TA Instruments DISCOVERY XENON FLASH User manual

DISCOVERY XENON FLASH
DXF-200
Getting Started Guide
Revision AIssued September 2020

DXF-200 Getting Started Guide Page 2
Notice
The material contained in this manual, and in the Help for the software used to support this instrument, is
believed adequate for the intended use of the instrument. If the instrument or procedures are used for pur-
poses other than those specified herein, confirmation of their suitability must be obtained from TA Instru-
ments. Otherwise, TA Instruments does not guarantee any results and assumes no obligation or liability.
TA Instruments also reserves the right to revise this document and to make changes without notice.
TA Instruments may have patents, patent applications, trademarks, copyrights, or other intellectual prop-
erty covering subject matter in this document. Except as expressly provided in written license agreement
from TA Instruments, the furnishing of this document does not give you any license to these patents,
trademarks, copyrights, or other intellectual property.
TA Instruments Operating Software, as well as Module, Data Analysis, and Utility Software and their asso-
ciated manuals and Help, are proprietary and copyrighted by TA Instruments. Purchasers are granted a
license to use these software programs on the module and controller with which they were purchased.
These programs may not be duplicated by the purchaser without the prior written consent of TA Instru-
ments. Each licensed program shall remain the exclusive property of TA Instruments, and no rights or
licenses are granted to the purchaser other than as specified above.
TA Instruments can accept no liability for loss or damage, however caused, arising from the faulty or
incorrect use of its products.TA Instruments shall not be liable for any damages caused by interactions
between exogenous materials (e.g. chemicals) and parts of the instrument. This includes interactions of
gaseous, liquid or solid materials with parts of the instrument.
©2020 by
TA Instruments — Waters LLC
159 Lukens Drive
New Castle, DE 19720

DXF-200 Getting Started Guide Page 3
Introduction
Important: TA Instruments Manual Supplement
Please click the TA Manual Supplement link to access the following important information supplemental
to this Getting Started Guide:
• TA Instruments Trademarks
• TA Instruments Patents
• Other Trademarks
• TA Instruments End-User License Agreement
• TA Instruments Offices

DXF-200 Getting Started Guide Page 4
Notes, Cautions, and Warnings
This manual uses NOTES, CAUTIONS, and WARNINGS to emphasize important and critical
instructions. In the body of the manual these may be found in the shaded box on the outside of the page.
NOTE: A NOTE highlights important information about equipment or procedures.
CAUTION: A CAUTION emphasizes a procedure that may damage equipment or cause loss of data
if not followed correctly.
MISE EN GARDE: UNE MISE EN GARDE met l'accent sur une procédure susceptible d'endom-
mager l'équipement ou de causer la perte des données si elle n'est pas correctement suivie.
Please heed the warning labels and take the necessary precautions when dealing with those parts of the
instrument. The DXF Getting Started Guide contains cautions and warnings that must be
followed for your own safety.
Safety
Instrument Symbols
The following label is displayed on the instrument for your protection:
Please heed the warning labels and take the necessary precautions when dealing with these areas. This Get-
ting Started Guide contains cautions and warnings that must be followed for your own safety.
A WARNING indicates a procedure that may be hazardous to the operator or to the environment
if not followed correctly.
Un AVERTISSEMENT indique une procédure qui peut être dangereuse pour l'opérateur ou
l'environnement si elle n'est pas correctement suivie.
Symbol Explanation
This symbol indicates that a hand crush hazard is present. Take care when placing
the top module onto the bottom module.
Ce symbole indique la présence d'un risque de broyage de main. Prenez soin de
placer le module supérieur sur le module inférieur.
This symbol indicates that a hot surface may be present. Take care not to touch
this area or allow any material that may melt or burn to come in contact with this
hot surface.
Ce symbole indique la présence possible d'une surface chaude. Prenez soin de ne
pas toucher cette zone ou de laisser un matériau susceptible de fondre ou de brûler
entrer en contact avec cette surface chaude.

