T H E R M A L A N A L Y S I S

THERMAL LFA
TF-LFA
CONDUCTIVITY TFA
THB
Since 1957 LINSEIS Corporation has been deliv-
ering outstanding service, know how and lead-
ing innovative products in the field of thermal
analysis and thermo physical properties.

Customer satisfaction, innovation, flexibility

and high quality are what LINSEIS represents.
Thanks to these fundamentals, our company
enjoys an exceptional reputation among the
leading scientific and industrial organizations.
LINSEIS has been offering highly innovative
benchmark products for many years.

The LINSEIS business unit of thermal analysis

is involved in the complete range of thermo
Claus Linseis
analytical equipment for R&D as well as qual- Managing Director
ity control. We support applications in sectors
such as polymers, chemical industry, inorganic
building materials and environmental analytics.
In addition, thermo physical properties of solids,
liquids and melts can be analyzed.

LINSEIS provides technological leadership. We

develop and manufacture thermo analytic and
thermo physical testing equipment to the high-
est standards and precision. Due to our innova-
tive drive and precision, we are a leading manu-
facturer of thermal Analysis equipment.

The development of thermo analytical testing

machines requires significant research and a
high degree of precision. LINSEIS Corp. invests
in this research to the benefit of our customers.

2
LFA
Information about the thermophysical proper- others. Trouble-free sample preparation, small
ties of materials and heat transfer optimization required sample dimensions, fast measurement
of fi­nal products is becoming more and more vi- times and high accuracy are only a few of the
tal for industrial applications. Over the past few advantages of this non-contact and non-de-
decades, the flash method has developed into structive measurement technique.
a commonly used technique for the measure-
ment of the thermal diffusivity and thermal con- LINSEIS offers a variety of instruments to measu-
ductivity of various kinds of solids, powders, pa- re the thermal diffusivity/conductivity. The LFA
stes and liquids. Application areas are electronic 500/1000/2000 Flash series provides a cost ef-
packaging, heat sinks, brackets, reactor cooling, fective solution for the temperature range from
heat exchangers, thermal insulators and many -125 up to 2800°C.

3
SYSTEM DESIGN
The vertical arrangement with sensor on top, 25 Joule/pulse. In addition the pulse duration
sample in the middle and Laser flash sour- can be adjusted. Due to this flexibility all kinds
ce on the bottom ensure easy handling and of demanding samples (even thin film or ultra-
best possible measurement results. The pulse low thermal conductivity) can be analyzed.
energy is adjustable in the range of 0.05 to

Detector

Iris

Furnance

Sample Carrier
Laser

Xenon Flash

ABSOLUTE METHOD
The method used is an absolute measurement 500/1000/2000 Flash Analyzers operate in ag-
technique (for thermal diffusivity), hence the- reement with national and international stan-
re is no need to calibrate the system. The LFA dards, such as ASTM E-1461, DIN 30905 and DIN
EN 821.

4
VISION CONTROL
The vision control feature provides best signal overcomes positioning accuracy problems with
quality for any sample dimension. The optimiza- existing zoom lens systems by ensuring best
tion ensures superior signal quality for big and possible specific heat determination capabili-
small samples. In addition, the arrangement ties.

IR-detector
active sensor area
distance (f)

Fixed position
zoom lense
distance (f')

sample

25.4mm 10mm 3mm sample diameter

DETECTORS
The system can be either equipped with an InSb 2800°C. Both are easily user exchangeable. An
or with a MCT detector, covering the comple- automatic LN2 refilling accessory with Dewar
te temperature range from sub-ambient up to can be ordered for prolonged measurement
cycles.

ENVIRONMENTAL OPTIONS
The instrument can be operated under defined dosing systems to measure under specific atmo-
at­mospheric conditions. It is either possible to spheres (argon, nitrogen, air, etc.).
attach a vacuum pump, in order to minimize
heat loss effects or to attach an additional gas

5
UNMATCHED SAMPLE
THROUGHPUT
Highest throughput in the market. The combi- les, as needed for quality control, takes only a
nation of sample robot and infrared furnace few hours even for measurements over the com-
allows unbeaten measurement turnaround plete temperature range.
time. A typical measurement of up to 18 samp-

Sample carriers

18 round or square 6 samples round or square 3 samples round

samples 3mm or 6 mm 3mm, 6mm, 10mm or 12.7mm 25.4mm or square 20mm

Sample holder

Sample holder square samples

3x3mm / 10x10mm / 20x20mm

Sample holder round samples

3mm / 6mm / 10mm / 12.7mm
/ 25.4mm

More sample holders available!

