Quick Start Guide: Data Collector

DATA COLLECTOR
Quick Start Guide

Data Collector
Quick Start Guide
EDITION NOTICE: 4022 339 20070, November 2012

This is the original publication of Edition 10 of this Quick Start Guide, to be used
with Data Collector version 4.2 or higher.
Data Collector Quick Start Guide
ACKNOWLEDGMENTS
All registered and unregistered trademarks, domain names and copyrights herein
are the property of their respective owners.
DISCLAIMER
The information provided herein is supplied under a non-exclusive license
authorizing its use solely for and in conjunction with PANalytical's products.
Although diligent care has been used to ensure that the information is accurate,
nothing contained herein can be construed to imply any representation or warranty
as to the accuracy, currency or completeness of this information.
COPYRIGHT NOTICE
© 2012, PANalytical B.V., Almelo, The Netherlands
PANalytical B.V.
Lelyweg 1
7602 EA, Almelo
The Netherlands
Tel: +31 546 534444
Fax: +31 546 534598
Internet www.PANalytical.com
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General Pages
Contents
Chapter 1 Introduction
Chapter 2 Starting to Work with Data Collector
Chapter 3 Using Data Collector with Empyrean
Chapter 4 Using Data Collector with MRD (XL) Systems
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Chapter 1
Introduction
1.1 INTRODUCTION............................................................ 1 - 3
1.2 21 CFR PART 11 SUPPORT MODE ................................ 1 - 3
1.3 CONVENTIONS USED ................................................... 1 - 3
Introduction
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Chapter 1. Introduction
1.1 INTRODUCTION
This Quick Start Guide is intended to help you to use the described software quickly
and efficiently. The examples show you how to start and perform fairly simple tasks.
This document is not designed to show in detail or explain all the various
possibilities of the software. For each of the examples in this document, only one
route to perform a task is shown. To explore other methods, you can experiment
with the system and learn the other possibilities yourself.
In order to follow the examples, start with Chapter 2. Then, proceed to either
Chapter 3 or 4 (depending on your system).
1.2 21 CFR PART 11 SUPPORT MODE

If you are operating in 21 CFR Part 11 Support Mode you will occasionally be faced
with situations that are slightly different to those described here. If that occurs,
follow the directions on your screen. For more detailed instructions about this mode,
please refer to the on-line help topic entitled “21 CFR Part 11 Support Mode”.
1.3 CONVENTIONS USED

◆ An instruction is preceded by a bullet “”.
◆ Menu items, keys and pushbuttons on a window are shown in bold text, for
example: File > Open, Enter, Ctrl, Apply, Cancel.
◆ There may be differences between the example screens given in this Quick
Start Guide and what you see on your screen. In all cases, where there is a
difference, follow what you see on your screen.
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Chapter 2
Starting to Work with Data Collector
2.1 INTRODUCTION............................................................ 2 - 3
2.2 CONVERTING THE DATABASE..................................... 2 - 3
2.3 STARTING DATA COLLECTOR...................................... 2 - 6
2.4 CREATING A NEW USER .............................................. 2 - 7
2.5 ORGANIZING YOUR RESULT DATA ............................. 2 - 8
2.6 SPECIFYING THE REPORT FOLDER............................. 2 - 11
Starting to Work with Data Collector
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Chapter 2. Starting to Work with Data Collector
2.1 INTRODUCTION
This chapter describes how to start Data Collector, and how to create a new user and
enable that user to work on the system with all the privileges of a system owner and
user manager.
• If you have upgraded Data Collector on your computer from a version
lower than 4.0, you must first convert your database and measurement
program data for use with the new version. Go to “Converting the
Database” (Section 2.2).
• If your current Data Collector is version 4.0 or higher, or you are using a
new installation, or the database has already been converted, go to
“Starting Data Collector” (Section 2.3).
2.2 CONVERTING THE DATABASE

If your current Data Collector is lower than version 4.0:
• Click OK to close the popup window.
• Select Start > All Programs > PANalytical Data Collector > Utilities >
Data Collector Database Conversion.
• Select the database to convert (DataCollector.db in this example).
• Click Open.
• Click the Yes button to make a backup.
• Either accept the proposed name or rename the database and click Save.
If a message about the disk space appears and you have enough disk space,
click OK.
A message about the version appears.
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• Click Yes.
The following screen appears.
• As soon as the Close button is enabled, click on it to exit from the database
conversion program.
You may get a message about incorrect conversion results.
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• Click OK.
• Select Start > All Programs > PANalytical Data Collector > Utilities >
XRDMP Exporter.
• In the PANalytical XRDMP Exporter window, select your database and
the folder where you want to store the exported measurement programs.
• Click Start.
• Wait until the following message appears.
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Your database is now converted to the SDF format, and your programs have been
exported to the XRDMP format. Refer to the XRDMP Exporter on-line help for
more information.
• Click OK.
• If you want to save a Conversion Report File, click Save.
• Click to exit from the XRDMP Exporter window.
2.3 STARTING DATA COLLECTOR

NOTES: a. If this is the first time Data Collector is used after an upgrade, a
warning about the database version may appear. If it does, click
OK. Then go to “Converting the Database” (Section 2.2). If this
warning does not appear, continue to log in.
b. If this is the first time Data Collector is used after a new installation,
or after a database conversion, you will be asked to enter a new user
account and password. Please follow the instructions on the screen.
• Double-click on the Data Collector icon .
• Type in the following information:

User: User-1
Password: galaxy
(the user name and password delivered with the software)
• Click OK.
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2.4 CREATING A NEW USER