DXF-200 Getting Started Guide Page 5
Warnings
Electrical Safety
Liquid Nitrogen Safety
The furnace uses the cryogenic (low-temperature) agent, liquid nitrogen, for cooling. Because of its low
temperature (–196°C [–321°F)]), liquid nitrogen may burn the skin. When you work with liquid nitrogen,
use the following precautions:
NOTE: Please adhere to your company’s safety guidelines for handling liquid nitrogen.
Wear goggles or a face shield, thermally insulated gloves large enough to be removed easily, and a rubber
apron. For extra protection, wear high-topped, sturdy shoes, and leave your pant legs outside the tops.
WARNING: The operator of this instrument is advised that if the equipment is used in a manner
not specified in this manual, the protection provided by the equipment may be impaired.
AVERTISSEMENT: L'utilisateur de cet instrument est prévenu qu'en cas d'utilisation contraire
aux indications du manuel, la protection offerte par l'équipement peut être altérée.
WARNING: Always unplug the instrument before performing any maintenance.
AVERTISSEMENT: Débranchez toujours l'instrument avant de procéder à la maintenance.
DANGER: This pulse source operates from a high voltage power supply. Do not override the
safety interlocks as they prevent contact with potentially lethal voltages.
DANGER: Cette source d'impulsion fonctionne à partir d'une alimentation électrique haute ten-
sion. N'annulez pas les dispositifs de sécurité car ils empêchent tout contact avec les tensions
potentiellement mortelles.
WARNING: Liquid nitrogen boils rapidly when exposed to room temperature. Be certain that
areas where liquid nitrogen is used are well ventilated to prevent displacement of oxygen in the
air.
AVERTISSEMENT: L'azote liquide bout rapidement lorsqu'il est exposé à la température ambi-
ante. Assurez-vous que les zones où l'azote liquide est utilisé sont bien aérées pour éviter le
déplacement de l'oxygène dans l'air.

DXF-200 Getting Started Guide Page 6
Thermal Safety
If the power has not come back on after a power failure, do NOT open the furnace. The temperature con-
trollers will not be displaying a temperature so you will not know what the temperature is inside the fur-
nace.
The test is over once a power failure occurs. This is no recovery method to restart the test at that point, but
all data is saved up until the power failure occurs.
Do not press any buttons on the front panel after a power failure, just start a test normally.
Chemical Safety
Lifting the Instrument
DANGER: Source instrument surfaces can be hot enough to cause discomfort when in contact
with the skin during a sample run. If you are conducting a subambient test, cold could also
cause injury. After running any type of experiment, you must allow the DXF system to return to
near room temperature before you touch the inner cell surfaces. Always use the available soft-
ware monitor to display temperature even after the termination of the test cycle.
DANGER: Les surfaces de l'instrument source peuvent être assez chaudes pour provoquer un
malaise au contact de la peau pendant l'analyse d'un échantillon. Si vous effectuez un essai à
basse température, le froid peut également provoquer des blessures. Après avoir effectué un
type d'expérience quelconque, vous devez laisser le système DXF revenir à la température
quasi ambiante avant de toucher les surfaces internes de la cellule. Utilisez toujours le moni-
teur logiciel disponible pour afficher la température même après la fin du cycle d'essai.
WARNING: In the event of a power failure, do NOT open the furnace.
AVERTISSEMENT: En cas de coupure de courant, N'ouvrez PAS le four.
WARNING: Do not use hydrogen, oxygen, or any other explosive gas in the DXF system. Only
inert gas, such as nitrogen or argon, should be used.
AVERTISSEMENT: N'utilisez pas d'hydrogène, d'oxygène ou tout gaz explosif dans le système
DXF. Seuls les gaz inertes comme l'azote ou l'argon doivent être utilisés.
WARNING: Use two people to lift and/or carry the instrument. The instrument is too heavy for
one person to handle safely.
AVERTISSEMENT: Demandez à deux personnes de soulever et/ou de porter l'instrument.
L'instrument est trop lourd pour qu'une seule personne le manipule en toute sécurité.

