Articles | Volume 2, issue 2
https://doi.org/10.5194/mr-2-699-2021
© Author(s) 2021. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
https://doi.org/10.5194/mr-2-699-2021
© Author(s) 2021. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
On the modeling of amplitude-sensitive electron spin resonance (ESR) detection using voltage-controlled oscillator (VCO)-based ESR-on-a-chip detectors
Anh Chu
Institute of Smart Sensors, University of Stuttgart, Pfaffenwaldring 47, 70569 Stuttgart, Germany
Benedikt Schlecker
Institute of Smart Sensors, University of Stuttgart, Pfaffenwaldring 47, 70569 Stuttgart, Germany
Michal Kern
Institute of Smart Sensors, University of Stuttgart, Pfaffenwaldring 47, 70569 Stuttgart, Germany
Justin L. Goodsell
Department of Chemistry, University of Florida, Gainesville, FL32611-7200, USA
Alexander Angerhofer
Department of Chemistry, University of Florida, Gainesville, FL32611-7200, USA
Klaus Lips
Department Spins in Energy Materials and Quantum Information Science (ASPIN), Helmholtz-Zentrum Berlin für Materialien und Energie, Hahn-Meitner-Platz 1, 14109 Berlin, Germany
Jens Anders
CORRESPONDING AUTHOR
Institute of Smart Sensors and IQST (Center for Integrated Quantum Science and Technology), University of Stuttgart, Pfaffenwaldring 47, 70569 Stuttgart, Germany
Related authors
Jan Lettens, Marina Avramenko, Ilias Vandevenne, Anh Chu, Philipp Hengel, Michal Kern, Jens Anders, Peter Moens, Etienne Goovaerts, and Sofie Cambré
Magn. Reson. Discuss., https://doi.org/10.5194/mr-2024-11, https://doi.org/10.5194/mr-2024-11, 2024
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Demonstration of an ultra-compact spectrometer for electrically-detected magnetic resonance on a chip (EDMRoC) of silicon carbide MOSFETs with comparable signal-to-noise ratio as state-of-the-art conventional resonator-based EDMR. The relatively low cost, high sensitivity and limited space requirements of the EDMRoC configuration holds promise for application in basic and applied research as well as in industrial environments.
Silvio Künstner, Anh Chu, Klaus-Peter Dinse, Alexander Schnegg, Joseph E. McPeak, Boris Naydenov, Jens Anders, and Klaus Lips
Magn. Reson., 2, 673–687, https://doi.org/10.5194/mr-2-673-2021, https://doi.org/10.5194/mr-2-673-2021, 2021
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Electron paramagnetic resonance (EPR) spectroscopy is the method of choice to investigate and quantify paramagnetic species. We present the application of an unconventional EPR detection method, rapid-scan EPR, to enhance the sensitivity on an improved design of a miniaturized EPR spectrometer implemented on a silicon microchip. Due to its size, it may be integrated into complex and harsh sample environments, enabling in situ or operando EPR measurements that have previously been inaccessible.
Jan Lettens, Marina Avramenko, Ilias Vandevenne, Anh Chu, Philipp Hengel, Michal Kern, Jens Anders, Peter Moens, Etienne Goovaerts, and Sofie Cambré
Magn. Reson. Discuss., https://doi.org/10.5194/mr-2024-11, https://doi.org/10.5194/mr-2024-11, 2024
Revised manuscript not accepted
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Demonstration of an ultra-compact spectrometer for electrically-detected magnetic resonance on a chip (EDMRoC) of silicon carbide MOSFETs with comparable signal-to-noise ratio as state-of-the-art conventional resonator-based EDMR. The relatively low cost, high sensitivity and limited space requirements of the EDMRoC configuration holds promise for application in basic and applied research as well as in industrial environments.
Qing Yang, Jianyu Zhao, Frederik Dreyer, Daniel Krüger, and Jens Anders
Magn. Reson., 3, 77–90, https://doi.org/10.5194/mr-3-77-2022, https://doi.org/10.5194/mr-3-77-2022, 2022
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We have presented a CMOS-based NMR platform featuring arbitrary phase control and coherent detection in a non-zero intermediate frequency (IF) receiver architecture as well as active automatic temperature compensation. The proposed platform is centered around a custom-designed NMR-on-a-chip transceiver. The entire system achieves a phase stability well below 1° in consecutive pulse acquire experiments and keeps a normalized standard deviation in the measured T2 values of 0.45 % over 100 min.