• From the menu, select System Settings > User Management.
• Click New.
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• Enter the following information:

Name: = My Name
Full user name: = My Full Name
Access level: = Select “System Owner”
Check the “User manager” box.
Password: = password (do not use spaces in your password)
Re-type Password: = password.
• Click OK.
• Check that “My Name” is included in the “Name” list and click Close.
The new user is now created. To start actions as this user, select File > Exit to exit
from Data Collector and restart Data Collector by double-clicking on the Data
Collector icon. Log in with the user name “My Name” and the password
“password”.
2.5 ORGANIZING YOUR RESULT DATA

Before you start to use it, you need to tell the system where to put the results of your
measurements.
• From the menu, select
User Settings > Measurement Types and Data Folders.
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Here is where we define the default folder where all of the results will be
placed. If there are types of measurement that you are never going to use
you could clear their check box here; in this example we will leave them
all on.
• Click the browse button ( ) of the Absolute scan Default folder field:
• Click New Folder and enter the name of the folder, in this example: “My
Name”.
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• Click OK.
• Put a check mark in the Apply to all single scans check box.
• Click OK.
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• Repeat these actions for the Multiple scan and Batches tabs.
• Click OK.
2.6 SPECIFYING THE REPORT FOLDER

If you create a report of a program or a configuration you can specify the default
destination folder.
• From the menu, select User Settings > Options.
• If a message appears that asks you if you want to create a report folder,
click No. We will set up the report folder in the following actions.
• In the Options window, select the Miscellaneous tab.
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• Click on the button to select the report folder, in this example:

“C:\XRD Data\My Name”.
• Click OK.
The preparation stage is now complete. You can now start defining configurations
and measurement programs, and performing measurements.
• Click to exit from Data Collector.
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Chapter 3
Using Data Collector with Empyrean
3.1 INTRODUCTION............................................................ 3 - 2
3.2 PREPARATION .............................................................. 3 - 2
3.3 STARTING THE SOFTWARE.......................................... 3 - 2
3.4 DESCRIBING YOUR HARDWARE ................................. 3 - 2
3.4.1 Defining the Hardware Family .......................................................... 3 - 3
3.4.2 Defining the Configuration................................................................ 3 - 4
3.4.3 Selecting your Optical Components .................................................. 3 - 5
3.4.4 Saving the Configuration ................................................................... 3 - 8
3.5 DEFINING A MEASUREMENT PROGRAM.................... 3 - 9
3.5.1 Defining the Measuring Program Parameters.................................... 3 - 9
3.5.2 Defining the Instrument Settings for the Measurement................... 3 - 11
3.5.3 Saving the Measurement Program................................................... 3 - 13
3.6 PERFORMING THE MEASUREMENT .......................... 3 - 15
3.6.1 Connecting to the Instrument........................................................... 3 - 15
3.6.2 Mounting the Sample....................................................................... 3 - 17
3.6.3 Starting the Measurement ................................................................ 3 - 19
Using Data Collector with Empyrean
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3.1 INTRODUCTION
This chapter describes how to use Data Collector to set up a measurement on an
Empyrean system. Although this chapter is about using Data Collector with an
Empyrean system (as used in these examples) the procedure is, in fact, almost the
same if you want to use an X’Pert PRO MPD or X’Pert Powder system.
Before performing the procedures that are described in this chapter, define a user
“My Name” as described in Chapter 2 of this guide.
3.2 PREPARATION
• Switch the system on by pressing the “On” button on the Empyrean
control panel. Wait until the control panel shows: “30 kV” and “10 mA”.
The system is now ready for use. If the power run up does not happen,
refer to the relevant hardware User’s Guide.
3.3 STARTING THE SOFTWARE

• Enter the user name and password: “My Name” and “password”
• Click OK.
3.4 DESCRIBING YOUR HARDWARE

Before you can start to collect data you have to tell the software what hardware is
used in your diffraction system.
• From the menu, select File > New Configuration.
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Chapter 3. Using Data Collector with Empyrean
3.4.1 Defining the Hardware Family
• In the System identification frame, select your hardware family

(Empyrean in this example) from the Hardware family drop-down box.
• Click Read Instrument.
NOTE: If the system has not been previously initialized an initialization wizard
will start. If this happens, just follow the instructions on the screen.
• Wait until the Connecting to instrument pop-up disappears. The system

is now ready for use.
• If the system cannot identify some of the items, it will ask you to specify
what you have.
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3.4.2 Defining the Configuration
• Click on the Next button. The Goniometer/Sample stage frame appears.
• Click on the Next button. The Incident beam path frame appears.
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• Check that the information displayed here is correct. If necessary, adjust

the fields to the correct settings.
• Click on the Next button. The Diffracted beam path frame appears.
• Check that the information displayed here is correct for all diffracted beam
paths. If necessary, adjust the fields to the correct settings.
• Click on the Next button. The Axes frame appears, which we will not
change at this time..
3.4.3 Selecting your Optical Components

Tell the system what changeable devices are available to you. Always start with the
PreFIX module products (default is “PreFIX module (Incident)”), then “PreFIX
module (Diffracted)” if any are available.
• Click on the Pre-select button to open the Pre selection window.
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• Browse through each entry in the Product type drop-down list and select
the products that are available to you, and that you want to use in this
configuration.
• To select an item, click on that item in the All products list and then click
.
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NOTE: If you have X-ray Mirror or Hybrid monochromator PreFIX modules in

your system, it is important that you enter their offsets that are provided
in the System Acceptance Form delivered with your system.
To enter the offset of a product, highlight that product in the
Pre-selected products list and enter the applicable offset in the
Offsets frame.
• When you have selected all of the items that you require, click OK.
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3.4.4 Saving the Configuration

