30 mm Hg;
-electric mains with 110/220 V (+10%/-15%), 50/60 Hz and grounding;
-the room should be protected from mechanical vibrations and acoustic noises, either
internal or external;
-the table intended for installation of the measuring unit of the instrument must be stable
and, whenever possible, massive;
-vibration criterion VC-C, 12.5 µm/s (one-third octave band criterion);
-the device should be protected from the direct sun radiation impact;
-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.
The operation of the device is susceptible to heat flows, draughts and sudden alternations
in temperature and humidity.
15

NTEGRATherma 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;
-Acceptable humidity inside the premises is < 80 %.
Transport Instructions
-The instrument should be carefully packaged to avoid damage during transport.
16

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.
To install the interface board:
1. Disconnect the control PC from the wall outlet.
2. Open the PC case.
3. Select an empty PCI slot on the motherboard.
4. Remove (unscrew) the gap closure from the selected slot. Insert the interface board
accurately into the slot against stop. Make sure the board is installed in the slot evenly
without any skew.
5. Fix the interface board using the screw from the gap closure.
6. Make sure no cords and wires touch the board. If necessary, properly fasten loose cords
inside the PC case.
7. Close the PC case and connect it to the wall outlet.
5.2. Software Installation
Install the Nova control program. Proceed as follows:
1. Insert the installation disk into the CD-drive.
2. Run file setup.exe. The screen will display the dialog box of the setup wizard. To
install the software follow the instructions of the wizard.
Upon finishing the installation a shortcut to the Nova program will appear on the desktop.
#NOTE. The details of the software installation are discussed in the manual «SPM
Software».
17

NTEGRATherma 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. Turn the approach mechanism housing counter-clockwise to the maximum (Fig. 5-2).
Fig. 5-2
3. Unscrew the three screws which fix the exchangeable mount to the base unit (see
item 3 in Fig. 5-1).
#NOTE. The screws have retaining washers and cannot be removed from the
exchangeable mount.
4. Remove the exchangeable from the base unit.
18

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.
Fig. 5-3
1 – retaining screw, 2 – guide holes
Fig. 5-4. VT thermal mount
1 – guides, 2 – approach mechanism shank; 3 - openings for bushings
#NOTE. When using a liquid temperature control system which maintains the fluid
temperature stable up to about 0.01°С, special bushings (Fig. 5-5) should be
inserted in openings 3 (Fig. 5-4) in order to isolate the thermal exchangeable
mount from the base unit.
Fig. 5-5. Bushing
19

NTEGRATherma 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. Turn the approach mechanism housing clockwise to the maximum (Fig. 5-7).
Fig. 5-7
4. Tighten the retaining screw (see item 1 in Fig. 5-6).
5. Insert the tubes in the adapter as shown in Fig. 5-8. Fix ~15 cm tubes in ports 1 and 2
to connect them with the thermal exchangeable mount. Ports 3 and 4 shall be fitted
with ~40 cm tubes and connected with the liquid-cooling system. Insert the tubes in
their ports up to the stop.
#NOTE. To remove the tube from the port, press the blue holder slightly until it is
recessed in the port.
20