NT-MDT Solver Next User manual
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
basic SPM techniques. “Fundamentals of Scanning Probe Microscopy” by V.L. Mironov
gives a good introduction to the subject. This book is available free of charge at
https://www.ntmdt-si.com/customer-support/manuals/textbook.
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give you comprehensive answers. Alternatively, you can contact our staff on-line using
the ask-on-line service (http://online.ntmdt-si.com/online).
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.
-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 (http://www.ntmdt-si.com/support).
Table of Contents
SOLVER NEXT SPM. Fluid Measurements
Table of Contents
1. OVERVIEW..............................................................................................................................................3
1.1. DESIGNATION AND MEASUREMENT TECHNIQUES.............................................................................3
1.2. DESIGN OF THE LIQUID HEAD...........................................................................................................5
1.3. DESIGN OF THE LIQUID CELL............................................................................................................6
2. PREPARATION FOR OPERATION.....................................................................................................7
2.1. POWERING SEQUENCE ......................................................................................................................7
2.2. SAMPLE INSTALLATION ....................................................................................................................8
2.3. PROBE INSTALLATION.....................................................................................................................12
2.4. INSTALLING THE LIQUID HEAD.......................................................................................................14
2.5. INITIAL APPROACH AND SELECTING RELEVANT AREA...................................................................17
2.6. ADJUSTING THE SYSTEM FOR DETECTING THE CANTILEVER DEFLECTIONS....................................19
2.6.1. Adjusting Detection System by Videoimage........................................................................21
2.6.2. Adjusting Detection System through Laser-Diode Scanning Window.................................22
3. PERFORMING MEASUREMENTS....................................................................................................25
3.1. CONTACT AFM ..............................................................................................................................25
3.2. SEMICONTACT AFM.......................................................................................................................25
3.2.1. Approach the Sample to the Probe......................................................................................26
3.2.2. Taking Resonance Curve and Adjusting Parameters of Generator Output ........................27
3.2.3. Preparation for Scanning....................................................................................................32
3.2.4. Scanning..............................................................................................................................32
3.2.5. Saving Measurement Data..................................................................................................32
3.2.6. Operation Completing.........................................................................................................33
SOLVER NEXT SPM. Fluid Measurements
Chapter 1. Overview
3
1. Overview
1.1. Designation and Measurement Techniques
The measuring head for operation in liquid (hereafter - liquid head) is designed for
measurements in liquid environment with basic AFM techniques. The liquid head is a
replaceable part of the SOLVER NEXT instrument.
The liquid head consists of the following parts (Fig. 1-1):
●liquid head itself;
●liquid cell;
●probe mounting wrench.
Fig. 1-1. Composition of the liquid head
1 –liquid head; 2 –liquid cell; 3 –wrench
For measurements in liquids, either the liquid cell is used or several droplets of interest are
deposited on the sample that is preliminary mounted on a standard substrate.
ATTANTION! Be utmost careful, when operating with liquid. The
scanner is not protected against penetrating the liquid inside it while
this liquid can damage the scanner.
SOLVER NEXT SPM. Fluid Measurements
4
The liquid head provides measurements with the following techniques:
●Contact AFM;
●Semicontact AFM;
●Lateral Force Imaging;
●Adhesion Force Imaging;
●Force Modulation Mode;
●Phase Imaging Mode;
●AFM Lithography.
Table 1-1. Specifications
Parameter
Value
Measuring Head dimensions
75×46.5×65 mm
Measuring Head mass
112 g
Cell dimensions
Ø27×9.7 mm
Cell mass
9 g
Material Cell
titan, teflon and stainless steel
Thickness of the liquid layer in the cell
up to 3 mm
Amount of the liquid in the cell
up to 1 ml
Sample size
up to 14×14×2 mm
Chapter 1. Overview
5
1.2. Design of the Liquid Head
Fig. 1-2 shows general view of the liquid head.
Fig. 1-2. Liquid head
1 –support balls; 2 –probe holder; 3 –magnetic fastener
The support balls serve for placing the liquid head in its mounting seats in the measuring
unit of the SOLVER NEXT. The magnetic fasteners provide stable securing of the head.
Design of the liquid cell provides high stability of its position so that the probe tip comes
to the same position relative to the sample when the head is remounted after removal.
Probe Holder
The liquid head contains a probe holder. Basic components of the holder are shown
schematically on Fig. 1-3. The holder consists of the glass prism 1 that is placed on the
liquid cell and the spring clip 2. The probe is placed on the bevel face of the glass prism
and fixed with the spring clip. For bending the spring in mounting or dismounting
operations, use the dedicated wrench supplied with the measuring head.
Fig. 1-3. Main parts of the probe holder
1 –glass pedestal; 2 –clip
1
2
SOLVER NEXT SPM. Fluid Measurements
6
1.3. Design of the Liquid Cell
The liquid cell contains (Fig. 1-4):
●titanium-made base for keeping liquid from entering the scanner;
●fluoroplastic housing for placing the sample and for filling with the liquid;
●two clips of stainless steel for securing the sample.
Fig. 1-4. Composition of the liquid cell
1 –base; 2 –housing; 3 –clips for placing the sample
ATTENTION! Use liquids chemically neutral to stainless steel, titan and
the probe material.
The cell is made of chemically neutral materials (titan, Teflon, and stainless steel) that are
resistant to the solutions of acids, such as H2SO4and HCl. Limitations on the liquid (gas)
are determined by the materials contacting with this liquid or gas.
Chapter 2. Preparation for Operation
7
2. Preparation for Operation
The explanations below assumes that the user is well aware of procedures on preparing for
measurements and on performing measurements with contact and semicontact AFM
techniques in air (see «SPM SOLVER NEXT. Instruction manual»).