• From the menu, select File > Save As to save the configuration.
• Enter the name of the configuration in the Name field. In this example,
enter “My Spinner”.
• Enter the description of the configuration in the Description field. In this
example, enter “Configuration for Powder Samples (QSG)”.
• Click OK.
• Close the Define Configuration window by clicking .
NOTE: If you have more than one sample stage, you should make a
configuration for each sample stage. In order to do that you must mount
each of your sample stages in turn and then create a configuration for
that stage by repeating the actions in this section.
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3.5 DEFINING A MEASUREMENT PROGRAM

At this stage in the procedure you can either connect to the instrument, or define a
measurement program. In this example we will first define a measurement program
and then connect to the instrument.
• From the menu, select File > New Program.
• From the Program type drop-down list, choose the type of program you
want to define (in this example: “Absolute scan”), and click OK.
3.5.1 Defining the Measuring Program

Parameters
You have just opened the Prepare Absolute Scan window:
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• If the value in the Configuration frame is not My Spinner, select

My Spinner from the drop-down list. This will cause the following
message to be displayed:
• Click OK.
• Set the applicable parameters in the Prepare Absolute Scan window to
the values shown in Table 1.
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Table 1 Prepare Absolute Scan Parameters
Parameter Value
Configuration Diffracted Beam Path*
Scan Axis Gonio
Scan Properties Continuous
Start angle (°) 20
End angle (°) 90
Step size (°) 0.020**
Time per step (s) 1
*The beam path radio buttons only appear if your system has a double detector arm.
Choose the beam path with Bragg-Brentano focussing optics.
**If you have a PIXcel or an X’Celerator detector in your system, the step size is
determined by the system according to the parameters of this detector (defined when
you click on the Settings button).
The Scan speed and Total time are automatically calculated when the parameters
in Table 1 are adjusted.
3.5.2 Defining the Instrument Settings for the

Measurement
• In the Prepare Absolute Scan window, click on the Settings button.
• To select the Stage and Optics settings for this program, click on the
Sample Stage icon.
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• Select Spinning, and if appropriate, a Revolution time of 1 s.

• Click on the Incident beam path icon to choose the items to use in this
program, starting with the PreFIX module, in this example:
Progr. divergence slit with anti-scatter slit.
Table 2 Incident Beam Path Parameters
Parameter Value
Divergence slit Prog. Div. Slit*
Usage Automatic
Irradiated length 10 mm
Offset 0 mm
Mask Inc. Mask Fixed 10 mm (MPD/MRD)
Soller slit Soller 0.04 rad
*If you do not have a programmable divergence slit, select a fixed slit of 1°.
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• Click on the Diffracted beam path icon to choose the items to use in this
program, starting with the PreFIX module, in this example: PRS/PASS.
Table 3 Diffracted Beam Path Parameters
Parameter Value
Anti-scatter slit Programmable anti-scatter slit*
Usage Automatic
Observed length 10 mm
Offset 0 mm
Receiving slit Programmable receiving slit (with a height of 0.3)**
Soller slit Soller 0.04 rad
Detector Select your detector
* If you do not have a programmable anti-scatter slit, select a fixed slit of 1°.
**If you do not have a programmable receiving slit, select a fixed slit of 0.3 mm.
• Click OK to apply the settings to your program.
3.5.3 Saving the Measurement Program

• In the Prepare Absolute Scan window, click Description.
• Enter the description of the program (in this example: “Example for
QSG”).
• Click OK.
• From the menu, select File > Save.
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• In the File name field, enter the file name (in this example:
“My Program”).
• Click Save.
• Click to close the Prepare Absolute Scan window.
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3.6 PERFORMING THE MEASUREMENT
3.6.1 Connecting to the Instrument

Before you can start a measurement, you must connect to the instrument.
• From the menu, select Instrument > Connect.
• Select the configuration that you made earlier (in this example: “My
Spinner”).
• If applicable, select the diffracted beam path with the Bragg-Brentano type
optics.
• Click OK.
A message window may appear, showing the assumptions that the software has
made about the status of the system.
• Carefully check if these assumptions are correct.
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• Click OK.
• To correct any incorrect assumptions that were shown in the previous
message window, select the applicable tabs on the instrument control
window and make the corrections.
• Check the Instrument Settings, Incident Beam Optics and Diffracted
Beam Optics tabs to make sure that you have the correct parts mounted.
• In the Instrument Settings tab, double-click on the Generator branch of

the tree.
• In the Instrument Settings window, select the X-ray tab.
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• In the Tension (kV) field, enter “45”.

• In the Current (mA) field, enter “40”.
• Put a check mark in the Generator on check box.
• Click Apply.
• Wait until the system has powered up to 45 kV and 40 mA.
3.6.2 Mounting the Sample

Depending on your system configuration, mount the Si sample as follows.
NOTE: This procedure assumes that the Instrument Settings window is opened.
3.6.2.1 No sample spinner

• Mount the sample on the sample stage.
• Close the enclosure doors.
• In the Instrument Settings window, click OK.
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3.6.2.2 Sample spinner, but no sample changer

• In the Instrument Settings window, select the Sample Stage tab.
• Lower the sample spinner platform with the handle.
• Mount the sample.
• Release the handle to bring the sample to the spinning position.
• Click OK.
3.6.2.3 Sample changer, positioned in the corner

• Clear the Lift Up check box.
• Click Apply.
• Open the enclosure doors.
• Mount the sample.
• Put a check mark in the Lift Up check box.
• Click OK.
3.6.2.4 Sample changer, ready for use

• Open the enclosure doors.
• Put the sample into an empty magazine or monitor position.
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• Indicate to load the sample from the position that you have placed the
sample into.
• Click OK.
3.6.3 Starting the Measurement

• From the menu, select Measure > Program.
• Select the desired program (in this example: “My Program”).