DXF-200 Getting Started Guide Page 7
Table of Contents
Introduction................................................................................................................................................. 3
Important: TA Instruments Manual Supplement ................................................................................... 3
Notes, Cautions, and Warnings .............................................................................................................. 4
Safety ...................................................................................................................................................... 4
Instrument Symbols ......................................................................................................................... 4
Warnings .......................................................................................................................................... 5
Electrical Safety ............................................................................................................................... 5
Liquid Nitrogen Safety .................................................................................................................... 5
Thermal Safety ................................................................................................................................ 6
Chemical Safety ............................................................................................................................... 6
Lifting the Instrument ...................................................................................................................... 6
Table of Contents........................................................................................................................................ 7
Chapter 1: Introducing the Discovery Xenon Flash................................................................................ 9
Overview ....................................................................................................................................................... 9
DXF System Components .......................................................................................................................... 10
Pulse Source Module ............................................................................................................................ 10
Environmental Modules and Solid State (Pins) Detector Assembly ................................................... 14
Instrument Specifications ........................................................................................................................... 15
Chapter 2: Installing the DXF System.................................................................................................... 17
Unpacking/Repacking ................................................................................................................................. 17
Installing the System ................................................................................................................................... 17
Inspecting the System .......................................................................................................................... 17
Choosing a Location ............................................................................................................................ 18
In .................................................................................................................................................... 18
On .................................................................................................................................................. 18
Near ............................................................................................................................................... 18
Away from ..................................................................................................................................... 18
Moving the Instrument ......................................................................................................................... 19
Connecting the Environmental Module to the Pulse Source Module .................................................. 20
DXF Back Panel ............................................................................................................................ 22
Connecting the Environmental Module to the Pulse Source ......................................................... 24
Setting Up System Communication with the Controller ...................................................................... 25
Connecting the Utilities ........................................................................................................................ 26
Connecting the Power .................................................................................................................... 26
Connecting the LN2 Lines ................................................................................................................... 26
Connecting the Gas Lines .................................................................................................................... 27
Chapter 3: Operating the DXF................................................................................................................ 28
Using the DXF ............................................................................................................................................ 28
Before You Begin ................................................................................................................................ 28
Startup and Shutdown Procedures .............................................................................................................. 29
Starting the DXF System ..................................................................................................................... 29
Shutting Down the DXF System .......................................................................................................... 29
Running a Discovery DXF Experiment ...................................................................................................... 30
Preparing the Sample ........................................................................................................................... 30
Sample Dimensions ....................................................................................................................... 30
Transparent or Translucent Materials ............................................................................................ 31
High Reflectance Samples ............................................................................................................. 31
Loading and Unloading the Sample ..................................................................................................... 33
Preparing the Instrument ...................................................................................................................... 37
Evacuating the System ................................................................................................................... 37
Starting an Experiment ............................................................................................................................... 38

DXF-200 Getting Started Guide Page 8
Stopping an Experiment ............................................................................................................................. 39
Chapter 4: Maintaining the DXF/EM..................................................................................................... 40
General Cleaning Practices ......................................................................................................................... 40
Recommended Cleaning Supplies .............................................................................................................. 41
Cleaning Maintenance Schedule ................................................................................................................. 41
Maintenance Procedures ............................................................................................................................. 42
Clean the Solid State Detector Pins ..................................................................................................... 42
Clean the Light Pipe Assembly ............................................................................................................ 43
Clean the Xenon Lamp Assembly Optics ............................................................................................ 44
Replacement Parts ...................................................................................................................................... 45

DXF-200 Getting Started Guide Page 9
Chapter 1:
Introducing the Discovery Xenon Flash
Overview
Thermal diffusivity (α) is the thermophysical property defined as a ratio of thermal conductivity and volu-
metric heat capacity. The thermal diffusivity is measured in cm2/s (SI units). The most popular method
used for measuring thermal diffusivity is the flash method. It has the advantage of being fast while provid-
ing values with excellent accuracy and reproducibility. The flash diffusivity method involves uniform irra-
diation of a small, disc-shaped specimen over its front face with a very short pulse of energy. The time-
temperature history of the rear face is recorded through high-speed data acquisition from a solid-state pins
sensor with very fast thermal response, and thermal diffusivity is determined from the time-dependent ther-
mogram of the rear face. Thermal conductivity can be calculated as a product of the thermal diffusivity, the
specific heat, and the density of the material. A Discovery Xenon Flash (DXF) system automatically deter-
mines the thermal conductivity using the measured (or separately entered) specific heat capacity and ther-
mal diffusivity, with separately-entered density data.
The DXF system is comprised of a DXF Pulse Source, Environmental Module, Solid State (Pins) Detector
Assembly, and associated software.
Figure 1 DXF system with EM-200 and Solid State (Pins) Detector Assembly.
Solid State (Pins) Detector
Assembly
Environmental Module
DXF

