Thermoreflectance by Pulsed Light Heating
NanoTR/PicoTR

Thermoreflectance - The Laser Flash Method for Thin Films

Laser Flash Method –

Laser Flash Method –

The Most Established Method for the Determination of Thermal Diffusivity

In modern industries, the knowledge of thermal properties, specifically thermophysical properties, becomes more and more important. They are required, for example, for the development of heat release materials of advanced and miniaturized electronics, thermoelectric materials as sustainable energy, insulating materials for saving energy, TBCs (thermal barrier coatings) for turbine blades, and safety operation of nuclear plants, etc.

Among the thermophysical properties, the thermal conductivity is of paramount importance. The determination of the thermal diffusivity/thermal conductivity can be realized with the established laser flash method (LFA). This method has been known for many years to provide reliable and accurate results. Sample thicknesses typically range from 50 μm to 10 mm.

NETZSCH is a world-wide leading manufacturer of instruments for testing thermophysical properties, specifically of laser flash analyzers. These LFA systems are used in the fields of ceramics, metals, polymers, nuclear research, etc.

Thermoreflectance –

Thermoreflectance –

The Method for the Determination of Thermal Diffusivity in the Thickness Range of Nanometer

With the significant progress in the design of electronic devices and the associated need for an efficient thermal management, accurate thermal diffusivity / thermal conductivity measurements in the nanometer range are more than ever crucial.

The National Institute of Advanced Industrial Science and Technology (AIST), Japan, already responded to industrial requirements with the development of a “pulsed light heating thermoreflectance method” in the early 90’s. PicoTherm Corporation was established in 2008 with the launch of a nano-second thermoreflectance apparatus “NanoTR” and a pico-second thermoreflectance apparatus “PicoTR”, which allows for absolute measurements of the thermal diffusivity of thin films in a thickness range of several 10 μm down into the nanometer range.

In 2014, NETZSCH Japan K.K, a subsidiary of NETZSCH, became the exclusive representative of the PicoTherm Corporation. In combination with our LFA systems, NETZSCH can now offer the solution for thin films in the nanometer range up to bulk materials in the range of mm.

Possible Heat Diffusion TimesPossible Heat Diffusion Times

Why measuring thin films?

Thermal Properties of Thin Films are Different from that of Bulk Materials

The thicknesses of nanometer-thin films are often less than the typical grain size. Consequently, their thermophysical properties differ significantly from the bulk material.

Thermoreflectance Methods

Thermoreflectance Methods

Ultrafast Laser Flash Method –
Rear Heating/Front Detection (RF)

Determination of Thermal Diffusivity and Interfacial Thermal Resistance

The fact that the thermophysical properties of thin layers and films differ considerably from those of the corresponding bulk material requires a technique which overcomes the limitations of the classical laser flash method (LFA). This so-called ultrafast laser flash technique is also known as the rear heating/front detection method.

The measurement setup is similar to the conventional LFA: detector and laser are on opposite sides of the sample which is located on a transparent substrate. The measured thermal diffusivity is the component through the thickness perpendicular to the sample’s surface. The pump laser irradiates the sample’s rear side.

As the sample heats up, its surface thermoreflectance varies. The thermal diffusivity is calculated from the temperature rise (lower plot). Here, the thermal diffusivity of a thin metal film (Mo) was determined to 1.59 • 10-5 m2/s.

RF configutation specifically for transparent substancesRF configutation specifically for transparent substances
Temperature histroy curve and measured thermal diffusivity of Mo thin film (90 nm) with RF methodTemperature history curve and measured thermal diffusivity of Mo thin film (90 nm) with RF method

Time Domain Thermoreflectance –
Front Heating/Front Detection (FF)

Determination of Thermal Diffusivity and Thermal Effusivity

In addition to the RF method, measurements can also be made in a front heating/front detection (FF) configuration. The term “front” refers to the open surface of the thin film deposited on a substrate, while “rear” refers to the boundary between the thin film and the substrate.

In the FF measurement setup (upper picture), the detector and laser are on the same side of the sample. An area of the front face of the thin film with a diameter of several tens of micrometers is heated by a pump laser, and a probe laser points at the same position. The change in the surface temperature is observed.

This method can be applied to thin layers on non-transparent substrates for which the RF technique is not suitable.