• Click Open. The Start window appears.
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• In the File frame, enter:

Name: My Program_1.xrdml (default)
Folder: C:\XRD Data\My Name (default)
Comment:“Example for Quick Start Guide”.
• In the Sample frame, give the sample a name:
ID: Standard Si Sample
Name: Silicon Pellet
Prepared by:“My Full Name”.
• Check that the enclosure doors are closed and click OK.
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• If a message appears that tells you to do something, perform the actions as

instructed and click OK.
The scan starts and will take some time, depending on the program parameters (in
this example: 1 hour). The scan is displayed as the measurement progresses. Notice
that the scale changes as the measurement proceeds.
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This scan is automatically saved with the file name “My Program_1.xrdml”.
You have now collected the data.
• To close Data Collector, select File > Exit and click OK.
You can use Data Viewer to view your results. A guide to using Data Viewer is
given in the Data Viewer Quick Start Guide.
If you want to automatically use the results of future measurements, you could for
example, utilize one of the scripts available with Automatic Processing Program.
Examples of these scripts and of how to use them is given in the Automatic
Processing Program - Quick Start Guide.
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Chapter 4
Using Data Collector

with MRD (XL) Systems
4.1 INTRODUCTION............................................................ 4 - 3
4.2 PREPARATION .............................................................. 4 - 3
4.3 STARTING THE SOFTWARE.......................................... 4 - 3
4.4 DESCRIBING YOUR HARDWARE ................................. 4 - 4
4.4.1 Defining the Hardware Family .......................................................... 4 - 5
4.5 SETTING UP TWO CONFIGURATIONS ......................... 4 - 6
4.5.1 First Configuration: Rocking Curve – Triple Axis............................ 4 - 6
4.5.2 Second Configuration: Other Optics.................................................. 4 - 9
4.6 MEASURING THE ROCKING CURVE .......................... 4 - 13
4.6.2 Setting the Tube Voltage and Current ............................................. 4 - 15
4.6.3 Preparing the Beam Paths ................................................................ 4 - 16
4.6.4 Sample Positioning .......................................................................... 4 - 19
4.6.5 Manual Scan .................................................................................... 4 - 21
4.6.6 Adjusting the Goniometer Position ................................................. 4 - 23
4.6.7 Optimize Chi.................................................................................... 4 - 24
4.6.8 Measuring ........................................................................................ 4 - 28
4.7 PERFORMING A REFLECTIVITY MEASUREMENT ...... 4 - 32
4.7.2 Setting the Tube Voltage and Current ............................................. 4 - 33
4.7.3 Preparing the Beam Paths ................................................................ 4 - 34
4.7.4 Mounting the Sample....................................................................... 4 - 37
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4.7.5 Positioning the Sample ....................................................................4 - 39

4.7.6 Calibrating the Attenuation Factor .................................................. 4 - 40
4.7.7 Aligning the Sample ........................................................................ 4 - 43
4.7.8 Creating a Measurement Program ...................................................4 - 49
4.7.9 Measuring the Reflectivity Curve.................................................... 4 - 52
4.7.10 Changing the Axes........................................................................... 4 - 53
Using Data Collector

with MRD (XL) Systems
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Chapter 4. Using Data Collector with MRD (XL) Systems
4.1 INTRODUCTION
This chapter describes how to use Data Collector to set up a measurement on an
MRD (XL) system.
Two measurements are described:
◆ The silicon (111) single crystal sample delivered with the system (section
4.5 - Measuring the Rocking Curve).
◆ A thin film sample at very shallow (small 2Theta) angles (section 4.6 -
Performing a Reflectivity Measurement). For this part we assume that a
beam attenuator is present in the system (as it should be).
Before performing the procedures that are described in this chapter, define a user
“My Name” as described in Chapter 2 of this guide.
4.2 PREPARATION
• Switch the system on by pressing the “Power On” button on the
instrument.
• Wait until the voltage and current that are shown on the control panel have
increased to 30 kV and 10 mA. The system is now ready for use.
• If the voltage and current do not increase to these values, refer to the
relevant hardware User’s Guide.
4.3 STARTING THE SOFTWARE

• Enter the user name and password: “My Name” and “password”
• Click OK.
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• From the menu, select User Settings > Options to check that the system is
set up to use the correct diffraction mode (in this case, Single Crystal
Mode).
• Choose the mode Single crystal.

• Click OK.
4.4 DESCRIBING YOUR HARDWARE

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4.4.1 Defining the Hardware Family

(X’Pert PRO MRD in this example) from the Hardware family
drop-down box.
NOTE: If the system has not been previously initialized an initialization wizard
will start. If this happens, just follow the instructions on the screen.

what you have.
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4.5 SETTING UP TWO CONFIGURATIONS

In this example we have a diffractometer with a requirement for two configurations:
1. A rocking curve - triple axis configuration with two detectors.
2. A configuration containing the remaining diffracted beam optics.
The next step is to set up two new configurations, one with two beam paths, and the
other with one beam path.
4.5.1 First Configuration:

Rocking Curve – Triple Axis
4.5.1.1 Removing the unnecessary beam path

If you have an MRD-type system with diffracted beam optics other than rocking
curve - triple axis PreFIX module, you will see an extra diffracted beam path.
Diffracted beam path 1 and Diffracted beam path 3 cannot be used together because
both of them have an offset of 0.000º. In this example, we will remove Diffracted
beam path 3.
• Click Diffracted beam path3 (scroll down if necessary).
• Click Delete.
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4.5.1.2 Defining the rest positions

• Click on the Manual load positions branch of the tree.
• Click on the Manual Load Positions button.
• Set the check boxes as shown below.
• Click OK.
4.5.1.3 Selecting your optical components

configuration.
.
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Offsets frame.
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4.5.1.4 Saving the configuration

• From the menu, select File > Save to save this configuration.
enter “My Triple Axis”.
• Click OK.