Silvio Künstner, Anh Chu, Klaus-Peter Dinse, Alexander Schnegg, Joseph E. McPeak, Boris Naydenov, Jens Anders, and Klaus Lips
Magn. Reson., 2, 673–687, https://doi.org/10.5194/mr-2-673-2021, https://doi.org/10.5194/mr-2-673-2021, 2021
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Electron paramagnetic resonance (EPR) spectroscopy is the method of choice to investigate and quantify paramagnetic species. We present the application of an unconventional EPR detection method, rapid-scan EPR, to enhance the sensitivity on an improved design of a miniaturized EPR spectrometer implemented on a silicon microchip. Due to its size, it may be integrated into complex and harsh sample environments, enabling in situ or operando EPR measurements that have previously been inaccessible.
Bernhard Blümich and Jens Anders
Magn. Reson., 2, 149–160, https://doi.org/10.5194/mr-2-149-2021, https://doi.org/10.5194/mr-2-149-2021, 2021
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The NMR-MOUSE is a magnetic resonance tool for non-destructive materials testing inside a laboratory. The history and use of this sensor are reviewed with attention to issues encountered when employed outside. Improvements are outlined to facilitate outdoor measurements.
Related subject area
Field: EPR | Topic: Instrumentation
Design and performance of an oversized-sample 35 GHz EPR resonator with an elevated Q value
Rapid-scan electron paramagnetic resonance using an EPR-on-a-Chip sensor
Hyperfine spectroscopy in a quantum-limited spectrometer
Jörg Wolfgang Anselm Fischer, Julian Stropp, René Tschaggelar, Oliver Oberhänsli, Nicholas Alaniva, Mariko Inoue, Kazushi Mashima, Alexander Benjamin Barnes, Gunnar Jeschke, and Daniel Klose
Magn. Reson., 5, 143–152, https://doi.org/10.5194/mr-5-143-2024, https://doi.org/10.5194/mr-5-143-2024, 2024
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We show the design, simulations, and experimental performance of a 35 GHz electron paramagnetic resonance (EPR) resonator based on a cylindrical cavity with 3 mm sample access. The design is robust; simple to manufacture and maintain; and, with its elevated Q value, well-suited to sensitive EPR experiments using continuous-wave or low-power pulsed excitation. Thus, we make multi-frequency EPR spectroscopy, a powerful approach to deconvolute overlapping paramagnetic species, more accessible.
Silvio Künstner, Anh Chu, Klaus-Peter Dinse, Alexander Schnegg, Joseph E. McPeak, Boris Naydenov, Jens Anders, and Klaus Lips
Magn. Reson., 2, 673–687, https://doi.org/10.5194/mr-2-673-2021, https://doi.org/10.5194/mr-2-673-2021, 2021
Short summary
Short summary
Electron paramagnetic resonance (EPR) spectroscopy is the method of choice to investigate and quantify paramagnetic species. We present the application of an unconventional EPR detection method, rapid-scan EPR, to enhance the sensitivity on an improved design of a miniaturized EPR spectrometer implemented on a silicon microchip. Due to its size, it may be integrated into complex and harsh sample environments, enabling in situ or operando EPR measurements that have previously been inaccessible.
Sebastian Probst, Gengli Zhang, Miloš Rančić, Vishal Ranjan, Marianne Le Dantec, Zhonghan Zhang, Bartolo Albanese, Andrin Doll, Ren Bao Liu, John Morton, Thierry Chanelière, Philippe Goldner, Denis Vion, Daniel Esteve, and Patrice Bertet
Magn. Reson., 1, 315–330, https://doi.org/10.5194/mr-1-315-2020, https://doi.org/10.5194/mr-1-315-2020, 2020
Short summary
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Electron spin detection was recently demonstrated using superconducting circuits and amplifiers at millikelvin temperatures, reaching the quantum limit of sensitivity. We use such a setup to measure electron-spin-echo envelope modulation on a small number of electron spins, in two model systems: bismuth donors in silicon and erbium ions doped in CaWO4 (calcium tungstate). Our results are a proof of principle that hyperfine spectroscopy is feasible with these quantum-limited ESR spectrometers.