In the example on the left, the thermal diffusivity of a thin metal film (Mo) was determined to 1.61 • 10-5 m2/s by applying the FF method. The results prove the high agreement between RF and FF modes (deviation < 2%).

FF configuration specifically for opaque substratesFF configuration specifically for opaque substrates
Temperature history curve and measured thermal diffusivity of Mo thin film (90 nm) with FF methodTemperature history curve and measured thermal diffusivity of Mo thin film (90 nm) with FF method
Prinicple of NanoTR

Prinicple of NanoTR

NanoTR’s state-of-the-art signal processing technology allows high speed measurements. With this thermoreflectance apparatus, a laser pulse of 1 ns pulse width is periodically (20 μs) irradiated to the sample. The resulting temperature response is applied to a CW laser (probe laser). Excellent s/n ratio can be attained by high speed integration of repetitive signals. It can be easily switched between the RF and FF configurations though the software for a wide variety of samples.

NanoTR is in accordance with JIS R 1689, JIS R 1690, and SI traceable by the thin film standard of heat diffusion time (RM1301-a), supplied from AIST.

Instrument setup of the NanoTR apparatusInstrument setup of the NanoTR apparatus
Principle of PicoTR

Principle of PicoTR

With picosecond thermoreflectance analyzer PicoTR, laser pulses (pump laser) of 0.5 ps pulse width are applied to the sample with the time period of 50 ns. The temperature response is detected with the probe laser.

PicoTR allows for an easy switching between the RF and FF mode by the user.

PicoTR is in accordance with JIS R 1689, JIS R 1690.

Instrument setup of the PicoTR apparatusInstrument setup of the PicoTR apparatus

Traceability to National Standard

NanoTR and PicoTR allow for an absolute measurement of the thermal diffusivity in the case of an opaque sample and a transparent substrate. For all other cases such as opaque substrate and transparent thin film, reference materials are available made of Molybdenum (CRM 5808-a, for PicoTR) and TiN (RM 1301-a, for NanoTR). It is supplied by AIST, the Japanese National Institute of Advanced Industrial Science and Technology. This guarantees the traceability to national standard. NanoTR and PicoTR are calibrated to ensure traceability to Japanese standards. The instruments are in accordance with the Japanese Industrial Standards (JIS):

  • JIS R 1689 “Determination of thermal diffusivity of fine ceramic films by pulsed light heating thermoreflectance method”
  • JIS R 1690 “Determination of interfacial thermal resistance between fine ceramic film and metal film”
Technical Specification (subject to change)

Technical Specification (subject to change)

Twoje urządzenie jest za małe, aby wyświetlić tę tabelę.
NanoTRPicoTR
Pump LaserPulse width
Wave length
Beam diameter
1 ns
1550 nm
100 μm
0.5 ps
1550 nm
45 μm
Probe Laser

Pulse width
Wave length
Beam diameter

contiuous
785 nm
50 μm
0.5 ps
775 nm
25 μm
Measurement itemsThermal diffusivity and effusivity, interfacial resistance

Sample Film Thickness
(RF method)

Resin
Ceramics
Metal
30 nm ... 2 μm
300 nm ... 5 μm
1 μm ... 20 μm
10 nm ... 100 nm
10 nm ... 300 nm
100 nm ... 900 nm

Sample Film Thickness
(FF method)

Thicker than 1 μmThicker than 100 nm
Substrate

Material
Size
Thickness

Opaque/Transparent
10 ... 20 mm square
1 mm max.
Thermal diffusivity


Range0.01 ... 1000 mm²/s
Accuracy± 6.2% with 40 min measurement time, for CRM 5808A in RF Mode, 400 nm thickness
Repeatability± 5%
SoftwareCalculation of thermal properties, multilayer analysis, database

Software

In-situ display and analyzing 100,000 shots

The state-of-the-art measurement/analysis software of NanoTR/PicoTR has an easy-to-handle user interface which allows for a precise determination of the thermal properties of thin films. The laser beam focusing can be adjusted by the software and CCD picture can be obtained.

NanoTR/PicoTR software runs under Microsoft Windows.

The plot shows that in 1 μs measurement time one measurement curve can be obtained.

Obtaining results in minutes