If you have other optics in your system, go to Section 4.5.2, “Second Configuration:
Other Optics”).
If not, go directly to Section 4.6, “Measuring the Rocking Curve”.
4.5.2 Second Configuration: Other Optics

4.5.2.1 Defining the Hardware Family

(X’Pert PRO MRD in this example).
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what you have.
4.5.2.2 Removing the unnecessary beam paths

• This configuration uses Diffracted beam path3 (the beam path that was
not used in the previous setup). We must now remove the other two beam
paths from this configuration.
• From the tree, select Diffracted beam path1. Click on the Delete button
to remove this beam path from the configuration.
• From the tree, select Diffracted beam path2. Click on the Delete button.
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4.5.2.3 Defining the rest positions

• Click on the Manual load positions branch of the tree.
• Click on the Manual Load Positions button.
• Set the check boxes as shown below.
• Click OK.
4.5.2.4 Selecting your optical components

configuration.
.
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Offsets frame.
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4.5.2.5 Saving the configuration

• From the menu, select File > Save to save this configuration.
enter “My Other Optics”.
• Enter the description of the configuration in the Description field. In this
example, enter “Configuration for other analyses for QSG”.
• Click OK.
4.6 MEASURING THE ROCKING CURVE

• Select your configuration (in this example: “My Triple Axis”).
• Select the diffracted beam path (in this example: “Diffracted beam
path2”).
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• Click OK.

• Click OK.
• If you have an In-plane type system and it has not been initialized, a
message appears. Follow the procedure that is given on the screen in order
to initialize the system.
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4.6.2 Setting the Tube Voltage and Current

the tree.
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• Click OK.
4.6.3 Preparing the Beam Paths
4.6.3.1 Preparing the Incident Beam Path

• Click on the Incident Beam Optics tab.
• In the tree, double-click on the Incident beam path branch.
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• In the Incident Beam Optics window, select the PreFIX Module tab.
• Select the module that you want to use from the Type drop-down list.
• Click Apply.

• To enter the remaining items of your incident beam setup, select the
relevant tabs of the Incident Beam Optics window and select your items
from the applicable drop-down lists. Click Apply before selecting another
tab.
• After you have entered all items of your incident beam setup, click OK to
close the Incident Beam Optics window.
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4.6.3.2 Preparing the Diffracted Beam Path

• Click on the Diffracted Beam Optics tab.
The Diffracted beam path2 branch of the tree is written in bold. This indicates that
Diffracted beam path2 is the active beam path.
• In the tree, double-click on the Diffracted beam path2 branch to open the
Diffracted Beam Optics window.
• In the Diffracted Beam Optics window, select the PreFIX Module tab.
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• Click Apply.

• To enter the remaining items of your diffracted beam setup, select the
relevant tabs of the Diffracted Beam Optics window and select your
items from the applicable drop-down lists. Click Apply before selecting
another tab.
• After you have entered all items of your diffracted beam setup, click OK
to close the Diffracted Beam Optics window.
4.6.4 Sample Positioning

Because we don’t know exactly where the sample is mounted on the stage, we must
use the Z-position dial gauge to accurately pinpoint the position of the sample.
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• In the Instrument Settings tab, double-click on the Positions branch of

the tree.
• In the Instrument Settings window, select the Position tab.

• If you haven’t already done so, mount the sample (silicon 111 single
crystal).
To position the sample stage so that you can read the Z-position dial gauge and not
damage the sample (in this example), proceed as follows:
• In the Chi field, enter “0”.
• In the Z field, enter “0”.
• Click Apply.
• Mount the Z-position dial gauge (to be used as a pointer to the middle of
the sample). Refer to the relevant hardware Reference Manual for dial
gauge mounting information.
Page 4 - 20
• Adjust the values of the X and Y fields until the pointer of the gauge is
over the center of the sample.
NOTE: To move the sample, click Apply after you have changed a value.
• Carefully change the Z-position (using the Z field) until the sample is
located exactly at the center of the goniometer (0 on the big scale of the
dial gauge and 1 on the small scale).
• Note the new Z-position (in this example it was “7.226”).
• Change the Z-position to 0 to prevent damaging the sample.
• Remove the dial gauge.
• Set the sample stage to a vertical position (Chi = 0°).
• Set the Z-position to the value just noted.
• Click OK to close the Instrument Settings window.
4.6.5 Manual Scan

Now we’ll do a manual scan to “find” a reflected X-ray beam.
• From the menu, select Measure > Manual Scan.
• In the Scan axis frame, select Omega from the drop-down box.
• In the Scan mode frame, select the Continuous radio button.
Page 4 - 21
• In the Instrument Settings tab of the instrument control window,

double-click on the Positions branch of the tree.
• In the Unit cell field, enter “Si[111]”.
• In the h k l field, enter “1 1 1”
(be sure to enter this as 1, space, 1, space, 1).
NOTE: The position information will be automatically calculated and entered
when you leave the h k l field.
• In the Prepare Manual Scan window, click Start.
The result (count rate) varies considerably according to individual systems.
Page 4 - 22
4.6.6 Adjusting the Goniometer Position