Cited articles
Abhyankar, N., Agrawal, A., Shrestha, P., Maier, R., McMichael, R. D.,
Campbell, J., and Szalai, V.: Scalable microresonators for room-temperature
detection of electron spin resonance from dilute, sub-nanoliter volume
solids, Sci. Adv., 6, eabb0620, https://doi.org/10.1126/sciadv.abb0620, 2020. a
Anders, J.: Fully-integrated CMOS Probes for Magnetic Resonance
Applications, PhD thesis, EPFL, Lausanne, Switzerland, https://doi.org/10.5075/epfl-thesis-5154,
2011. a
Anders, J., Ortmanns, M., and Boero, G.: Frequency noise in current-starved
CMOS LC tank oscillators, Nonlinear Dynamics of Electronic Systems,
Proceedings of NDES 2012, 11–13 July 2012, Wolfenbuettel, Germany, 1–4, 2012c. a
Andreani, P., Wang, X., Vandi, L., and Fard, A.: A study of phase noise in
colpitts and LC-tank CMOS oscillators, IEEE J. Solid-St.
Circ., 40, 1107–1118, 2005. a
Azarkh, M., Singh, V., Oklre, O., Seemann, I. T., Dietrich, D. R., Hartig,
J. S., and Drescher, M.: Site-directed spin-labeling of nucleotides and the
use of in-cell EPR to determine long-range distances in a biologically
relevant environment, Nat. Protoc., 8, 131–147, 2013. a
Boero, G.: Integrated NMR Probe for Magnetometry, vol. 9 of Series in
Microsystems, Hartung-Gorre, Konstanz, Germany, 2000. a
Chauhan, S. K., Kumar, R., Nadanasabapathy, S., and Bawa, A.: Detection Methods for Irradiated Foods, Compr. Rev. Food Sci. F., 8, 4–16, https://doi.org/10.1111/j.1541-4337.2008.00063.x, 2009. a
Chu, A., Schlecker, B., Lips, K., Ortmanns, M., and Anders, J.: An 8-channel
13 GHz ESR-on-a-Chip injection-locked vco-array achieving 200 µM-concentration sensitivity, in: 2018 IEEE International Solid-State Circuits Conference (ISSCC), 11–15 February 2018, San Francisco, USA, 354–356, https://doi.org/10.1109/ISSCC.2018.8310330, 2018. a
Cristea, D., Wolfson, H., Ahmad, R., Twig, Y., Kuppusamy, P., and Blank, A.:
Compact electron spin resonance skin oximeter: Properties and initial
clinical results, MAGN. RESON. MED., 85, 2915–2925,
https://doi.org/10.1002/mrm.28595, 2021. a
Dayan, N., Ishay, Y., Artzi, Y., Cristea, D., Reijerse, E., Kuppusamy, P., and Blank, A.: Advanced surface resonators for electron spin resonance of single microcrystals, Rev. Sci. Instrum., 89, 124707, https://doi.org/10.1063/1.5063367, 2018. a
Demir, A.: Phase noise and timing jitter in oscillators with colored-noise
sources, IEEE T. Circuits-I, 49, 1782–1791, 2002. a
Elias, R. J., Andersen, M. L., Skibsted, L. H., and Waterhouse, A. L.:
Identification of Free Radical Intermediates in Oxidized Wine Using Electron
Paramagnetic Resonance Spin Trapping, J. Agri. Food Chem., 57, 4359–4365, https://doi.org/10.1021/jf8035484, pMID: 19358607, 2009. a, b
Fehr, M., Schnegg, A., Rech, B., Lips, K., Astakhov, O., Finger, F., Pfanner,
G., Freysoldt, C., Neugebauer, J., Bittl, R., and Teutloff, C.: Combined
multifrequency EPR and DFT study of dangling bonds in a-Si:H, Phys.