The basic operations performed when preparing for the work:
1. Powering Sequence (see i. 2.1 on p. 7).
2. Sample Installation (see i. 2.2 on p. 8).
3. Probe Installation (see i. 2.3 on p. 12).
4. Installing the Liquid Head (see i. 2.4 on p. 14).
5. Initial Approach (see i. 2.5 on p. 17).
6. Adjusting the System for Detecting the Cantilever Deflections (see i. 2.6 on p. 19).
Below, these stages are explained in details.
2.1. Powering Sequence
Before preparing for operation, perform the following steps:
1. Switch on the computer.
2. Switch on the vibration protection system.
3. Switch on the SPM controller.
ATTENTION! All connectors should be secured before switching
the computer on. Any disconnection in the process of operation can
result in damage of electronic components.
4. Start the Nova Px Control Program. The Program Main window appears on the screen
(Fig. 2-1).
Fig. 2-1. The Program Main window
5. Operation of the Control program starts with initialization of the instrument. If
initialization is successful, the indicator in the Initialization panel will
change its appearance to .
If the initialization has not run automatically, launch it by clicking the button.
SPM state indicator
SOLVER NEXT SPM. Fluid Measurements
8
2.2. Sample Installation
Details of sample installation depend on how the liquid is used (in bulk or in droplets).
Further those details are explained.
Mounting Sample in Liquid Cell
ATTENTION! Be utmost careful, when operating with liquid. The
scanner is not protected against penetrating the liquid inside it while
this liquid can damage the scanner.
NOTE. If either of the built-in heads is in its working position before starting the sample
installation, move it to inoperative one by clicking the button.
Fig. 2-2
To install the sample on the liquid cell, perform the following steps:
1. Place the cell on a flat surface.
2. Install the sample (or the substrate with the fixed sample) in the cell and secure it with
the clips (see Fig. 2-3).
Fig. 2-3. Cell with the sample installed
NOTE. The sample should be positioned with the scan region as close to the center of
the cell (i.e. to the scanner axis) as possible. Otherwise a surface tilt appears when
scanning which limits the application of some techniques.
3. Fill the cell with liquid. Amount of the liquid depends on the sample thickness. The
sample should be covered with the liquid completely.
Chapter 2. Preparation for Operation
9
4. Place the cell with the sample on the sample stage so that the clips were perpendicular
to the built-in measuring heads after the cell was placed (see Fig. 2-4). Observe that the
support balls meet the slots in the cell base.
Fig. 2-4. Installing the liquid cell
Arrows show location of the clips
Now, the liquid cell is installed.
Sample installation for operation in a droplet
ATTENTION! Be utmost careful, when operating with liquid. The
scanner is not protected against penetrating the liquid inside it while
this liquid can damage the scanner.
Sample installation for operation in a droplet is basically the same as that for operation in
air (see book “SPM Solver NEXT. User’s manual”).
Here, only steps specific for operation in a droplet are given. Those are:
1. Fix the sample on a substrate. Place the substrate on the sample holder.
2. Spill a few drops of liquids on the sample. Height of a droplet above the sample surface
should be at least 0.5 mm.
3. Place the sample-substrate assembly on the sample stage.
Now, sample installation is complete.
SOLVER NEXT SPM. Fluid Measurements
10
Setting the sample height value
For better accuracy of scanning along X and Y directions in the scanning-by-sample mode,
the total height of the assembly of the sample with the liquid cell or with the substrate
should be properly considered. The Control program Nova Px operates with the total
height using the Sample Height parameter.
Estimate the total height of the sample with the cell (including the sample holder)
(Fig. 2-5), and enter that value in the SampleHeight parameter of the Control program.
Calculate value of the Sample Height parameter (see Fig. 2-5) as:
Sample Height = a+ b,
where
ais intrinsic height of the sample;
bis thickness of the liquid cell bottom or height of the sample holder.
Thickness of the liquid cell bottom is 3.8 mm.
Sample inside the liquid cell
a –sample height; b –cell bottom thickness;
Sample Height –sample height corrected for the cell bottom
Sample on the substrate
a –sample height; b –sample holder height;
Sample Height –sample height corrected for the substrate
Fig. 2-5. Taking the combined sample height
Chapter 2. Preparation for Operation
11
For setting the sample height in the program, perform the following steps:
1. Open the ScanSettings window by clicking the button in the Scanning
window (Fig. 2-6).
Fig. 2-6. Settings
2. In the SampleHeight input field (Fig. 2-7), enter the desired composite sample height.
Fig. 2-7. Setting the sample height
3. Click the OK button to apply your modifications and to close the ScanSettings
window.
The SampleHeight parameter should be modified every time when another value of the
sample height is required.
SOLVER NEXT SPM. Fluid Measurements
12
2.3. Probe Installation
To install probe, do the following:
1. Verify that the glass pedestal is clean. If necessary, remove the clip from its slot on the
base and then wipe the pedestal with a lint-free tissue moistened with alcohol.
2. Place the measuring head on an even surface with the probe holder directed upwards.
ATTENTION! To avoid deformation of the clip unbend it only on the
minimum angle required.
3. Use the special wrench of the measuring head kit for mounting the probe. Capture the
clip in its bending with the wrench bracket (Fig. 2-8) and press the wrench handle
slightly to straighten the clip.
Fig. 2-8. Probe installation.
The arrow shows the direction of force application
4. Using tweezers take a probe from the set. So not turn the chip over as the probes are
placed with their tips pointing upwards. (Fig. 2-9).
Fig. 2-9. Container with probes
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