DXF-200 Getting Started Guide Page 10
Your controller is a computer that performs the following functions:
• Provides an interface between you and the analysis instrument.
• Enables you to set up experiments and enter necessary information.
• Stores experimental data.
• Allows data analysis of results.
DXF System Components
A DXF system has three major components: the DXF Pulse Source module, the Environmental Module
with Detector Assembly, and the controller.
Pulse Source Module
The Discovery Xenon Flash (DXF) covers the most commonly needed cryogenic to 200°C temperatures
with a range of Environmental Modules, and employs a High Speed Xenon-Pulse Delivery Source
(HSXD). The reflective optic configuration effectively harnesses the power of a Xenon flash tube, and,
with the aid of proprietary wave guides, delivers it to the sample inside the Environmental Module. The
DXF produces a maximum pulse width of 400 to 600 μswhile uniformly concentrating sufficient power
from the flash source directly on the entire face of the sample. This optimized energy gathering scheme
and the broad light spectrum allows samples as large as 25 mm in diameter to be illuminated with suffi-
cient energy.
Figure 2 DXF Pulse Source Module.
Table 1: DXF Front Panel LED Indicators - Flashlamp
Indicator Function
BYPASS This function is not used.
INTERNAL INTERLOCK 1 This internal interlock checks to make sure the metal covers
are in place around the flashlamp assembly. When the covers
are closed the INTERNAL INTERLOCK 1 LED changes
from red to green. When all interlocks are green, the flash-
lamp is safe to fire.

DXF-200 Getting Started Guide Page 11
INTERNAL INTERLOCK 2 This internal interlock checks to make sure the metal covers
are in place for the high voltage power section of the instru-
ment. When the covers are closed the INTERNAL INTER-
LOCK 2 LED changes from red to green. When all interlocks
are green, the flashlamp is safe to fire.
UNLABELED INTERLOCK 3 This function is not used. This indicator will remain green.
UNLABELED INTERLOCK 4 When the internal interlocks for the optical path are enabled
and the operating software enables it, the UNLABELED
INTERLOCK 2 LED changes from red to green. When all
interlocks are green, the flashlamp is safe to fire.
POWER When the flashlamp 12 VDC power supply is ON, the green
POWER LED lights up.
INTERLOCK This function is not used.
CHARGE The flashlamp controller has 4 control states. The CHARGE
indicator shows when the controller is charging the main
capacitors with the programmed flash voltage.
ARM The flashlamp controller has 4 control states. The ARM indi-
cator shows when the controller has charged the fire capacitor
and is able to fire the flashlamp.
FIRE The flashlamp controller has 4 control states. The FIRE indi-
cator shows when the controller has fired the flashlamp.
DUMP The flashlamp controller has 4 control states. The DUMP
indicator shows when the controller has dumped all the
charge on the main capacitor and disabled the fire circuit.
Table 1: DXF Front Panel LED Indicators - Flashlamp
Indicator Function

DXF-200 Getting Started Guide Page 12
Table 2: DXF Front Panel LED Indicators - Temperature Displays
Indicator Function
FURNACE TEMPERATURE°C Indicates the current temperature of the furnace. There are
several indicators just to the left of the temperature display
that may light up during normal operation.
SPECIMEN TEMPERATURE °C Indicates the current temperature of the sample. There are
several indicators just to the left of the temperature display
that may light up during normal operation.
OVER TEMP When the temperature controllers detect a temperature out-
side the acceptable range, an alarm is triggered, and the
OVER TEMP red LED will light up. If the interlock ON LED
is enabled, it will be disabled.
OPTICAL When the internal interlocks for the optical path are enabled
and the operating software enables it, the OPTICAL LED
lights up. When the OPTICAL LED is ON, the flashlamp is
enabled to fire.
ALARM This indicator shows the status of the External Alarm input.
This unit does not have an External Alarm Input and this
LED will not be on.
POWER When the internal 12 VDC power supply is ON, the yellow
POWER LED lights up.
DET. POWER When the operating software is ready to start a test, a separate
DC power supply is connected to the Detector Electronics
and the DET POWER LED lights up.

