Analysis Equipment

Signatone S-302-4 Four Point Probe with Keithley 4200-SCS Semiconductor Characterization System 

The purpose of the 4-point probe is to measure the resistivity of any semiconductor material. It can measure either bulk materials or thin films. The 4-point probe consists of four equally spaced tungsten metal tips with a finite radius. Each tip is supported by springs on the distal end to minimize sample damage during probing. The four metal tips are part of an auto-mechanical stage that travels up and down during measurements. A high-impedance current source is used to supply current through the two outer probes; a voltmeter measures the voltage across the two inner probes to determine the sample resistivity.

The Signatone S-302-4 features a mounting stand for wafers up to 4" in diameter, and the unit incorporates a Keithley 4200-SCS parameter analyzer for the electrical characterization of devices, materials, and semiconductor processes. 4200-SCS can conduct tests, including very low-level DC measurements, C-V, and ultra-fast I-V for pulse and transient tests. It has 2 independent voltage sources that can slew the voltage at 1 V/ns while simultaneously measuring both the voltage and the current.

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AMETEK Scientific Instruments Solartron SI 1287A Potentiostat Galvanostat

The impedance analyzer is used to examine the impedance and other electrical properties of thin films. Typically these are films that have been made using a potentiostat.

The SI 1287A features two high-resolution digital voltmeters which provide simultaneous voltage and current measurements. They have high accuracy, stability, and linearity throughout the entire range of the instrument. The 1287A has excellent measurement resolution and accuracy down to 1μV for the reference electrodes and 1 pA for the working electrode, which makes it an ideal choice for measurements where signal levels are extremely low.

The SI 1287A data sheet on the AMETEK Scientific Instruments website.

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Metrohm Autolab PGSTAT30 Potentiostat

At the ISN, two potentiostats are used in the electrochemical synthesis of polymers and for analytical electrochemical measurements. Inside an electrochemical cell, polymers can be grown in solution or directly onto a conducting substrate. Both of the ISN potentiostats are on portable carts, allowing them to be moved to any of the ISN fume hoods or to specially modified ISN glove boxes.

The PGSTAT30 is a modular high-current potentiostat/galvanostat with a maximum current of 1 A, a compliance voltage of 30 V and the possibility to do iR-compensation. The instrument has a bandwidth of over 1 MHz.

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Deben Biaxial Tensile Mechanical Testing Machine

Deben biaxial tensile stages can be used for biaxially stretching sheet material such as textiles and also various polymers. Two axes move and the opposite axes track on slides. The tensile stage allows engineers and scientists to study the effects of biaxial force upon various materials. Systems may also be used as a uniaxial tensile stage if so required.

The ISN's biaxial mechanical tester is used primarily for evaluating the tensile strength of large sample films and fabrics.

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TA Instruments Discovery DMA Q850 Dynamic Mechanical Analyzer

Dynamic Mechanical Analyzers (DMAs) measure the mechanical properties of materials as functions of time, temperature, and frequency. A material sample is clamped at two opposite ends, with one end fixed and the other end oscillating. In addition to quantifying viscoelastic properties of materials, DMAs can also quantify finished component and product characteristics, reflecting the important contribution that processing has on end-use product performance. A DMA is commonly used to measure glass transition temperatures (Tg) and secondary transitions, orientation caused by processing, cold crystallization, cure optimization, filler effects in composites, and more. A DMA provides an accurate measure of material modulus and product stiffness plus other important mechanical properties such as damping, creep, and stress relaxation.

A DMA is a mechanical instrument that applies specific displacement or force to a sample and quantifies its force versus displacement response. It calculates the phase relationship between the signals. This enables a DMA instrument to quantify the elastic versus viscous components of the sample response, which is crucial for reliable and complete viscoelastic property characterization such as Storage Modulus, Loss Modulus, and Tan 𝛿.

The DMA Q850 provides a range of force measurements from 0.1 mN to 18 N and a temperature range from approximately -160℃  to 600 ℃.