Rev. B, 84, 245203, https://doi.org/10.1103/PhysRevB.84.245203, 2011. a, b
Fehr, M., Schnegg, A., Rech, B., Lips, K., Astakhov, O., Finger, F., Freysoldt, C., Bittl, R., and Teutloff, C.: Dangling bonds in amorphous silicon investigated by multifrequency EPR, J. Non-Cryst. Solids, 358, 2067–2070, 2012. a
García-Martín, J., Gómez-Gil, J., and
Vázquez-Sánchez, E.: Non-Destructive Techniques Based on Eddy
Current Testing, Sensors, 11, 2525–2565, 2011. a
Gardiner, C. W.: Stochastic methods : a handbook for the natural and social
sciences, Springer series in synergetics, 4th edn., Springer, Berlin, Germany, 2009. a
Gualco, G., Anders, J., Sienkiewicz, A., Alberti, S., Forró, L., and Boero, G.: Cryogenic single-chip electron spin resonance detector, J.
Magn. Reson., 247, 96–103, 2014. a
Haag, S. F., Taskoparan, B., Darvin, M. E., Groth, N., Lademann, J., Sterry,
W., and Meinke, M. C.: Determination of the antioxidative capacity of the
skin in vivo using resonance Raman and electron paramagnetic resonance
spectroscopy, Exp. Dermatol., 20, 483–487,
https://doi.org/10.1111/j.1600-0625.2010.01246.x, 2011. a
Hajimiri, A. and Lee, T. H.: A general theory of phase noise in electrical
oscillators, IEEE J. Solid-St. Circ., 33, 179–194, 1998. a
Handwerker, J., Schlecker, B., Wachter, U., Radermacher, P., Ortmanns, M., and Anders, J.: A 14 GHz battery-operated point-of-care ESR spectrometer
based on a 0.13 µm CMOS ASIC, in: 2016 IEEE International Solid-State Circuits Conference (ISSCC), 31 January–4 February 2016, San Francisco, USA, 476–477, 2016. a, b, c, d, e, f, g
Jordan, D. W. and Smith, P.: Nonlinear ordinary differential equations ; an
introduction for scientists and engineers, 4th edn., Oxford University Press,
Oxford, UK, New York, USA, 2007. a
Kaertner, F. X.: Analysis of white and f-α noise in oscillators,
Int. J. Circ. Theor. App., 18, 485–519, 1990. a
Kiers, C. T., De Boer, J. L., Olthof, R., and Spek, A. L.: The crystal
structure of a 2,2-diphenyl-1-picrylhydrazyl (DPPH) modification, Acta
Crystallogr. B, 32, 2297–2305,
https://doi.org/10.1107/S0567740876007632, 1976. a
Kinget, P.: Amplitude detection inside CMOS LC oscillators, in: 2006 IEEE
International Symposium on Circuits and Systems, 21–24 May 2006, Kos, Greece, p. 4, 2006. a
Kopani, M., Celec, P., Danisovic, L., Michalka, P., and Biro, C.: Oxidative
stress and electron spin resonance, Clin. Chim. Acta, 364, 61–66, 2006. a
Matsumoto, N. and Itoh, N.: Measuring Number of Free Radicals and Evaluating
the Purity of Di(phenyl)-(2,4,6-trinitrophenyl)iminoazanium [DPPH] Reagents
by Effective Magnetic Moment Method, Anal. Sci., 34, 965–971,
https://doi.org/10.2116/analsci.18P120, 2018. a
Murphy, D., Rael, J. J., and Abidi, A. A.: Phase Noise in LC Oscillators: A
Phasor-Based Analysis of a General Result and of Loaded Q, IEEE
T. Circuits-I, 57, 1187–1203, 2010. a
Nallatamby, J. C., Prigent, M., Camiade, M., and Obregon, J.: Phase noise in
oscillators – Leeson formula revisited, IEEE T. Microw. Theory, 51, 1386–1394, 2003. a
Ottaviani, M. F., Spallaci, M., Cangiotti, M., Bacchiocca, M., and Ninfali, P.: Electron Paramagnetic Resonance Investigations of Free Radicals in Extra
Virgin Olive Oils, J. Agr. Food Chem., 49,
