Materials Testing - Thermal, Mechanical, Electrical Materials Testing Services Provided by CoorsTek

Topics Covered

Background

Quality Assurance

Safety

Thermal Testing

DSC – Differential Scanning Calorimetry

DTA – Differential Thermal Analysis

TMA – Thermomechanical Analysis

DMA – Dynamic Mechanical Analysis

Orton Quartz-Tube Dilatometer

Theta High/Low Temperature Dilatometer

Microscopy

Physical Testing

Mechanical Testing

Micromeritics

Electrical Testing

X-Ray Diffraction

Chemical Testing

X-Ray Fluorescence

Elemental Analysis by Inductively Coupled Plasma-Optical Emission Spectroscopy

Elemental Analysis by Inductively Coupled Plasma-Mass Spectrometry

Analysis Case File: Laser Ablation – ICP-MS of a Ceramic Material

Additional Facilities

Tests / Sample Sizes

Background

The CoorsTek Analytical Laboratory offers a wide variety of services – from Analytical Chemistry to Material Testing. We employ a staff of trained professionals using the latest techniques and state-of-the-art analytical instrumentation to provide you with quick and accurate solutions tailored to your particular needs.

Standard services include:

•        X-Ray Fluorescence

•        X-Ray Diffraction

•        ICP-Optical Emission Spectroscopy

•        ICP-Mass Spectrometry

•        Classical Wet Chemistry

•        Electrical Testing

•        Mechanical Testing

•        Particle Size Distribution

•        Surface Area Measurements

•        Thermal Analysis

•        Scanning Electron Microscopy

•        Optical Microscopy

•        Atomic Force Microscopy

         Custom Services – Many tests and analyses other than those listed are available. Please contact us for fees and techniques on particular requirements.

Quality Assurance

CoorsTek Analytical Laboratory is committed to a quality program designed to provide the highest quality attainable for our customers. This proven quality program assures the highest probability of confidence both in the precision as well as the accuracy of our analyses.

To insure that all equipment and instrumentation are functioning at optimum capability, all analytical instruments are calibrated on a regularly scheduled basis. Calibration data are traceable to the National Institute of Standards and Technology or other recognized reputable sources. Complete calibration records are maintained in compliance with government and military standards.

Safety

If available, please submit a Material Safety Data Sheet to help with proper handling and disposal.

Thermal Testing

Thermal testing capabilities include low and high-temperature thermal expansion,“green” ceramic shrinkage, reaction enthalpy, heat capacity, glass transition temperature, reaction kinetics, viscoelastic properties, loss on drying, loss on ignition filler content, binder content, softening temperature, and rheological behavior.

The Thermal Testing Laboratory is equipped with Orton Quartz-Tube Dilatometers, Theta High/Low Temperature Dilatometer, DuPont Thermal Analyzer with DTA, DSC, TMA, TGA, and DMA.

DSC – Differential Scanning Calorimetry

An enthalpy-change method in which the difference in the energy inputs into a substance and a reference material is measured as a function of temperature, while the substance and the reference material are subjected to a controlled atmosphere and temperature program. Temperature range: -180° C to 700° C.

Typical Applications:

         Melting Points

         Glass Transition

         Degree of Cure

         Oxidative Stability

         Heat of Fusion

         Crystallinity

         Specific Heat Capacity

         Kinetics

DTA – Differential Thermal Analysis

A temperature-change method in which the temperature difference between a substance and a reference material is measured as a function of temperature, while the substance and the reference material are subjected to a controlled atmosphere and temperature program. Temperature range: -180° C to 1600° C.

Typical Applications:

         Melting points

         Glass Transition

         Degree of Cure

         Oxidative Stability

         Heat of Fusion

         Crystallinity

TGA – Thermogravimetric Analysis

A dynamic-mass change method where the mass of a sample is measured as a function of temperature while the sample is subjected to a controlled atmosphere and temperature program. Temperature range: Ambient to 1200° C.

Typical Applications:

         Compositional Analysis

         Thermal Stability

         Reactive Atmosphere Analysis

TMA – Thermomechanical Analysis

A mechanical-characteristic-change method in which the deformation of a substance is measured under nonoscillatory load as a function of temperature, while the substance is subjected to a controlled atmosphere and temperature program. Temperature range: -160° C to 1000° C.

Typical Applications:

         Expansion Coefficient

         Glass Transition Temperature

         Physical Testing

         Thermal Dimensional Stability

         Softening & Yield Temperature

DMA – Dynamic Mechanical Analysis

A mechanical characteristic-change method in which the dynamic modulus and/or damping of a substance is measured under oscillatory load as a function of temperature, while the substance is subjected to a controlled temperature program. Temperature range: -150° C to 500° C.