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PAI Gas Gun with Cordin Scientific Imaging High Speed Rotating CMOS Camera

Manufactured by PAI (Physics Applications Inc.), the ISN gas gun is a single stage gas gun with a 0.5” bore. It has a velocity range of 65–5300 ft/s (20–1,600 m/s) due to an integrated Hoke 0760A4 pump that generates 33k PSI pressure. It is used to launch projectiles at material samples in order to evaluate their ballistic properties. It is also used for launching polymeric projectiles at a fixed solid metal plate in order to observe the deformation of the sample. 

The gas gun is paired with a Cordin Scientific Imaging high speed rotating CMOS camera. This camera features 32 imagers for capturing the target impact in high detail and rapid series.

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TA Instruments ElectroForce DMA 3200 High Force Dynamic Mechanical Analyzer

The DMA 3200 features patented ElectroForce linear motor technology enabling a single instrument to deliver unequalled performance and data accuracy. This unique motor technology combines powerful rare-earth magnets with a frictionless flexural suspension for the most precise force and displacement control over a wide range of frequencies and amplitudes. The DMA 3200 motor delivers a force output of up to 500 N and controlled displacements ranging from 1 micron to 13 mm. Testing can be conducted in both static and dynamic modes.

(Instrument specifications from TA Instruments, https://www.tainstruments.com/dma-3200/)

Instron Dynatup 9250 Impact Testing Machine

The drop weight tower is the ISN's instrument for the low strain-rate testing of the mechanical properties of materials.

At full force, the Dynatup 9250 provides complete computer control with impact velocities up to 22 m/s. The entire impact event can be captured, plotted, and analyzed to determine the ductile-to-brittle transition point, ductility, incipient damage, max load, absorbed energy, and other qualities. 

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PAI 6120-41-22S-7X10 Split Hopkinson Pressure Bar

The Split Hopkinson Bar, sometimes known as a Kolsky Bar, is an example of medium strain-rate testing. It helps to provide the user with an observation of the dynamic stress-strain behavior of a sample material. The ISN maintains a PAI (Physics Applications, Inc.) Split Hopkinson Bar with a maximum strain rate of 5000 s^-1.

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Custom ZwickRoell Material Testing Machine

The ZwickRoell extensometer is used to test the tensile strength; the compression, bend, fatigue, and impact resistance; and the hardness of materials and components, simplifying the evaluation of the performance and the mechanical properties of the material being examined.

The ISN's material testing machine is based on a Zwick T1-FR010TH Material Testing Machine that is upgraded with modern electronics to approximate the specifications and capabilities of a Zwick AllroundLine Universal Testing Machine Z100, which has a crosshead speed (v_min–v_max) of 0.00005–1000 mm/min and a maximum crosshead return speed of 1500 mm/min. It has a test load of 5 kN–250 kN.

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Brookhaven Instruments NanoBrook ZetaPALS

In a solution, particles have a surface charge. The Zeta Potential Analyzer measures that surface charge for particles of sizes ranging from 10 nm-300 µm. It uses phase analysis light scattering (PALS) to determine the electrophoretic mobility of roughly spherical particles in colloidal suspensions. It is far more accurate than the laser Doppler method, particularly near the isoelectric point of suspension.

The NanoBrook ZetaPALS incorporates both traditional ELS and the more sensitive and versatile Phase Analysis Light Scattering (PALS). The instrument has a mobility range of 10^-11 to 10^-7 m² /V•s and a Zeta potential range of -500 mV to 500 mV, depending on the sample.

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Micromeritics 3Flex

The Flex family of  high-performance adsorption analyzers for measuring surface area, pore size, and pore volume of powders and particulate materials.  Standard methods or user customized protocols can be used to characterize adsorbents, catalysts, zeolites, MOFs, APIs, excipients, and a wide variety of porous and non-porous materials.  The 3Flex is ideally suited for gas or vapor adsorption analysis of microporous (< 2nm) and mesoporous (2 to 50nm) materials and delivers superior accuracy, resolution and data reduction.

A chemisorption option extends the application range of both Flex to both physical and chemical adsorption for characterizing the texture and active surface of catalysts, catalyst supports, sensors and a variety of other materials.

The 3Flex brochure on the Micromeritics website.

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TA Instruments Discovery HR-20 Hybrid Rheometer

The ISN's Discovery HR-20 features TA’s Magnetic Thrust Bearing which reduces basic system friction by 70% compared to traditional designs. By eliminating the contributions of high pressure, turbulent air flow from the measurement system, lower torques can be measured reliably and accurately.

