Rigaku MiniFlex 600 User manual

Benchtop X-
ray Diffractometer
Instruction Manual
This image is an example of MiniFlex series. The actual product may differ from the image.

This manual describes the correct use of the product as well the usage precautions to be observed. To
obtain full-expected performance from the product, thoroughly read this manual.
Also, store this manual at an easily accessible place so that you can promptly refer to it whenever
it is necessary.
The contents of this manual are subject to change without prior notice.
This manual described in it may not be disclosed to a third party or copied, in whole or in part, without
the written consent of Rigaku Corporation.
In no event will Rigaku Corporation be responsible for the results of the use of this manual.
As a rule, one set of the instruction manual has to be purchased for each product.
If there are any missing or incorrectly collated pages in the delivered instruction manual, please
contact the sales representative who you purchased the instrument from for instruction manual
replacement.
Windows is a registered trademark of Microsoft Corporation in the United States and other countries.
The ® marks have been omitted.
Adobe, the Adobe logo, and Reader are either registered trademarks or trademarks of Adobe Systems
Incorporated in the United States and/or other countries. The ™ and ® marks have been omitted.
The names of actual companies and products mentioned herein may be the registered trademarks or
trademarks of their respective owners.

MiniFlex 600: Benchtop X-ray Diffractometer i
Contents
Overview .............................................................................................................1
Overview of MiniFlex 600........................................................................................... 1
Optical System using SC ........................................................................................... 2
Configuration ......................................................................................................3
Standard Configuration ............................................................................................... 3
Names of Parts......................................................................................................... 4
List of Shipped Items ................................................................................................ 8
Specifications.......................................................................................................9
X-Ray Generator ...................................................................................................... 9
Tube shield .............................................................................................................. 9
Goniometer (Angle measuring device) ........................................................................ 9
Detector (SC)......................................................................................................... 10
Counting control circuit (ECP)................................................................................. 10
Radiation enclosure ................................................................................................ 10
Cooling-Water Unit ................................................................................................ 10
X-ray tube ..............................................................................................................11
Computer (reference specifications)...........................................................................11
Standard Software ...................................................................................................11
Optional accessories ............................................................................................... 12
D/teX Ultra High-speed 1D Detector (Optional)......................................................... 12
Installation Condition ........................................................................................13
Installation Room ................................................................................................... 13
Environmental Conditions of Installation Room ......................................................... 13
Preparing Power Supply.......................................................................................... 14
Cooling water ........................................................................................................ 15
Drainage ............................................................................................................... 15
Others ................................................................................................................... 15
Installation of MiniFlex600 ................................................................................17
Unpacking............................................................................................................. 17
Installing the X-Ray tube......................................................................................... 17
Connecting the Cooling Water Hose ......................................................................... 18
Installing the Scintillation Counter (SC) .................................................................... 19
Installing the D/teX Ultra (Optional)......................................................................... 22
Installing the Beam Stop ......................................................................................... 24
Installing and retracting the variable knife edge.......................................................... 24
Installing the variable knife edge ....................................................................... 24
Retracting the slider ......................................................................................... 26