• Right-click somewhere in the graph.
• From the context menu, select Move Mode.
• Drag the hairline to the center of the peak. The goniometer moves to that
angle.
• Right-click in the graph, and from the context menu select Zoom Mode.
• Zoom in.
• Inspect the position of the hairline.
Page 4 - 23
• If necessary, go back to Move Mode and move the hairline into the middle
of the peak.
• Close the Manual Scan window and the Prepare Manual Scan window
(click to close the windows).
4.6.7 Optimize Chi
4.6.7.1 Prepare Optimize Program

• From the Program type drop-down list, choose Optimize Program.
• Click OK.
Page 4 - 24
• Select the Optimize Chi radio button.

• In the Optimize mode frame and the 2nd axis Chi frame, set the
parameters as specified in Table 1.
Table 1 Optimize Program Parameters
Parameter Value
Optimize mode frame
Range (°) 0.090
Step size (°) 0.01
Time per step (s) 0.5
2nd axis Chi frame
Range (°) 4
Step size (°) 0.5
Page 4 - 25
• Click Description.
• Enter the description of the program (in this example: “Example for Quick
Start Guide”).
• Click OK.
• In the File name field, enter the file name (in this example: “My Optimize
Program”).
• Click Save.
• Click to close the Prepare Optimize Program window.
Page 4 - 26
4.6.7.2 Optimizing the Sample Orientation

• Select the desired program (in this example: “My Optimize Program”).

ID: Si(111) Sample
Name: Standard High Resolution Sample
• Click OK.
Page 4 - 27
The sample orientation is now automatically optimized. This is done by performing

a series of Omega scans at various fixed Psi settings.
After all the scans are finished, the cradle automatically moves to the optimal Psi
position and the shutter will be closed (the shutter number on the control console is
no longer shown).
The optimized Psi position can be seen on the instrument control window on the
Instrument Settings tab, and on the status bar.
From the menu, select User Settings > Status Bar to select the items that you want
to see on the status bar.
• Click to close the Scan window.
4.6.8 Measuring
4.6.8.1 Prepare Rocking Curve Program

• From the Program type drop-down list, choose Relative scan.

• Click OK.
Page 4 - 28
• Check that you have the correct configuration and diffracted beam path
(in this example: “My Triple Axis” and “Diffracted beam path2”).
• In the Scan axis frame, select Omega from the drop-down list.
• On the Scan Properties tab, enter the following parameters:
Range: 0.189
Step: 0.001
Time per step: 0.5
• Click Description and enter the description of the program (in this
example: “Example for Quick Start Guide”).
• Click OK.
• Enter the name of the program in the File name field. In this example,
enter “My Rocking Curve Program”.
• Click Save.
• Click to close the Prepare Relative Scan window.
Page 4 - 29
4.6.8.2 Measure the Rocking Curve

• From the Measurement type drop-down box, select Relative scan.
• Select the desired program (in this example: “My Rocking Curve
Program”).

ID: Si(111) Sample
Name: Standard High Resolution Sample
Page 4 - 30
• Click OK.
After a while the scan window will appear. Shortly afterwards, your rocking curve
measurement will be completed. At this time the goniometer will return to its
manual load positions.

• To disconnect from the instrument, select Instrument > Disconnect and
click OK.
Page 4 - 31
4.7 PERFORMING A REFLECTIVITY

MEASUREMENT

• Select your configuration (in this example: “My Other Optics”).
• Click OK.

• Click OK.
Page 4 - 32

4.7.2 Setting the Tube Voltage and Current

the tree.

• Click Apply.
• Click OK.
Page 4 - 33
4.7.3 Preparing the Beam Paths
4.7.3.1 Preparing the Incident Beam Path

• Click on the Incident Beam Optics tab.
• In the Incident Beam Optics window, select the PreFIX Module tab.
• Click Apply.

• To enter the remaining items of your incident beam setup, select the
relevant tabs of the Incident Beam Optics window and select your items
Page 4 - 34
from the applicable drop-down lists. Click Apply before selecting another
tab.
• After you have entered all items of your incident beam setup, click OK to
close the Incident Beam Optics window.
4.7.3.2 Preparing the Diffracted Beam Path

• Click on the Diffracted Beam Optics tab.
The Diffracted beam path3 branch of the tree is written in bold. This indicates that
Diffracted beam path3 is the active beam path.
• In the tree, double-click on the Diffracted beam path3 branch.
Page 4 - 35
• In the Diffracted Beam Optics window, select the PreFIX Module tab.
• Select the module that you want to use for this parallel beam experiment
from the Type drop-down list.
• Click Apply.