DXF-200 Getting Started Guide Page 13
Table 3: DXF Front Panel Switches
Indicator Function
HARDWARE ENABLE When prompted by the operating software, this switch is
pressed to enable the operation of the electronic hardware. If
all the electronic checks are correct, the switch's integrated
green LED will light up.
ON INTERLOCK When prompted by the operating software, this switch is
pressed to enable the temperature control of the furnace. If all
the electronic checks are correct, the switch's integrated green
LED will light up.
OFF INTERLOCK At any time, this switch is pressed to disable the temperature
control of the furnace. The switch's integrated red LED does
not light up. When the switch is pressed, if the ON interlock
LED is enabled, it will be disabled.
INDEX ON This switch is not used.

DXF-200 Getting Started Guide Page 14
Environmental Modules and Solid State (Pins) Detector Assembly
The Environmental Module includes a cooling block with heater cartridge-resistance furnace, providing
temperature control of the sample operation in air or inert gas. The EM also includes a two-sample holder,
supporting a variety of sample sizes. Adapters are available for smaller cylindrical and/or square samples.
The module includes a Solid State (Pins) Detector.
Figure 3 EM and Solid State (Pins) Detector Assembly.
Locking Arm
Purge Gas Adjusting
Valve
LN2 Outlet
Solid State (Pins)
Detector Assembly
LN2 Inlet
EM

DXF-200 Getting Started Guide Page 15
Instrument Specifications
The tables found below contain the technical specifications for the DXF and EM.
**Using ideal, well-defined, well-behaved 12-mm diameter samples of known properties
Table 4: DXF Technical Specifications
Item/Area Specifications
Dimensions Depth 66.04 cm (26 in)
Width 53.34 cm (21 in)
Height 40.64 cm (16 in)
Weight 44 kg (96 lbs)
Powera
a. This instrument is supplied with a power cord 2.4 m (7.75 ft) long, rated for 10A and 250V and a USA
NEMA 6-15P style plug. The TA Representative installing the instrument will provide the appropriate
power cable for the geographical location where the instrument is being installed. Connect the instrument,
computer, and monitor to wall outlets on the same circuit and make sure that the mains assigned do not
also supply power to noise generating equipment nearby, such as motors, welders, transformers, etc.
System supply voltage: 198–242 VAC (rated for 10A)
50/60 Hz.
Operating environmental conditions Temperature: 15 to 35°C
Relative humidity: 5 to 80% (non-condensing)
Installation Category II
Pollution Degree 2
Maximum altitude: 2000 m
Pulse Source High speed Xenon module
Table 5: EM Technical Specifications
Item/Area EM-200
Thermocouple Measurement 3 wire PT 100ΩRTD ± 0.15%
Thermal Diffusivity Accuracy** ± 4% (worst case)
Measurement Repeatability** ± 2% (worst case)
Temperature Range -150 to 200°C
Atmosphere Air, inert gas
Number of Specimens 2
Sample Dimension 12.7/25.4 mm (d) x up to 6 mm (t)
Sample Shape Round disk, square plate (with adapters)
Solid State Detector
Assembly
8 and 10 mm diameter Intrinsic thermocouples (8, 10, 12.7
mm length Bismuth telluride [Bi2Te3] pins)

DXF-200 Getting Started Guide Page 16
CAUTION: Dewar LN2tank minimum 50 litters capacity. Maximum 22 psi (1.5 bar) supply pres-
sure. Pressure exceeding 22 psi will damage the instrument.
MISE EN GARDE: Réservoir Dewar LN2 d'une capacité minimale de 50 litres. Pression d'alimenta-
tion maximale de 22 psi (1,5 bar). Une pression supérieure à 22 psi endommagera l'instrument.