6
SOFTWARE: COMBINED MODEL
ACCORDING TO DUSZA
Combining simultaneous heat loss and finite pulse correction in a
single evaluation model, providing highest measuremet accuracy.

The plot illustrates a measurement on an Inconel sample. The raw data were evaluated using diffe-
rent common models. It can clearly be observed, that the combined model provides the best fit,
resulting in the most accurate measurement result.

Conclusion

The combined model with nonlinear parameter between the different models and corrections is
estimation has been proven for more than 100 necessary, and that it can be applied to any type
samples. In all cases it worked reliably and its re- of sample. The quality of the fit can be checked
sults gave the correct adiabatic, finite pulse, and by plotting the model curve and also as a nu-
heat loss corrected values. The two main advan- meric value.
tages of the method are that no operator choice

7
SPECIFICATIONS
LLFA 500 LFA 1000/2000

Temperature range –100 / –50°C up to 500°C –125 up to 500°C

RT up to 500 / 1000 / 1125°C RT up to 1250 / 1600 / 2000 /
2800°C

Heating rate 0.01 up to 100°C 0.01 up to 20°C

Thermal Diffusivity 0.01 up to 2000 mm2/s 0.01 up to 2000 mm2/s

Thermal 0.1 up to 4000 W/(m•K) 0.1 up to 4000 W/(m•K)

Conductivity

Accuracy Thermal diffusivity ± 2.4% Thermal diffusivity ± 2.4%

Specific Heat ± 5% Specific Heat ± 5%

Repeatability Thermal diffusivity ± 1.9% Thermal diffusivity ± 1.9%

Specific Heat ± 3% Specific Heat ± 3%

Flash source Light flash 15 J/pulse Laser Nd:YAG 25 J/pulse

variable pulse energy: software variable pulse energy: software
controlled controlled

Vision control Perfect field of view Perfect field of view

Pulse width 20 up to 2000 µs 0.05 up to 5 ms

IR-detector InSb: RT up to 500 / 1000°C InSb: RT up to 1250 / 1600°C

MCT: –100 up to 500°C MCT: –100 up to 500°C

Atmosphere inert, oxidizing, reducing, vacu- inert, oxidizing, reducing, vacu-

um um

Vacuum up to 10–5mbar up to 10–5mbar

Data aquisition 2 MHz 2 MHz

Gas control manual or MFC manual or MFC

gas dosing systems gas dosing systems

Sample holders round or square - solid samp- round or square - solid samp-
les, powders, pastes, liquids, les, powders, pastes, liquids,
laminates - special holder for laminates - special holder for
measurement under mechani- measurement under mechani-
cal pressure (option) cal pressure (option)

sample numbers up to 18 samples up to 18 samples

8
THB – TRANSIENT
HOT BRIDGE
Instrument for rapid measurement of thermal conductivity,
thermal diffusivity and specific heat

Two flat surfaces of the specimens are put in a few minutes. The sensors are automatically
contact with both sensor sides in order to as- identified by the software (THB-100/THB-500).
sure a good thermal contact without air inclu- Multiple measurements with automatic calcula-
sions. Either the delivered sample holder or tion of the mean values are possible as well as
a weight can be used. The shapes of the faces the storage of measurement programs.
which are not in contact with the sensor are of
no importance so that sample preparation is Measurement can be done either at room tem-
reduced to a minimum. Minimum sample thick- perature (no further equipment required) or at
nesses depend on their thermal diffusivity. In high or low temperatures. The set-up including
most cases some mms are sufficient. After ad- the sensor can be placed in a normal lab oven or
justing the heating power and heating time the climatic chamber often available in laboratories.
measurement and the evaluation run automati- LINSEIS offers specially adapted furnaces cove-
cally. Results can be post-processed if needed. ring temperatures from -150 up to 700°C.
Measurements take only some seconds up to

9
THE MEASUREMENT SET-UP
Advantages Transient Hot Bridge Method
• Short measurement times (seconds to few The THB measurement method initially deve-
minutes) loped by the National Metrology Institute of
• High accuracy due to patented sensor design Germany is an optimized hot wire technique to
• Easy set-up and sample preparation measure all relevant thermal transport proper-
• Nondestructive measurement ties (thermal conductivity, thermal diffusivity
• Absolut method - no calibration required and volumetric specific heat) with the highest
• Suitable for solids, liquids, powders, pastes etc. possible accuracy.
• Temperature range -150 to 700 °C
• Measurements at different atmospheres, LX LL

vacuum and pressures up to 150 bar

• Broad thermal conductivity range from 0.01 to
500 W/m·K Leff

• Modular design Patented meander-shaped tandem hot wire

SENSORS
For the THB-100 and THB-500 additional hot wire measurement techniques are available based on
innovative and patented new sensors:

The Quasi-Steady-State (QSS) sensors have The LINSEIS Hot Point Sensors (HPS) work accor-
been developed for the measurement of high ding to the transient plane method. They are
thermal conductivities. It combines the advan- suitable to measure small samples with dimen-
tages of steady-state and transient measure- sions down to 3x3x1 mm and to measure aniso-
ment techniques and enables measurements in tropic samples. Due to the small amount of heat
the range between 1 and 500 W/m*K which is produced by the hot point sensors,
they are a good choice to measure liquids with
negligible convection.
R2
R1

R3
R4

10
SPECIFICATIONS
All sensor types are available as Kapton-foil-sen- a temperature range up to +700°C (THB-100
sors and resist to temperatures from -150 up to and THB-500).
+200°C. Ceramic sensors are available covering

THB-1 THB 100 THB 500

thermal conductivity range 0 to 5 W/mK 0 to 100 W/mK 0 to 500 W/mK

THB/SENSOR/A

THB/SENSOR/B

THB/SENSOR/C

QSS-Sensors

Hotpoint-Sensors

SENSOR TYPES
Min. sample Temperature Measuring
Sensor type Sensor size suitable for...
size range range

THB/Sensor/A/B 82 x 42 mm 20 x 40 x 5 mm -150 up to 200°C 0.01 – 1 W/m·K solids, powders,

42 x 22 mm 10 x 20 x 3 mm gases

THB/Sensor/A/B/Metal 105 x 42 mm 20 x 40 x 5 mm -150 up to 200°C 0.01 – 1 W/m·K solids, powders,

54 x 22 mm 10 x 20 x 3 mm gases

THB/Sensor/C 300 x 3 mm 10 x 10 x 10 mm -150 up to 700°C 0.01 – 1 W/m·K liquids, powders

THB/Sensor/D/E/QSS 42 x 22 mm 22 x 42 x 3 mm -150 up to 200°C 0.2 – 100 W/m·K solids, powders,

0.2 – 500 W/m·K gases

THB/Sensor/G/HOTPOINT/ 65 x 5 mm 3 x 3 x 2 mm -150 up to 200°C 0.01 – 1 W/m·K solids, liquids,

Kapton powders, gases

more sensors on request

11
TF-LFA
Thermophysical properties of thin films are differ from bulk material, these data are required
becoming more and more important in indus- for accurate thermal management predictions.
tries such as, phase-change optical disk media,
thermo-electric materials, light emitting diodes Based on the well established Laser flash tech-
(LEDs), phase change memories, flat panel dis- nique, the LINSEIS “Thin-Film-Laserflash-Analyz-
plays, and the semiconductor industry. All these er” now offers a whole range of new possibilities
industries deposit a film on a substrate in order to analyze thermophysical properties of thin
to give a device a particular function. Since the films from 80nm up to 20µm thickness.
physical properties of these films significantely

Bulk materials Thin plates and coatings Thin films

10-2 10-3 10-4 10-5 10-6 10-7 10-8
Heat diffusion length (l) [m]

Laser Flash Method

Nanosecond thermoreflectance method

100 10-2 10-4 10-6 10-8 10-10 10-12

Heat diffusion time (t) [s]
l2
(Thermal diffusivity a=l•10-5m2s-1, t= a )

12
FURNACE OPTION

Furnace RT up to 500°C
Cryo Furnace -100 up to 500°C

70 Ag λ = 418 W/mK
Cu λ = 398 W/mK
W λ = 172 W/mK
60 Mo λ = 135 W/mK
Pt λ = 71 W/mK
Ti λ = 16 W/mK
50
Deviation [%]

40

30

20

10

0
0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
d [mm]

The graph from Schoderböck et. al., Int. J. Ther- thickness of less than 2mm (depending on the
mophys. (2009) illustrates the limitation of the thermal diffusivity of the material) already show
classic Laserflash technique. Samples with a a significant deviation from literature values.

13
DESCRIPTION OF THE
LASERFLASH TECHNIQUE
As thermal properties of thin layers and films differ considerably from the properties of the corre-
sponding bulk material, a technique overcoming the limitations of the classical Laserflash method is
required: the “High Speed Laserflash Method”.