Furthermore, the Discovery HR-20's dual reader improves phase angle precision by 70% compared to conventional single-reader designs. This leads directly to a more accurate measurement of G’, G”, and tan δ. The sensor eliminates errors associated with thermal expansion without the need for special high inertia iron core geometries and environmental systems.

The Discovery HR-20 brochure on the TA Instruments website.

For additional training information and user tips, see the TA Instruments YouTube channel.

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Horiba Jobin Yvon LabRAM HR800 Confocal Raman Spectrometer

Raman spectroscopy is a non-destructive optical method, which is based on the laser-beam focused on the surface of the sample. By using Raman measurement, detailed information about chemical composition, crystal structure, and the nature of chemical bonds can be obtained. Raman spectroscopy can be used in analysis of both organic and inorganic materials. Samples can be either solid or liquid.

In μ-Raman measurement, the spot size of the laser beam is kept very small, only a few micrometers in diameter. This makes it possible to get very accurate spatial information about the sample under investigation. It is also possible to scan the beam across the sample surface and to get information about the changes in the chemical compositions or phases of the sample. Also, information considering the mechanical stresses of the sample can be obtained.

LabRAM HR800 is a high-resolution confocal μ-Raman system where the analysis area and depth can be limited down to one μm and two μm, respectively.

The system is equipped with 532 nm, 633 nm, and 785 nm laser sources.

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Thermo Nicolet iS50 FTIR Spectrometer with built-in ATR

The FTIR measures the chemical signature of materials. A researcher can tell by the peaks of the spectrum what material is being observed. The ISN has several specialized FTIR accessories that allow the characterization of thin film samples in reflectance and attenuated total reflectance modes. 

For Transmission Measurements: 
DLaTGS detector (5000 - 100 cm-1) Liquid N2 Cooled MCT-A Detector with CdTe window (11,700-600 cm-1)
For built-in diamond ATR Measurements: DLaTGS detector (5000 - 100 cm-1)

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Park Systems Accurion Nanofilm EP4 Spectroscopic Imaging Ellipsometer

Imaging ellipsometers combine the benefits of ellipsometry and optical microscopy in a single device. The unification of the two technologies creates a unique metrology tool that redefines the limits of both ellipsometric measurements and polarization-contrast microscopy. The enhanced spatial resolution of imaging ellipsometers (about 1 µm) expands ellipsometry into new areas of microanalysis, microelectronics, and bio analytics.

The EP4 combines ellipsometry and microscopy. This enables the characterization of thickness and refractive index with the sensitivity of ellipsometry on micro-structures as small as 1 µm. The microscopic part enables a simultaneous measurement of all structures inside the field of view of the optical system. Conventional ellipsometers have to focus on the measurement spot, while not achieving comparable lateral resolution, and measure spot by spot. it provides a spectral range of 250–1700 nm.

The microscopic part of the EP4 enables an ellipsometric-enhanced contrast for microscopic images obtained. Minor changes in refractive index or thickness can be seen in the live view of the camera. This allows to identify regions of interest for the ellipsometric measurements to obtain values for thickness (0.1 nm–10 µm) and refractive index. 3D maps of the lateral variation of thickness and/or refractive index can be recorded within a single measurement.

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Horiba Jobin Yvon Fluorolog-3 Modular Spectrofluorometer

The Spectrofluorometer measures the fluorescence excitation or emission spectrum of liquid, solid, or thin film samples.

Fluorescence spectroscopy has certain advantages over other optical spectroscopies, namely sensitivity (<10–12 mol) and specificity. Fluorescence spectroscopy is sensitive to the micro-environment of a molecule (up to ~10 nm away), and depends on molecular motion.

The Fluorolog-3 combines high sensitivity, fast speed, and full automation for all types of steady-state fluorescence research in quantum chemistry, materials science, biology, analysis, and quality control. The device is completely computer-controlled, and delivers high-quality fluorescence data throughout the ultraviolet, visible, and near-IR regions of the electromagnetic spectrum.