ii MiniFlex 600: Benchtop X-ray Diffractometer
Installing the DS and IHS (Length limiting)............................................................... 27
Connecting the power cable..................................................................................... 27
Connecting with Computer...................................................................................... 27
Installing the Software ............................................................................................ 28
Setting and Adjustment...................................................................................... 29
Types of Soller Slit, Confirming the Soller Slit........................................................... 29
Types of incident Soller slit............................................................................... 29
Confirming the incident Soller slit ..................................................................... 29
Types of receiving Soller slit............................................................................. 30
Optics Alignment (Required for Periodic Inspection or Installing X-Ray Tube).............. 31
Optics alignment (for SC)................................................................................. 31
Optics alignment (D/teX Ultra) ......................................................................... 42
Optics alignment (for D/teX only) ..................................................................... 50
HV/PHA Adjustment of Scintillation Counter (SC)..................................................... 64
Discriminator Value Setting by D/teX Ultra............................................................... 67
Automatic adjustment of discriminator value ...................................................... 67
Directly entering the D/teX Ultra adjustment value.............................................. 69
Initial Setting of the Measurement Environment (Required When the X-Ray Tube Type Has
Been Changed)....................................................................................................... 71
Data Measurement and Setting Procedure for Real-Time 2 theta Axis Correction (Required
for Initial Setup or Periodic Inspection)..................................................................... 72
Startup and Shutdown (Daily routine)................................................................77
Starting Up the System............................................................................................ 77
Shutting Down the System ...................................................................................... 78
Measurement of Samples (Daily routine) ............................................................79
Preparing the Sample Plate ...................................................................................... 79
Preparation of powder sample on aluminum sample plate ..................................... 79
Preparation of block sample on aluminum sample plate........................................ 81
Preparation of powder sample on glass sample plate ............................................ 81
Cleaning spilled or deposited powder sample ...................................................... 82
Slit system............................................................................................................. 83
Slit Correction........................................................................................................ 83
Measurement with MiniFlex Guidance...................................................................... 85
Maintenance ......................................................................................................91
X-Ray Tube and Scintillation Counter (SC) ............................................................... 91
Replacing the X-ray Tube (Procedures required when cleaning filter or replacing tube) 91
Removing and installing the X-Ray tube ............................................................ 91
Disassembling the X-ray tube and cleaning the filter............................................ 93
Cleaning and Further Information............................................................................. 94
Confirming the Alarm Information ........................................................................... 95

MiniFlex 600: Benchtop X-ray Diffractometer iii
Installing the Optional Sample Attachment ........................................................97
Installing the Counter Monochromator (Optional) .............................................99
Installing the Counter Monochromator.................................................................... 100
Optics alignment and notes on monochromator ........................................................ 103
Arrangement of slits ............................................................................................. 104
Item No. 2005L101 / L102 / L201 / L202 / L301 / L302 / L401 / L402
Manual No. ME14992A03
2014. 02 (3rd Edition)

MiniFlex 600: Benchtop X-ray Diffractometer 1
Overview
Before starting to use the MiniFlex 600 Benchtop X-ray Diffractometer (hereon
called MiniFlex 600), be sure to read this instruction manual thoroughly. Also, be
sure to read the "Guidelines for safe use of the Benchtop X-ray Diffractometer"
(ME11594*).
Overview of MiniFlex 600
The MiniFlex 600 is a successor of the MiniFlex Benchtop X-ray Diffractometer
(XRD) series. The MiniFlex 600 significantly improved its basic performance
while maintaining the compact size of MiniFlex series products.
Characteristics of MiniFlex 600
・By incorporating the real-time angle correction system, compact and wide-area
scintillation counter (hereafter called SC) which is equivalent to intensity of
150%, counter monochromator (optional) and other features, MiniFlex 600 has
significantly enhanced its basic specifications as a powder XRD system in terms
of angle accuracy, intensity and P/B ratio. Thus, a high quality data can be
obtained from a XRD system completed in a compact enclosure.
・An X-ray generator of 600 W (40 kV - 15 mA) enables 1.3 times higher output
than the existing model.
・The system is a location-free tool that can readily be transported and installed in a
relatively small indoor or outdoor space.
Optional accessories to enable good quality high speed measurements
・The MiniFlex 600 can be used for a variety of applications; starting from
diffraction pattern comparison of polycrystalline materials (such as powder
samples and metal plates) and up to qualitative & quantitative analyses as well as
quality control management of raw materials and products. Optional softwares*
for these purposes are available.
・Optional sample attachments, such as sample rotation attachment*, sample
changer*, and general atmosphere separator* can be used to improve quantitative
measurement accuracy or to automate the measurement.
・The counter monochromator* cuts X-rays (fluorescence X-rays, etc.) other than
the characteristic X rays (CuKα) used for the analysis. When the counter
monochromator is used, the data with low background and high P/B ratio can be
obtained.
・By replacing the SC with D/teX Ultra high-speed 1D detector*, a measurement
with 100 times higher intensity than SC, under the same slit conditions, is
enabled.
Items with * are optional.