Page 4 - 36
• To enter the remaining items of your diffracted beam setup, select the
relevant tabs of the Diffracted Beam Optics window and select your
items from the applicable drop-down lists. Click Apply before selecting
another tab.
• After you have entered all items of your diffracted beam setup, click OK
to close the Diffracted Beam Optics window.
• Perform the actions as instructed and click OK.
4.7.4 Mounting the Sample

Because we don’t know exactly where the sample is mounted on the stage, we must
use the Z-position dial gauge to accurately pinpoint the position of the sample.
• In the Instrument Settings tab, double-click on the Positions branch of
the tree.
Page 4 - 37
• If you haven’t already done so, mount the sample (silicon 111 single
crystal). For better access to the sample stage during mounting of the
sample, you can send the goniometer to a comfortable position with the
Move to Manual Loading Position button.
To position the sample stage so that you can read the Z-position dial gauge and not
damage the sample (in this example), proceed as follows:
• In the Z field, enter “0”.
• Click Apply.
• Mount the Z-position dial gauge (to be used as a pointer to the middle of
the sample). Refer to the relevant Reference Manual for dial gauge
mounting information.
• Adjust the values of the X and Y fields until the pointer of the gauge is
over the center of the sample.
NOTE: To move the sample, click Apply after you have changed a value.
• Carefully change the Z-position (using the Z field) until the sample is
located exactly at the center of the goniometer (0 on the big scale of the
dial gauge and 1 on the small scale).
Page 4 - 38
• Note the new Z-position (in this example it was “7.984”).

• Change the Z-position to 0 to prevent damaging the sample.
• Remove the dial gauge.
• Set Chi to 0°.
• Set 2Theta to 0°.
• Click Apply.
4.7.5 Positioning the Sample

In order to ensure that the sample is at the precisely correct height, we will first
measure the output of the direct X-ray beam, and then move the sample up until the
count rate is exactly half the previously measured level (= sample in the middle of
the beam).
• In the instrument control window, click on the Incident Beam Optics tab.
• In the Incident Beam Optics window, select the Beam Attenuator tab.
• Select the Do not switch from the Usage drop-down list.
• Put a check mark in the Activated check box.
• Click Apply.
• Click OK.
Page 4 - 39
4.7.6 Calibrating the Attenuation Factor

If you have a calibrated beam attenuator, you can skip this section.
If you are using an uncalibrated beam attenuator, you must calibrate the attenuation
factor as described in this section before you continue.
An uncalibrated beam attenuator shows a beam attenuation factor of 20.00.
• Make sure that the status bar is switched on and shows the count rate.
• If the status bar is not shown, select View > Status Bar > Top or Bottom.
• If the count rate is not shown, select User Settings > Status Bar, choose
Count rate for one of the five columns, and click OK.
Page 4 - 40
• In the Scan axis frame, select 2Theta from the drop-down box.
• Click Start.
• Check the count rate that is shown on the status bar.
• If the count rate is above 1000, go to the move mode (right-click in the
graph) and move the hairline to a position on the peak where the count rate
is below 1,000 (but preferably above 500).
• Close all of the manual scan windows by pressing on each of them.

• In the Incident Beam Optics tab of the instrument control window, set the
beam attenuator to Do not switch and De-activated, and click OK.
Page 4 - 41
• Open the shutter by pressing the button on the toolbar.

• Double-click on the Beam Attenuator branch of the tree view.
• Take a note of the intensity shown in the status bar, activate the attenuator
and click Apply. Then note the intensity again (in this example:
“108000”). The attenuation factor is the second intensity divided by the
first intensity.
• Set your beam attenuator to switch At Pre-set Intensity, change the
Activate level to 500000 and click OK.
• From the menu, select System Settings > Beam Attenuation Factors.
• Click New and define the attenuation factor for your attenuator (in this
example: “165.9”).
Page 4 - 42
• Click OK.
• In the instrument control window, select the Instrument Settings tab.
• Double-click on the Shutter, de-select Shutter open and click OK.
4.7.7 Aligning the Sample
4.7.7.1 Manual Scan

We will now make a short manual scan to ensure that the beam is located exactly at
0° 2Theta (= maximum count rate).
• In the Instrument Settings tab of the instrument control window, check
that the positions for 2Theta, Omega, Phi and Psi are all zero and
click OK.
Page 4 - 43
• Enter the parameters as given in the table below.

Table 2 Manual Scan Parameters
Parameter Value
Scan axis 2Theta
Scan mode Continuous
Range 0.9900°
Step size 0.0100°
Time per step 0.50 s
Scan speed 0.020000°/s
• Click Start.
After a while, a manual scan result window will appear.
Page 4 - 44
• Right-click somewhere in the graph.

• From the context menu, select Move Mode.
• Drag the hairline to the center of the peak.
• Click Start.
• If necessary, continue moving the hairline and clicking Start until you
have moved the hairline to the center of the peak.
• Make a note of the count rate at the peak. You can see the count rate at the
peak by moving the + cursor to the top of the peak and reading the count
rate in the status bar (approximately 770 in this example).
• Close the Manual Scan window and the Prepare Manual Scan window
(click to close the windows).
• In the Incident Beam Optics tab, double-click on Beam Attenuator
Page 4 - 45
• Set Usage to Do not switch and put a check mark in the Activated check
box.
• Click OK.
• Open the shutter by pressing the button on the toolbar.

• Change the Z-position until the count rate that is shown in the status bar is
approximately half the value that you noted when you were moving the
hairline in the previous step.
In this example, we have a count rate of 770. We now must move the sample until
the measured count rate is half that value (385). This is an iterative process as with
the following example:
- Enter 7.5 into the Z field and click Apply, result = 770
- Enter 7.798 into the Z field and click Apply, result = 385.
• When you are satisfied that you are at half the count rate, click OK.
• In the Scan axis frame, select Omega from the drop-down box.
• Click Start.
Page 4 - 46
• Right-click somewhere in the graph and from the context menu, select
Move Mode.
• Drag the hairline to the position with the highest intensity. Wait until the
goniometer has moved to that angle.
• Minimize the Manual Scan window and the Prepare Manual Scan
window.
• Once again, change the Z-position until the count rate that is shown in the
status bar is approximately half the value that you noted earlier (in this
example: 385), and click OK.
Page 4 - 47
• Restore the Manual Scan window and right-click on the graph.