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J.A. Woollam M-2000D Spectroscopic Ellipsometer

The Spectroscopic Ellipsometer measures the thickness of thin films. Light with a known polarization is reflected off a sample at a known angle, the polarization will change based on the refractive index (known) and the film thickness (unknown). By measuring the polarization change, one can model the resulting spectrum to extract the film thickness.

The ISN's Woollam M-2000D Spectroscopic Ellipsometer features an XLS-100 head unit. It has a spectral range of 193–1000 nm.

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Oxford Instruments WITec alpha300 R Raman Imaging Microscope

The Raman effect is based on inelastic scattering of excitation light by the molecules of gaseous, liquid, or solid materials. The interaction of a molecule with photons causes vibrations of its chemical bonds, leading to specific energy shifts in the scattered light that can be identified in its Raman spectrum.

Chemical compounds can be easily identified by this individual spectral “fingerprint” in a nondestructive imaging process. When Raman spectra are collected at every measurement point using a confocal microscope combined with a spectrometer, a Raman image can be generated that visualizes the distribution of the sample's compounds.

The ISN’s alpha300 R features 325 nm, 532 nm, 633 nm, and 785 nm lasers.

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Agilent Technologies 5975C TAD Gas Chromatograph/Mass Selective Detector (GC/MSD) system

The ISN's Agilent Technologies 5975C TAD Inert XL MSD Gas Chromatograph/Mass Selective Detector (GC/MSD) system with CI High Mass Performance Turbo Pump is a transmission quadrupole mass spectrometer for qualitative and quantitative analysis in electron ionization (EI), positive chemical ionization (PCI), and negative chemical ionization (NCI) modes.

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Agilent Cary 60 UV-Vis Spectrophotometer

A spectrophotometer is an instrument that measures the amount of light that a sample absorbs. Spectrophotometers work by passing light beam of known intensity through a sample and measuring the resulting beam after the sample. Such instruments can also determine the amount of a particular substance present in the sample but further analyzing them resulting beam.

The Cary 60 UV-Vis spectrophotometer has a wavelength range of 190–1100 nm that can be scanned in under three seconds. The xenon source lamp requires zero warmup, and causes no photodegradation of samples. Fast reactions can be recorded with 80 data points per second. The Cary 60 is well-suited as a routine UV-Vis spectrophotometer or for use in teaching labs.

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Agilent Cary 7000 Universal Measurement Spectrophotometer UV-Vis-NIR Spectrometer

The Agilent Cary 7000 universal measurement spectrophotometer (UMS) allows users to collect hundreds of UV-Vis-NIR spectra overnight or characterize optical components and thin films in minutes. The Cary 7000 UMS is a turn-key solution for research, development, and QA/QC in optics, thin films/coatings, solar, and glass. 

The Cary 7000 UMS features multiangle specular reflectance and transmittance capabilities that expand research while the automated reflectance and transmission reduce analysis time. It achieves complete sample characterization and measures absolute reflection and transmission in a single sequence at variable angle and s or p polarization without moving or disturbing the sample.  It measure diffusely scattered transmission and reflection at angle, with the freedom to control detector and sample position independently. It features a large sample chamber to accommodate many sample types and delivering 360 degree rotational flexibility. It offers a maximum scanning speed of 2000 nm/min in the UV–vis range and 8000 nm/min in the near IR, a spectral bandwidth of 0.01–5.00 nm in UV-vis and 0.04–20 nm in NIR, and a wavelength range of 175–3300 nm. A 10 Abs photometric range ensures high-quality results with challenging sample measurements, such as high optical density (OD) or under difficult measurement conditions.

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Micromeritics ASAP 2020 Accelerated Surface Area and Porosimetry System

For small pore-size measurements (0.2–500 nm)

Accurate and precise surface area and porosimetry measurements are essential to the determination of the effectiveness and quality of a wide variety of materials. The Micromeritics ASAP 2020 Accelerated Surface Area and Porosimetry system integrates multiple gas sorption techniques into a single, convenient tabletop instrument.

The ASAP 2020 provides maximum versatility over a remarkable range of applications. System features include dual independent vacuum systems allowing simultaneous preparation of two samples and analysis of a third, a two-station intelligent degas system for fully automated degassing with precisely controlled heating profiles, and a flexible, interactive reporting system that includes a graphical user interface allowing custom presentation of results.