Overview
2MiniFlex 600: Benchtop X-ray Diffractometer
Optical System using SC
Fig. 1.1 outlines the optical system of MiniFlex 600 using the scintillation counter.
This optical system adopts focusing geometry used in powder XRD generally and
irradiates the sample with divergent X-rays limited by a divergent slit. The features
of this geometry are the high diffracted X-ray intensity, which is provided by
diffracted rays from the sample concentrating on the RS (Receiving slit), and
high-resolution analysis patterns.
An X-ray beam from the X-ray tube (focal point F) is emitted in the direction 6 °
below the horizontal direction. With respect to this incident beam, the sample is
rotated by θ and the detector by 2θ. The diffraction pattern is obtained by rotating
2θ /θ repeatedly and measuring the diffracted rays from the sample.
A counter monochromator is available as an optional accessory. This accessory is
placed behind the RS (further side from the sample) shown in Fig. 1.1. The counter
monochromator cuts not only the Kβrays but also fluorescent X-rays and
continuous X-rays, which have an adverse effect for detecting micro peaks, thus
lowers the background and offers data with a higher P/B ratio. (Refer to “Installing
the Counter Monochromator (Optional)”).
Although omitted in Fig. 1.1, an auxiliary variable DS (Divergence slit) is placed
between the DS and Soller slit. This auxiliary slit helps to achieve the DS width of
0.1 mm at the time of optical axis adjustment. It also limits the radiation width to
"sample width + α" to prevent the irradiated area to spread outside the sample
without limit, thus improves the P/B ratio at low angles. The slit functions in the
background, and there is no need to concern about it on a daily basis.
DS (Divergence slit) is a slit to determine the width of the irradiation. Width of
1.25° and 0.625° are available. The 0.625°DS slit is used for measuring a sample
whose main peaks concentrate at low angles (2θ < 20°), such as organic sample.
For the RS (Receiving slit), the 0.3 mm RS is available. SS (Scattering slit) is a slit
to cut the scattered radiation from outside of the sample. Usually, the SS with the
same receiving angle as DS is used.
The Soller slits on the incidence and receiving sides limit the diffracted rays to
spread out in vertical direction (the top and bottom direction of this manual is the
vertical direction in the figure), thereby preventing the peak resolution from
decreasing.
Fig. 1.1 Outline of the optical geometry

MiniFlex 600: Benchtop X-ray Diffractometer 3
Configuration
Standard Configuration
X-ray generator (XG): Power source for X-ray generation
Tube shield: X-ray tube holder
Goniometer: Measurement unit at 2θdiffraction angle
Detector (SC): Scintillation counter
Counting control circuit (ECP): Counting and measurement controller
Radiation enclosure: Enclosure cabinet of the main unit that
provides protection from radiation
Flow rate detector: For monitoring flow rate of cooling water.
X-ray tube
LAN cable
Computer (for Japanese market only):
PC, Printer
An X-ray tube and a computer (PC, etc.) are required to use this equipment.
These components may be required to be prepared by the user or distributor due
to warranty issues.
If an auto-transformer or an external heat exchanger is required, contact the sales
representative who you purchased the instrument from.

Configuration
4MiniFlex 600: Benchtop X-ray Diffractometer
Names of Parts
(a) MiniFlex600 main unit
(b) Block diagram
Fig. 2.1 Appearance and block diagram of MiniFlex 600 (including optional components)
Heat
exchanger
Scan
HV
Detector(SC)
Sample
Water
cooling
Data output
2θ
X-ray
X-ray tube
Electronic
circuit panel
(ECP)
Angle control
Goniometer
Cable
High voltage
generator
Computer
X-ray generator