Typical Applications:

         Curing of Thermosets

         Polymer Blend Compatibility

         Analysis of Soft Elastomers

         Observation of Plasticizer Effects

         Measure of Subtle Transitions

Orton Quartz-Tube Dilatometer

A mechanical characteristic-change method where the length of a sample is measured in a quartz tube as a function of temperature, while the sample is subjected to a heating profile. Temperature range: ambient to 1000° C.

Typical Application:

         Expansion Coefficient

Theta High/Low Temperature Dilatometer

A mechanical characteristic-change method where the length of a sample is measured in a 995 Al2O3 tube as a function of temperature, while the sample is subjected to a heating profile Low temperature range: -140° C to 350° C, High temperature range: ambient to 1600° C.

Typical Applications:

         Expansion Coefficient

         “Green” Ceramic Shrinkage Profile

Microscopy

The Microscopy Laboratory performs qualitative measurements by light optical and electron microscopic techniques and elemental analyses of micro samples by X-ray Spectroscopy.

The laboratory routinely produces thin and polished sections of ceramic material with corresponding photomicrographic examination for crystal size and related properties, and in the identification of foreign substances by observation of optical properties. Typical tests performed by the laboratory are crystal size by linear intercept, thin and polished sections, particle size distribution, and identification of foreign substances.

Instrumentation includes JEOL (JSM-840) SEM with energy dispersive X-ray Spectroscopy (EDS), Zeiss Ultrashot 11 and 111B Camera Microscopes, a Zeiss Universal Microscope, Bausch & Lomb stereo binocular microscopes, and a Burleigh Atomic Force Microscope.

Typical Applications:

         Particle Sizing

         Sieve Metallography

         Thin Section

         Polished Section

         Photomicrographs

         AFM

         Optical Microscopy

Physical Testing

Mechanical Testing

Various methods are used for mechanical testing. Flexural and compressive strengths are routinely performed. Fracture toughness can be measured using similar techniques. From these measurements, Weibull modulus can be determined.

Young’s modulus, shear modulus and Poisson’s ratio can be measured by sonic resonance. Knoop, Vickers, and Rockwell hardness can be done at various loads.

The Mechanical Testing Laboratory is equipped with a Sintech system, as well as an Instron 20,000 lb. system, a Leco Microhardness tester, various Wilson Rockwell testers, various polishing machines, abrasion resistance testing machines and Tinius Olson Impact Testing machines.

Typical Applications:

         Abrasion Resistance

         Hardness

         Fracture Mechanics

         Strength

         Impact

         Dye Penetrant Inspection

Micromeritics

The Micromeritics Laboratory is concerned with the measurement of surface area, porosity, density, and particle-size distribution of powders.

Surface area is determined by the classical gas adsorption method of Brunauer, Emmet and Teller (BET). The average particle size distribution is determined by several techniques including sedimentation and sieve analysis. Porosity is measured by mercury intrusion and density by suspension and bulk methods.

The laboratory instrumentation includes a Micromeritics-BET Apparatus, a Schimadzu Particle Size Analyzer, Micromeritics Mercury Porosimeter and certified sieves from 400 mesh to 8 mesh.

Typical Applications:

         Surface area analysis

         Pore size distribution

         Sedigraph Analysis

         Density

Electrical Testing

The Electrical Testing Laboratory is equipped to perform electrical characterizations of all types of electrical insulating materials under a varietry of conditions and electrical frequencies. Dielectric strength is determined under oil at 60 Hz ac. Dielectric constant is evaluated at frequencies up to 2.0 MHz.

Dielectric strength is checked on an instrument capable of applying 150 kvp ac. Dielectric constant and loss are measured on a QuadTech 7600 RLC meter. Volume and surface resistivities can be measured in a small furnace coupled to a Hewlett-Packard 4339B high resistivity meter.

Typical Applications:

         Dielectric Constant

         Dissipation factor

         Loss Index

         Volume Resistivity

         Surface Resistivity

         Dielectric Strength

X-Ray Diffraction

Our X-Ray Diffraction Laboratory offers a variety of X-ray powder diffraction analyses including qualitative, semi-quantitative and quantitative measurements based on the crystal structure of the sample.

Instrumentation includes a high resolution Scintag Automated Powder Diffraction system with a theta-theta goniometer and a germanium solid-state detector.

Typical Applications:

         Qualitative identification of unknowns

         Quantitative determination of free quartz

         Quantitative determination of alpha alumina, mullite and cristobalite in alumina ceramics

         Quantitative determination of cubic and monoclinic phases in zirconia

         Quantitative determination of alpha and beta phases in silicon-nitride

Chemical Testing

X-Ray Fluorescence

The X-Ray fluorescence technique is method for elemental analysis. Samples are excited with an X-ray beam and the resulting secondary or fluorescent X-radiation is measured. Quantitative and qualitative analyses are provided for elements above neon in the periodic table.

XRF is our method of choice for major oxide chemical analysis of ceramics, refractories, glasses, geological raw materials, and slags. We are particularly adept at making standards from pure oxides to match the sample matrix using the fused lithium borate glass disk method. Most oxides can be analyzed by this method to a detection limit of 0.05% with slightly higher limits for light elements. In addition we are equipped to prepare pressed pellets and to use whole sample and thin sample techniques.