The ASAP 2020 brochure on the Micromeritics website.

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Ramé-Hart Model 500 Advanced Goniometer / Tensiometer

A contact angle can be measured by producing a drop of liquid on a solid. The angle formed between the solid/liquid interface and the liquid/vapor interface is referred to as the contact angle. The most common method for measurement involves looking at the profile of the drop and measuring two-dimensionally the angle formed between the solid and the drop profile with the vertex at the three-phase line. Young's equation is used to describe the interactions between the forces of cohesion and adhesion and measure what is referred to as surface energy.

The ISN's Model 500 goniometer has been upgraded to include a fast U4 Series SuperSpeed camera at 520 fps and DROPimage Advanced software, which measures contact angle, surface energy, surface and interfacial tension, advancing and receding contact angle, surface dilatational elasticity and viscosity. It is well-suited to time-dependent and dynamic studies. The instrument features a temperature controlled stage with a temperature range up to 300° C at 0.1° C precision).

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Custom Built Thickness Measurement System

The ISN maintains a custom built thickness measurement system featuring two 30 mm focused spot-type Keyence CL-P030 1D Confocal Displacement Sensor Heads and a Zaber X-ASR100B120B-SE03D12-KX14P Motorized XY Aperture Stage.

The instrument can measure film/sample thicknesses from about ~1 µm to 7.4 mm over a sample sizes up to 100 mm x 120 mm in X and Y. The Zaber motorized XY aperture stage features a 0.15625 µm micro step size with 40 µm accuracy and sub-2 µm repeatability.

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TA Instruments DSC 2500 Differential Scanning Calorimeter   
(includes TA Instruments RCS 90 Refrigerated Cooling System)

NOTE: Users must run their sample on the TGA before using the DSC.

Differential Scanning Calorimeters (DSCs) measure temperatures and heat flows associated with thermal transitions in a material. A DSC measures energy absorption as a material sample undergoes phase transitions. As the sample is heated, energy is absorbed and peaks will show where a phase transition has taken place. Common usage includes investigation, selection, comparison, and end-use performance evaluation of materials in research, quality control and production applications. Properties measured by TA Instruments’ DSC techniques include glass transitions, “cold” crystallization, phase changes, melting, crystallization, product stability, cure/cure kinetics, and oxidative stability.

At the ISN, this instrument is primarily used to characterize polymeric materials and the results will yield glass transition temperatures as well as other phase transformation temperatures/energies.

The DSC 2500 features a baseline flatness (-50 to 300° C) of ≤5 μW and a baseline repeatability of <10µW. Within a temperature range of -180°C–725°C, it has a temperature accuracy of ±0.025° C and a temperature precision of ±0.005° C. It has an enthalpy precision of ±0.04%.

The equipped RCS 90 cooling system permits DSC operation from -90° C to 550° C. The RCS90 has the ability to cool the Tzero DSC Cell from 500 to 25° C in around 7 minutes.

For additional training information and user tips, see the TA Instruments YouTube channel.

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TA Instruments Discovery TGA 5500 Thermogravimetric Analyzer

Thermal analyzers typically measure heat flow, weight loss, dimension change, or mechanical properties as a function of temperature. Understanding a material’s behavior under different temperatures is crucial for the successful design, processing, and end use of completed products.

The TGA 5500 is designed and built to maximize temperature control and minimize drift, and it has less drift than other competitive TGAs including after post-test data manipulation. An IR furnace delivers the very fast heating and cooling rates, and the autosampler increases productivity.

The ultra-low drift balance design ensures accurate detection of weight changes; the high capacity (1g) balance with auto-ranging capability ensures high sensitivity no matter the size of the sample; the free-hanging sample eliminates the heat sink prevalent in top-loading designs, for efficient heat transfer and gas flow around the sample, the thermally isolated balance with low drift and high sensitivity provides accurate real time data.

The ISN’s TGA 5500 has an ambient temperature range of up to 1200° C with an accuracy of ±1° C and a linear heating rate of 0.1–500° C/min.

For additional training information and user tips, see the TA Instruments YouTube channel.

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