DXF-200 Getting Started Guide Page 17
Chapter 2:
Installing the DXF System
Unpacking/Repacking
You may wish to retain all the shipping hardware, the plywood, and boxes from the instrument in the event
you wish to repack and ship your instrument.
Installing the System
Before shipment, the DXF is inspected both electrically and mechanically so that it is ready for operation
upon proper installation. Only limited instructions are given in this manual; consult the Help documenta-
tion for additional information. Installation involves the following procedures:
• Inspecting the system for shipping damage and missing parts
• Choosing a location for instrument installation
• Connecting the Environmental Module to Pulse Source Module
• Setting up system communication with the controller
• Connecting the utilities
It is strongly recommended that you have your DXF system installed by a TA Instruments Service Repre-
sentative; call for an installation appointment when you receive your instrument.
CAUTION: To avoid mistakes, read this entire chapter before you begin installation.
MISE EN GARDE: Pour éviter de commettre des erreurs, lisez tout le chapitre avant de commencer
l'installation.
Inspecting the System
When you receive your DXF system, look over the instrument and shipping container carefully for signs of
shipping damage, and check the parts received against the enclosed shipping list.
• If the instrument is damaged, notify the carrier and TA Instruments immediately.
• If the instrument is intact but parts are missing, contact TA Instruments.

DXF-200 Getting Started Guide Page 18
Choosing a Location
Because of the sensitivity of DXF experiments, it is important to choose a location for the instrument using
the following guidelines. The DXF system should be:
In
• A temperature and humidity controlled area.
• A clean, vibration-free environment.
• An area with ample working and ventilation space.
On
• A stable, non-flammable work surface.
Near
• A power outlet for the specific voltage of the instrument.
• The controller (computer).
• Compressed lab air and purge gas supplies with suitable regulators and filtering where needed.
Away from
• Dusty environments.
• Exposure to direct sunlight.
• Direct air drafts (fans, room air ducts).
• Poorly ventilated areas.
• Electrically noisy areas or areas prone to mechanical vibrations.
NOTE: Do not place equipment against walls or cabinets that might impede air flow. Leave at least 7.5 cm
(3 in) clearance between the back of the instrument and any objects
CAUTION: An independent heavy GROUND wire must be provided through the power hook up.
Improper grounding may cause severe damage for which the supplier will not accept responsibility.
WARNING: For safety, position the equipment in a manner that allows access to the power cord
for emergency disconnection.
AVERTISSEMENT: Par mesure de sécurité, placez l'équipement de sorte qu'il permette d'accéder
facilement au cordon d'alimentation en cas de débranchement d'urgence.
WARNING: Protect power and communication cable paths. Do not create tripping hazards by
laying the cables across access ways.
AVERTISSEMENT: Protégez les chemins de câble électriques et de câbles de télécommunica-
tion. Ne créez pas de risques de déclenchement en posant des câbles sur les voies d'accès.

DXF-200 Getting Started Guide Page 19
All power strips must be fully grounded and carry the ground through to the sockets into which the
computer is plugged.
MISE EN GARDE: Un fil de masse lourd et indépendant doit être fourni via le raccordement élec-
trique. Une mise à la terre incorrecte peut causer de graves dommages pour lesquels le fournisseur
décline toute responsabilité. Toutes les barrettes d'alimentation doivent être entièrement mises à la
terre et acheminer la terre jusqu'aux prises dans lesquelles l'ordinateur est branché.
Moving the Instrument
Lifting the DXF should always be done with two people.
1With each person standing on either side of the DXF, place hands on the outside bottom corners of the
DXF and lift upwards, keeping the module in an upright position.
Figure 4 Lifting the DXF.
WARNING: Use two people to lift and/or carry the instrument. The instrument is too heavy for
one person to handle safely.
AVERTISSEMENT: Demandez à deux personnes de soulever et/ou de porter l'instrument.
L'instrument est trop lourd pour qu'une seule personne le manipule en toute sécurité.
Place hands on the outside of
the DXF feet

DXF-200 Getting Started Guide Page 20
Connecting the Environmental Module to the Pulse Source Module
1Before making any connections, make sure the DXF is level.
2Place the reflector in the location shown in the image below, and then install the sealing foam.
Figure 5 Reflector and sealing foam.
3Place the Environmental Module on top of the DXF so that they are stacked; make sure to align the 4
pins on the bottom of the furnace with the corresponding holes on the alignment tracks on the top of the
DXF.
Figure 6 Pins on the bottom of the Environmental Module.
Reflector
Alignment Tracks
Alignment Pins
Sealing Foam