Rapid thermal processing chamber for in-situ x-ray diffraction Md. Imteyaz Ahmad, Douglas G. Van Campen, Jeremy D. Fields, Jiafan Yu, Vanessa L. Pool, Philip A. Parilla , David S. Ginley, Maikel F. A. M. Van Hest, and Michael F. Toney Citation: Review of Scientific Instruments 86, 013902 (2015); doi: 10.1063/1.4904848 View online: http://dx.doi.org/10.1063/1.4904848 View Table of Contents: http://scitation.aip.org/content/aip/journal/rsi/86/1?ver=pdfcov Published by the AIP Publishing Articles you may be interested in A furnace to 1200 K for in situ heating x-ray diffraction, small angle x-ray scattering, and x-ray absorption fine structure experiments Rev. Sci. Instrum. 79, 126101 (2008); 10.1063/1.3021473 Erratum: “An image plate chamber for x-ray diffraction experiments in Debye–Scherrer geometry” [Rev. Sci. Instrum. 71, 4007 (2000)] Rev. Sci. Instrum. 72, 2511 (2001); 10.1063/1.1355274 Construction of laser-heated diamond anvil cell system for in situ x-ray diffraction study at SPring-8 Rev. Sci. Instrum. 72, 1289 (2001); 10.1063/1.1343869 An image plate chamber for x-ray diffraction experiments in Debye–Scherrer geometry Rev. Sci. Instrum. 71, 4007 (2000); 10.1063/1.1318915 A novel thick-layer electrochemical cell for in situ x-ray diffraction Rev. Sci. Instrum. 69, 512 (1998); 10.1063/1.1148723
This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP: 137.99.31.134 On: Mon, 01 Jun 2015 08:29:06
REVIEW OF SCIENTIFIC INSTRUMENTS 86, 013902 (2015)
Rapid thermal processing chamber for in-situ x-ray diffraction Md. Imteyaz Ahmad,1 Douglas G. Van Campen,1 Jeremy D. Fields,2 Jiafan Yu,1 Vanessa L. Pool,1 Philip A. Parilla,2 David S. Ginley,2 Maikel F. A. M. Van Hest,1 and Michael F. Toney1,a) 1 2
SSRL, SLAC National Accelerator Laboratory, 2575, Sand Hill Road, Menlo Park, California 94025, USA National Renewable Energy Laboratory, Golden, Colorado 80401, USA
(Received 27 September 2014; accepted 8 December 2014; published online 5 January 2015) Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 ◦Cs−1, and with a maximum operating temperature of 1200 ◦C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi2O3-SiO2 glass frit obtained during heating with ramp rates 5 ◦C s−1 and 100 ◦C s−1, revealing numerous phase changes. C 2015 AIP Publishing LLC. [http://dx.doi.org/10.1063/1.4904848] I. INTRODUCTION
Rapid thermal processing (RTP) is widely used for the processing of photovoltaics (PV), electronics, and energy storage materials.1–4 RTP involves fast heating ramp rates, generally in the range of 10-100 ◦C s−1 and processing times of seconds to minutes.5 Compared to conventional thermal processes (e.g., belt-furnace), advantages include low thermal cost, high throughput, and better access to metastable phases. So far, RTP process optimization has evolved empirically based on the microstructure and properties obtained after repeated process iterations. Thus, the reaction pathways and accompanying phase transformations during RTP are poorly understood, primarily due to a lack of in-situ characterization on a time-scale characteristic of the fast heating rates. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP. RTP is also ideally suited for synthesis of metastable phases. Formation of a specific material phase depends strongly on the processing conditions, specifically the heating and cooling rates.6,7 Rapid addition or removal of energy during synthesis can result in kinetic constraints, allowing access to metastability. This is potentially valuable since metastable phases often have different and useful properties compared to equilibrium phases, and this can be beneficial for certain applications.8 Since the phase evolution depends strongly on the process conditions, understanding the relationship between key process conditions and the reaction pathway is paramount.9–11 Therefore, an in-situ RTP facility for the characterization of the reaction pathways as a function of processing parameters (e.g., ramp rate, processing temperature, and precursor) is particularly useful here. a)Author to whom correspondence should be addressed. Electronic mail:
[email protected]
Up to now, there has been no capability for in-situ characterization during RTP with heating rates as high as 100 ◦C s−1, as commonly applied in industry practice, and previous technologies have not allowed simultaneous recording of diffraction data with time resolution of the order of 100 ms. Beamline X20C at the National Synchrotron Light Source (not presently operational) was equipped with a RTP tool, which could heat at
This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP: 137.99.31.134 On: Mon, 01 Jun 2015 08:29:06
REVIEW OF SCIENTIFIC INSTRUMENTS 86, 013902 (2015)
Rapid thermal processing chamber for in-situ x-ray diffraction Md. Imteyaz Ahmad,1 Douglas G. Van Campen,1 Jeremy D. Fields,2 Jiafan Yu,1 Vanessa L. Pool,1 Philip A. Parilla,2 David S. Ginley,2 Maikel F. A. M. Van Hest,1 and Michael F. Toney1,a) 1 2
SSRL, SLAC National Accelerator Laboratory, 2575, Sand Hill Road, Menlo Park, California 94025, USA National Renewable Energy Laboratory, Golden, Colorado 80401, USA
(Received 27 September 2014; accepted 8 December 2014; published online 5 January 2015) Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 ◦Cs−1, and with a maximum operating temperature of 1200 ◦C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi2O3-SiO2 glass frit obtained during heating with ramp rates 5 ◦C s−1 and 100 ◦C s−1, revealing numerous phase changes. C 2015 AIP Publishing LLC. [http://dx.doi.org/10.1063/1.4904848] I. INTRODUCTION
Rapid thermal processing (RTP) is widely used for the processing of photovoltaics (PV), electronics, and energy storage materials.1–4 RTP involves fast heating ramp rates, generally in the range of 10-100 ◦C s−1 and processing times of seconds to minutes.5 Compared to conventional thermal processes (e.g., belt-furnace), advantages include low thermal cost, high throughput, and better access to metastable phases. So far, RTP process optimization has evolved empirically based on the microstructure and properties obtained after repeated process iterations. Thus, the reaction pathways and accompanying phase transformations during RTP are poorly understood, primarily due to a lack of in-situ characterization on a time-scale characteristic of the fast heating rates. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP. RTP is also ideally suited for synthesis of metastable phases. Formation of a specific material phase depends strongly on the processing conditions, specifically the heating and cooling rates.6,7 Rapid addition or removal of energy during synthesis can result in kinetic constraints, allowing access to metastability. This is potentially valuable since metastable phases often have different and useful properties compared to equilibrium phases, and this can be beneficial for certain applications.8 Since the phase evolution depends strongly on the process conditions, understanding the relationship between key process conditions and the reaction pathway is paramount.9–11 Therefore, an in-situ RTP facility for the characterization of the reaction pathways as a function of processing parameters (e.g., ramp rate, processing temperature, and precursor) is particularly useful here. a)Author to whom correspondence should be addressed. Electronic mail:
[email protected]
Up to now, there has been no capability for in-situ characterization during RTP with heating rates as high as 100 ◦C s−1, as commonly applied in industry practice, and previous technologies have not allowed simultaneous recording of diffraction data with time resolution of the order of 100 ms. Beamline X20C at the National Synchrotron Light Source (not presently operational) was equipped with a RTP tool, which could heat at