Instrumentation includes a computer controlled Phillips MagiX Sequential X-Ray Spectrometer system. Computer control makes the method particularly useful for multiple samples and quality control work.

Typical Applications:

         Ceramics

         Glasses

         Metals

         Slags

         Refractories

         Geological Materials

Elemental Analysis by Inductively Coupled Plasma-Optical Emission Spectroscopy

ICP-OES is a versatile technique for elemental analysis of a wide variety of materials. Concentrations for most metals and some nonmetals can be determined at major, minor or trace levels using standard methods. Materials routinely analyzed include ceramics, glass, metals, alloys, aqueous solutions, pharmaceuticals and pottery glazes.

The laboratory uses a sequential Thermo-Jarrel Ash AtomScan 25 ICP-OES. This instrument is capable of scanning essentially any emission line from 160 to 800 nm.

Typical Applications:

         Ceramics (aluminas, zirconias, etc.)

         Glass

         Solders

         Electroplating solutions

         Organometallic compounds (such as magnesium stearate)

         Pottery glazes (for heavy metal release)

Elemental Analysis by Inductively Coupled Plasma-Mass Spectrometry

ICP-MS is a rapid, multi-element analytical technique capable of determining elemental and isotopic concentrations to sub ng/ml levels in solution. It combines two proven technologies: an inductively coupled plasma for ion generation and a quadrupole mass analyzer for the subsequent separation and detection of these ions. Up to 70 elements can be determined in every scan with this technique.

The laboratory uses a VG Elemental PlasmaQuad 2+ ICP-MS with Laser Lab direct solid sampling accessory.

With the Laser Lab sampling accessory, direct solid analysis is routine. The laser can vaporize a contaminated surface without affecting the underlying material of a solid sample. Sensitivities are generally to the μg/g level. Since there is no sample preparation, there is less opportunity for contamination.

Typical Applications:

         Isotope ratios

         Aqueous Solutions

         Metals

         Solid surfaces/ contaminated areas

         Ceramics

         Glass

         Micro-electronic devices

Analysis Case File: Laser Ablation – ICP-MS of a Ceramic Material

The Laser Ablation sampling accessory is a powerful tool for elemental analysis when used with the ICP-MS. For some solid samples a total dissolution is not practical because the distribution of the elements of concern may be inhomogeneous or because dissolution may introduce contamination. CoorsTek Analytical Laboratory applies the laser sampling technique when it is the most appropriate and when a fast, inexpensive qualitative survey is needed.

A sample of ZrSnTiO4 ceramic was submitted for analysis. The client requested a qualitative elemental analysis for trace contaminants. We studied the material by LA-ICP-MS and also by SEM/EDS. The former identified 14 elements to be present in the sample while the latter identified only four. Since a standard material was not available, an accurate quantitative determination of the elements could not be made using these techniques. However, since the LA-ICP-MS technique found many more elements than the SEM/EDS technique, relative sensitivity became of interest.

As a first order approach to quantitative determination, the integrated spectral peak intensities were compared as though their concentrations were directly proportional to the elemental concentrations. In the following table the units are in percent of total detected peak intensity:

From the table it is seen that the two techniques are in reasonable agreement regarding the concentrations of the majors components, but the estimated detection limit of the SEM/EDS is only about 1% whereas the LA-ICP-MS detected impurities down to the parts per million level.

In addition to sensitivity, LA-ICP-MS has the advantages of:

1.      Depth profiling capability

2.      No requirement for electrical conductivity in samples

3.      Detection of Li, Be and B

SEM/EDS has two advantages of its own:

1.      The spatial resolution is superior

2.      The analysis is non-destructive

Comparison of Analysis Techniques

 

LA-ICP-MS

SEM/EDS

Ti

48

42.6

Cu

0.0029

-

Zn

0.86

1.3

Zr

40

43.7

Sn

9.2

12.4

Sb

0.00050

-

Ba

0.0042

-

La

1.4

-

Ce

0.00019

-

Nd

0.0013

-

Hf

0.65

-

Ta

0.0088

-

Pb

0.0010

-

Bi

0.0021

-

Additional Facilities

The laboratory is equipped with several instruments for molecular spectroscopy and element-specific analysis. These include:

         Perkin-Elmer UV-VIS absorption spectrophotometer

         Leco carbon and sulfur analyzers

Tests / Sample Sizes

CoorsTek Analytical Laboratory offers a wide variety of services from Analytical Chemistry to Material Testing. Many of the services we offer are routine and for these services we provide standard fees for a given material. However, some samples require custom work for which we quote individual pricing. Please contact us for detailed information.

 

Source: CoorsTek

 

For more information on this source please visit CoorsTek

 

Date Added: Sep 22, 2006 | Updated: Jun 11, 2013
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