High Speed Laserflash Time Domain

Method Thermoreflectance Method
Rear heating Front detection (RF) Front heating Front detection (FF)
The measurement geometry is the same as for The measurement geometry is called “front
the standard Laserflash technique: detector and heating front detection (FF)” because detector
laser are on opposite sides of the samples. Be- and laser are on the same side of the sample.
cause IR-detectors are to slow for measurement This method can be applied to thin layers on
of thin layers, detection is done by the so called various substrates (e.g. non transparent sub-
thermoreflectance method. The idea behind strates or very thin films) for which the RF tech-
this technique is that once a material is heated nique is not suitable. For the measurement, a
up, the change in the reflectance of the sur- heating pulse is applied to the front side of the
face can be utilized to derive the temperature sample and the temperature rise at this spot is
change and thus the thermal properties. The re- measured with a detection laser coming from
flectivity is measured with respect to time, and the side. The thermal diffusivity of the sample
the data received can be matched to a model layer can be calculated by using the falling edge
which contains coefficients that correspond to of the normalized temperature rize in combina-
thermal properties. tion with a multilayer modell developed by Lin-
seis in cooperation with Prof. David G. Cahill of
detector the Univerity of Illinois.
probe pulse
m S
3n PS
47 D
CW

substrate
opaque thin film

opaque thin film

transparent substrate detector
probe pulse
m S
3n PS
47 D
CW

Nd: Yag
pump pulse Nd: Yag 1064 nm
1 ns, 90 mJ 1064 nm pump pulse
1 ns, 90 mJ

14
SPECIFICATIONS

Thin Film Laser Flash Analyzer TF-LFA

Sample dimensions Round with a diameter of 10mm to 20mm

Film thickness 80nm up to 20µm (depends on sample)

Temperature range RT, RT up to 500°C or -100 to 500°C

Heating and cooling rates 0.01 up to 10°C/min

Vacuum up to 10-4mbar

Atmosphere inert, oxidizing or reducing

Thermal diffusivity measuring 0,01mm2/s up to 1000mm2/s

range
Pump-Laser Nd:YAG Laser (1064 nm), maximum pulse current: up to
120mJ/pulse (software controlled),
pulse width: 1 - 5 ns, spot size 2-4 mm (depends on arrangement)

Probe-Laser DPSS CW Laser (473 nm, 50 mW)

Photoreceiver Si-PIN-Photodiode, active diameter: 0.8mm,

bandwidth DC … 400MHz, risetime: 1ns

15
THIN FILM ANALYZER
The LINSEIS Thin Film Analyzer TFA is the perfect Measurement Setup
solution to characterize a broad range of thin film The LINSEIS TFA is a chip-based platform to si-
samples in a very comfortable and quick way. It multaneously measure the in-plane electrical
is an easy to use, single stand alone system and and thermal conductivity, the Seebeck coeffi-
delivers high quality results using an optimized cient as well as the Hall constant of a thin film
measurement design as well as the proven sample in the temperature range from -170°C
LINSEIS firmware and software package. up to 280°C and in a magnetic field of up to 1 T.
Due to the design of the setup, time consuming
Motivation preparation steps can be omitted and a nearly
Due to new research efforts in the field of se- simultaneous measurement of the sample pro-
miconducting materials with a focus on size ef- perties is achieved. Typical errors caused by dif-
fects, there is a growing need for measurement ferent sample compositions, varying sample ge-
setups dedicated to samples with small geome- ometries and different heat profiles are avoided
trical dimensions like thin films and nanowires with this measurement method.
with considerably different physical properties The system can handle a broad range of diffe-
than bulk material. The characterization of the- rent materials. It is possible to measure samp-
se samples is important to learn more about les with semiconducting behaviour as well as
their structure and conduction mechanism but metals, ceramics or organics. Therefore many
also important for technical applications. different deposition methods like PVD or spin
coating and drop casting can be used.

16
PACKAGING OPTIONS
Following packaging options are available for 3. Magnetic package
the LINSEIS Thin Film Analyzer (TFA): The design is optimized for measuring the fol-
lowing parameters:
1. Basic device (incl. transient package) • AH - Hall constant
Consists of measurement chamber, vacuum • μ - mobility
pump, basic sample holder with included heat- • n - charge carrier concentration
er, system integrated lock-in amplifier for the
3w-method, PC and LINSEIS software package 4. Low temperature option for controlled coo-
including measurement and evaluation soft- ling down to 100 K
ware. The design is optimized to measure fol- • TFA/KREG controlled cooling unit
lowing physical properties: • TFA/KRYO Dewar 25l
• l - thermal conductivity
• cp - specific heat Software
• e - emissivity (depends on material) The TFA software package consists of two parts.
A measurement software which displays the ac-
2. Thermoelectric package tual values and which allows to define a meas-
Consisting of extended measurment electronics urement routine and the dircet control of the
(DC) and evaluation software for thermoelectric setup. And an additional evaluation software for
experiments. The design is optimized for meas- the post processing of the measured raw data.
uring the following parameters:
• s - electrical conductivity / electrical resistivity
• S - Seebeck coefficient

