Purity of ingredients is a constant concern for the semiconductor industry,
because a mere trace of contaminants can damage or ruin tiny devices. In a step
toward solving a long-standing problem in semiconductor manufacturing, scientists
at JILA and collaborators have used their unique version of a "fine-toothed
comb" to detect minute traces of contaminant molecules in the arsine gas
used to make a variety of photonics devices.
JILA is a joint institute of the National Institute of Standards and Technology
(NIST) and the University of Colorado at Boulder (CU). The research was conducted
with collaborators from NIST’s Boulder campus and Matheson Tri-Gas (Longmont,
Colo.).

A NIST invention may help purify a process for making semiconductors used in devices such as light-emitting diodes (LEDs). ©Igor Stepovik/courtesy Shutterstock
The research, described in a new paper,* used a NIST/CU invention called cavity-enhanced
direct frequency comb spectroscopy (CE-DFCS).** It consists of an optical frequency
comb—a tool for accurately generating different colors, or frequencies,
of light—adapted to analyze the quantity, structure and dynamics of various
atoms and molecules simultaneously. The technique offers a unique combination
of speed, sensitivity, specificity and broad frequency coverage.
The semiconductor industry has long struggled to find traces of water and other
impurities in arsine gas used in manufacturing of III-V semiconductors for light-emitting
diodes (LEDs), solar-energy cells and laser diodes for DVD players. The contaminants
can alter a semiconductor’s electrical and optical properties. For instance,
water vapor can add oxygen to the material, reducing device brightness and reliability.
Traces of water are hard to identify in arsine, which absorbs light in a complex,
congested pattern across a broad frequency range. Most analytical techniques
have significant drawbacks, such as large and complex equipment or a narrow
frequency range.
The JILA comb system, previously demonstrated as a "breathalyzer"
for detecting disease***, was upgraded recently to access longer wavelengths
of light, where water strongly absorbs and arsine does not, to better identify
the water. The new paper describes the first demonstration of the comb system
in an industrial application.
In the JILA experiments, arsine gas was placed in an optical cavity where it
was "combed" by light pulses. The atoms and molecules inside the
cavity absorbed some light energy at frequencies where they switch energy levels,
vibrate or rotate. The comb’s "teeth" were used to precisely
measure the intensity of different shades of infrared light before and after
the interactions. By detecting which colors were absorbed and in what amounts—matched
against a catalog of known absorption signatures for different atoms and molecules—the
researchers could measure water concentration to very low levels.
Just 10 water molecules per billion molecules of arsine can cause semiconductor
defects. The researchers detected water at levels of 7 molecules per billion
in nitrogen gas, and at 31 molecules per billion in arsine. The researchers
are now working on extending the comb system even further into the infrared
and aiming for parts-per-trillion sensitivity.
The research was funded by the Air Force Office of Scientific Research, Defense
Advanced Research Projects Agency, Defense Threat Reduction Agency, Agilent
Technologies, and NIST.
* K.C. Cossel, F. Adler, K.A. Bertness, M.J. Thorpe, J. Feng, M.W. Raynor,
J. Ye. 2010. Analysis of Trace Impurities in Semiconductor Gas via Cavity-Enhanced
Direct Frequency Comb Spectroscopy. Applied Physics B. Published online July
20.
** U.S. Patent number 7,538,881: Sensitive, Massively Parallel, Broad-Bandwidth,
Real-Time Spectroscopy, issued in May 2009, NIST docket number 06-004, CU Technology
Transfer case number CU1541B. Licensing rights have been consolidated in CU.
*** See "Optical ‘Frequency Comb’ Can Detect the Breath of
Disease", in NIST Tech Beat Feb 19, 2008, at www.nist.gov/public_affairs/techbeat/tb2008_0219.htm#comb.