A key part of the NIST Combinatorial Methods Center 

(NCMC) is a set of facilities dedicated to the design 

and fabrication of polymer materials combinatorial 

libraries, and for developing and demonstrating 

high-throughput measurements of polymer materials 

structure and performance. In addition to being 

the central test bed for the Division’s Combinatorial 

Methods Group, these facilities help to advance NIST 

programs in biomaterials, nanomaterials, electronic 

materials, and polymer processing. Moreover, these 

labs serve as an essential demonstration and technology transfer facility through which industry part-ners 

and collaborators from academia and govern-ment 

can evaluate first-hand, NCMC methodologies and 

devices for use in their research. 

Polymer Film Library Fabrication and 

Characterization

The central NCMC facilities house a suite of devices 

for creating gradient combinatorial libraries that systematically explore factors that govern the structure 

and behavior of polymer coatings and thin films. 

The NIST Flow Coater generates film libraries that 

gradually increase in their thickness. This instrument 

is capable of creating well-behaved libraries that 

span 10 nm to a μm or more in film thickness. These 

libraries are characterized via automated interferometry and ellipsometry instrumentation in the same 

facility. Another device, pictured below, can generate 

a variety of libraries by producing a gradient in light 

exposure. One implementation of this instrument 

can create substrates that systematically vary in their 

surface energy. Characterized via an automated 

contact angle goniometer, such libraries are a key 

tool for examining the role of substrate hydrophobicity on film performance measures such as stability. 

This same instrument can create gradients in photopolymerization, UV-aging and other quantities related 

to light-exposure. Gradient hot stages in the facility 

enable high-throughput analysis of temperature 

processing, and provide a route to gradient polymer 

phase diagrams. The micro- and nano-structure 

of film libraries created in these facilities can be 

rapidly characterized through two automated optical 

microscopes, and a large-platform atomic force 

microscope.

Recently, devices for creating libraries of grafted copolymers have been added to the NCMC facility. As 

shown in the left-hand image above, this instrumentation delivers graded combinations of monomers to 

an initiator-functionalized substrate via a microfluidic 

channel. The resulting library of surface grafted 

polymers can exhibit systematic variations in polymer 

molecular weight, composition or architecture. In 

addition, this year we commissioned fabrication of a 

new instrument capable of depositing libraries of viscous polymer mixtures. Pictured above on the right, 

this direct-write instrument incorporates a miniature 

mixing rod in the deposition head, allowing delivery 

of discrete and continuous film libraries of up to three 

input fluids. In coming months, the device will be 

optimized for creating arrays of multi-component 

polymer specimens for advanced coatings applications.

FACILITIES

Measurement Facilities:

NIST Combinatorial Methods Center

Materials Science and Engineering Laboratory

854-00-02

POLYMERS DIVISION

Newest NCMC library fabrication tools

Device for creating gradients in light exposure
Materials Science and Engineering Laboratory

Polymers Division

High-Throughput Mechanical Testing

Housing instruments developed in the Division’s Mechanics of Complex Interfaces Project, a second NCMC 

facility focuses on the mechanical performance of polymer 

materials. A keystone set of devices supports the NISTdeveloped buckling metrology, which harnesses wrinkling 

instabilities to quantify the mechanical properties of thin film 

libraries. This equipment includes precision strain stages, 

environmental control chambers, and a static light scattering 

instrument to provide rapid, essential, measurements of the 

modulus of thin films.

Two pieces of equipment in this facility can accomplish highthroughput measures of surface and inter-facial adhesion 

in polymeric systems. The NCMC lens contact adhesion 

instrument, pictured above, uses the Johnson-Kendall-Roberts 

(JKR) approach to measure the weak adhesion inherent to 

biosystems and pressure sensitive adhesives. This year, the 

in-strument was modified to accomplish measurements in the 

aqueous environments relevant to cell adhesion and marine 

coatings, and a positionable probe enables systematic 

measurements across gradient libraries. For strongly 

adhering systems, such as structural adhesives, electronics 

packaging, and coat-ings materials, the NCMC has 

developed combinato-rial edge lift-off testing instrumentation 

capable of parallel delamination measurements across 

library arrays. This device drives a pre-formed array of 

flaws at the adhesive-substrate interface, and monitors this 

crack growth in parallel across a library. This instrument is 

being optimized to examine the adhesion between dissimilar 

materials inherent to application systems such as flip-chip 

epoxies and aerospace coatings.

Microfluidic Device Prototyping and Integration

The NCMC Polymer Formulations Project produces 

microfluidic technologies appropriate for the high-throughput 

analysis of the polymer solutions and mixtures central to a 

range of technologies. Central to this effort are facilities for 

prototyping microfluidic devices that hold up to the rigors 

of organic solvents, polymerization reactions, and higher 

temperatures. Key infrastructure includes the light sources 

and other equipment necessary for a NIST-developed 

process for fabricating microfluidic devices from thiolene, 

a UV patternable optical adhesive that exhibits enhanced 

solvent resistance. In addition, machining tools enable the 

production of metal microfluidic de-vices that can withstand 

both solvents and high-temperatures.

For in-situ measurements on microfluidic devices, this facility 

has a suite of fiber-based optical probes for assessing fluid 

structure and chemistry. Raman and near-IR spectroscopy 

probes enable chemical analy-sis of a wide range of fluid 

specimens, and the speed to gauge composition in real 

time. In addition, NIST-developed microfluidic Dynamic Light 

Scattering (DLS) probes allow measurements of nanoscopic 

polymer structures such as micelles and latexes, and fluid 

dispersed particles.

Michael Fasolka

(301) 975-8526

mfasolka@nist.gov

Christopher Stafford

(301) 975-4368

chris.stafford@nist.gov

Measurement Facilities:

NIST Combinatorial Methods Center

Lens contact adhesion instrument

Metal microfluidic device fitted with DLS probe