Measurement software Evaluation software

17
MEASURING PRINCIPLES
Pre-structured measuring chips between the remaining two is measured. By
The chip is combining the 3w measure- clockwise changing of the contacts and repea-
ment technique for the thermal conductivity ting of the procedure, the resistivity of the sam-
measurement with a 4-point Van-der-Pauw se- ple can be calculated using the Van-der-Pauw
tup for the determination of the electrical trans- equation.
port properties. The Seebeck coefficient can
exp ( – πd πd
r ∙ RAB,CD ) + exp ( – r ∙ RBC,DA )=1
be measured using additional resistance ther-
mometers located near the sample. For an easy
sample preparation either a strip-off foil mask or By applying a magnetic field and measuring the
a metallic shadow mask can be used. This confi- corresponding change of the diagonal Van-der-
guration allows for a nearly simultaneous cha- Pauw resistance, the Hall constant of the sample
racterization of a sample which has been pre- can be calculated.
pared by either PVD (e.g. thermal evaporation,
d
AH = B
∙ ∆RAC,BD
sputtering, MBE), CVD (e.g. ALD), spin coating,
drop casting or ink-jet printing in one step.
For the determination of the Seebeck coeffici-
Van-der-Pauw measurement ent, an additional thermometer and heater is
To determine the electrical conductivity (s) placed on the chip near the sample. This confi-
and Hall constant (AH) of the sample, the Van- guration allows for the measurment of the ther-
der-Pauw method is used. After depositing the movoltage at different temperature gradients
sample on the chip, it is already connected to wich can be used in order to calculate the See-
four elec­trodes A, B, C & D at their edge. For the beck coefficient S=-Vth/∆T.
measurement, a current is applied between two
S = –Vth / ∆T
of the contacts and the corresponding voltage

18
SPECIFICATIONS
TFA
Temperature range RT up to 280°C
-170°C up to 280°C

Sample thickness from only a few nm to µm range (depends on sample)

Measurement principle chip based (pre-structured measurement chips)

Desposition techiques include: PVD (sputtering, evaporation), ALD, spin coating, ink-jet printing and more

Measured parameters thermal conductivity (3w)

specific heat

Optional Seebeck coefficient

electrical resisitivity / conductivity
Hall constant / mobility / charge carrier concentration
permanent magnet 0.5 T or electromagnet up to 1 T

Vacuum up to 10-5mbar

Electronics integrated

Interface USB

Measurement range

Thermal conductivity 0.05 up to 200 W/m∙K

Electrical resistivity 0.05 up to 1 ∙ 106S/cm

Seebeck coefficient 1 up to 2500 µV/K

Hall mobility 1 up to 107 (cm2 /Volt sec)

Charge carrier concentration 107 up to 1021 (1/cm³)

Repeatability & accuracy

Thermal conductivity ± 10% (for most materials)

Electrical resistivity ± 6% (for most materials)

Seebeck coefficient ± 7% (for most materials)

Hall constant ± 9 % for most materials

19
 LINSEIS GmbH Germany LINSEIS Inc. USA
Vielitzerstr. 43 109 North Gold Drive
95100 Selb Robbinsville, NJ 08691
Tel.: (+49) 9287 880 0 Tel.: (+1) 609 223 2070
Fax: (+49) 9287 70488 Fax: (+1) 609 223 2074
E-mail: info@linseis.de E-mail: info@linseis.com

LINSEIS China LINSEIS France

Kaige Scientific Park 2653 Hunan Road Bureaux Paris
201315 Shanghai 52 Boulevard Sébastopol
Tel.: (+86) 21 6190 1202 75003 Paris
Fax.: (+86) 21 6806 3576 Tel.: (+33) 1.73.02.82.72

Bureaux Lyon
LINSEIS Poland 2A Chemin des Eglantines
ul. Dabrowskiego 1 69580 Sathonay Village
05-800 Pruszków Tel.: (+33) 4.26.68.70.55
Tel.: (+48) 692 773 795

www.linseis.com

Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect, Thin Film Analyzer, Hall-Effect
Services: Service Lab, Calibration Service
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