• From the context menu, select Start to re-do the scan.
• If necessary, move the hairline to the center of the peak again.
There are three criteria that must be met at this stage:

◆ The peak should be triangular (the scan above is a good example). You can
zoom in on the peak for a closer inspection to make sure that it really is
triangular.
◆ The hairline must be in the center of the peak.
◆ The count rate at the center of the peak (where the hairline is) should be
half the original value that you noted.
If your peak does not meet all three criteria, continue with the iterative procedure
until it does.
Page 4 - 48
4.7.7.2 Setting the Sample Offset

At this time you must tell the goniometer exactly where the surface of the sample is
parallel to the incident beam (“zero” the goniometer).
• From the menu, select User Settings > Sample Offsets.
• In the Current position column, set 2Theta and Omega to 0.

This creates a sample offset.
• Click OK.
• Close both of the Manual Scan windows (click to close the windows).
4.7.8 Creating a Measurement Program

• From the Program type drop-down list, choose Absolute scan.
• Click OK.
Page 4 - 49
• In the Scan axis frame, select Gonio from the drop-down list.
• On the Scan Properties tab, enter the following parameters:
Start angle: 0.3°
End angle: 1.5°
Step size: 0.005°
Time per step: 5 s
• Click Settings.
Page 4 - 50
• In the tree, click on the Beam attenuator branch (under Incident beam
path).
• Select the beam attenuator that your system has from the drop-down list
(in this example: “Attenuator Ni 0.125 mm automatic”).
• Check that Attenuation factor has the correct value.
• Set Usage to At pre-set intensity, Activate level to 500000 cps and
De-activate level to 200000 cps.
• Click Apply and then OK.
• From the menu, select File > Save As to save the program.
• Enter a file name for the program (in this example: “My Reflectivity
Program”) and click Save.
• Click to close the Prepare Absolute Scan window.
Page 4 - 51
4.7.9 Measuring the Reflectivity Curve

• Select My Reflectivity Program.

ID: Thin Film Sample
Name: Cr layer
• Click OK.
Page 4 - 52
4.7.10 Changing the Axes

Once the scan has started, change the scale to “logarithmic” to show the reflectivity
curve better.
• Right-click in the graph window and from the context menu, choose Axes.
• Set Units to Counts and Type to Logarithmic.

• Put a check mark in the Automatic change of intensity scale check box,
and in the Automatic X-scaling check box.
• Click Close.
The resulting curve can be used to calculate the thickness of the film measured.
Page 4 - 53

• To disconnect from the instrument, select Instrument > Disconnect and
click OK.
Page 4 - 54

Quick Start Guide: Data Collector

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Quick Start Guide: Data Collector

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DATA COLLECTOR

Quick Start Guide

Quick Start Guide

EDITION NOTICE: 4022 339 20070, November 2012

1.2 21 CFR PART 11 SUPPORT MODE

1.3 CONVENTIONS USED

Starting to Work with Data Collector

Starting to Work with Data Collector

2.2 CONVERTING THE DATABASE

• Wait until the following message appears.

2.3 STARTING DATA COLLECTOR

• Double-click on the Data Collector icon .

• Type in the following information:

2.4 CREATING A NEW USER

• Enter the following information:

2.5 ORGANIZING YOUR RESULT DATA

2.6 SPECIFYING THE REPORT FOLDER

• Click on the button to select the report folder, in this example:

Using Data Collector with Empyrean

3.3 STARTING THE SOFTWARE

• Double-click on the Data Collector icon .

3.4 DESCRIBING YOUR HARDWARE

3.4.1 Defining the Hardware Family

• In the System identification frame, select your hardware family

• Wait until the Connecting to instrument pop-up disappears. The system

3.4.2 Defining the Configuration

• Click on the Next button. The Goniometer/Sample stage frame appears.

• Check that the information displayed here is correct. If necessary, adjust

3.4.3 Selecting your Optical Components

NOTE: If you have X-ray Mirror or Hybrid monochromator PreFIX modules in

3.4.4 Saving the Configuration

• Close the Define Configuration window by clicking .

3.5 DEFINING A MEASUREMENT PROGRAM

3.5.1 Defining the Measuring Program

• If the value in the Configuration frame is not My Spinner, select

Table 1 Prepare Absolute Scan Parameters

3.5.2 Defining the Instrument Settings for the

• Select Spinning, and if appropriate, a Revolution time of 1 s.

Table 2 Incident Beam Path Parameters

Table 3 Diffracted Beam Path Parameters

• Click OK to apply the settings to your program.

3.5.3 Saving the Measurement Program

3.6 PERFORMING THE MEASUREMENT

3.6.1 Connecting to the Instrument

• Carefully check if these assumptions are correct.

• In the Instrument Settings tab, double-click on the Generator branch of

• In the Tension (kV) field, enter “45”.

3.6.2 Mounting the Sample

3.6.2.1 No sample spinner

3.6.2.2 Sample spinner, but no sample changer

3.6.2.3 Sample changer, positioned in the corner

3.6.2.4 Sample changer, ready for use

3.6.3 Starting the Measurement

• Select the desired program (in this example: “My Program”).

• In the File frame, enter:

• If a message appears that tells you to do something, perform the actions as

Using Data Collector

4.7.5 Positioning the Sample ....................................................................4 - 39

Using Data Collector

4.3 STARTING THE SOFTWARE

• Double-click on the Data Collector icon .

• Choose the mode Single crystal.

4.4 DESCRIBING YOUR HARDWARE