3691–3696, https://doi.org/10.1021/jf001203+, 2001. a, b
Qi, M., Gross, A., Jeschke, G., Godt, A., and Drescher, M.: Gd(III)-PyMTA
Label Is Suitable for In-Cell EPR, J. Am. Chem. Soc., 136, 15366–15378, 2014. a
Qin, P. Z. and Warncke, K.: Electron Paramagnetic Resonance Investigations of
Biological Systems by Using Spin Labels, Spin Probes, and Intrinsic Metal
Ions Part B, vol. 564 of Methods in Enzymology, Academic Press, London, UK, 2015. a
Romanyukha, A., Trompier, F., Reyes, R. A., Christensen, D. M., Iddins, C. J., and Sugarman, S. L.: Electron paramagnetic resonance radiation dose
assessment in fingernails of the victim exposed to high dose as result of an
accident, Radiat. Environ. Bioph., 53, 755–762,
https://doi.org/10.1007/s00411-014-0553-6, 2014. a
Sancho, S., Suarez, A., and Ramirez, F.: Phase and Amplitude Noise Analysis in Microwave Oscillators Using Nodal Harmonic Balance, IEEE T. Microw. Theory, 55, 1568–1583, https://doi.org/10.1109/TMTT.2007.900213, 2007. a
Schweiger, A. and Jeschke, G.: Principles of pulse electron paramagnetic
resonance, Oxford University Press, Oxford, UK, New York, USA, 2001. a
Thiessen, T. and Mathis, W.: On Noise Analysis of Oscillators Based on
Statistical Mechanics, International Journal of Electronics and
Telecommunications, 56, 357–366, 2010. a
Tseitlin, M., Rinard, G. A., Quine, R. W., Eaton, S. S., and Eaton, G. R.:
Rapid frequency scan EPR, J. Magn. Reson., 211, 156–161, 2011. a
Twahir, U. T., Stedwell, C. N., Lee, C. T., Richards, N. G. J., Polfer, N. C., and Angerhofer, A.: Observation of superoxide production during catalysis of Bacillus subtilis oxalate decarboxylase at pH 4, Free Radical Bio. Med., 80, 59–66, 2015. a
Twahir, U. T., Ozarowski, A., and Angerhofer, A.: Redox Cycling, pH
Dependence, and Ligand Effects of Mn(III) in Oxalate Decarboxylase from
Bacillus subtilis, Biochemistry, 55, 6505–6516, 2016. a
Twig, Y., Dikarov, E., and Blank, A.: Ultra miniature resonators for electron
spin resonance: Sensitivity analysis, design and construction methods, and
potential applications, Mol. Phys., 111, 2674–2682, 2013. a
Wang, H., Barton, R. J., Robertson, B. E., and Weil, J. A.: Structural studies of 2,2-Diphenyl-1-picrylhydrazine: A clathrate forming compound, J. Inclus. Phenom. Mol., 10, 203–217, https://doi.org/10.1007/BF01066204, 1991a. a
Wang, H., Barton, R. J., Robertson, B. E., Weil, J. A., and Brown, K. C.:
Crystal and molecular structures of two polymorphs of 2,2-di(p-nitrophenyl)-1-picrylhydrazine dichloromethane, C18H11N7O10 ⋅ CH2Cl2, Can. J. Chem., 69, 1306–1314,
https://doi.org/10.1139/v91-194, 1991b. a
Williams, D. E.: Crystal structure of 2,2-diphenyl-1-picrylhydrazyl free
radical, J. Am. Chem. Soc., 89, 4280–4287, https://doi.org/10.1021/ja00993a005, 1967. a
Wolfson, H., Ahmad, R., Twig, Y., Kuppusamy, P., and Blank, A.: A Miniature
Electron Spin Resonance Probehead for Transcutaneous Oxygen Monitoring,
Appl. Magn. Reson., 45, 955–967, https://doi.org/10.1007/s00723-014-0593-8,
2014. a
Zhang, L. and Niknejad, A. M.: An Ultrasensitive 14-GHz 1.12-mW EPR
Spectrometer in 28-nm CMOS, IEEE Microw. Wirel. Co.,
31, 819–822, https://doi.org/10.1109/LMWC.2021.3060730, 2021. a
Short summary
Novel electron spin resonance (ESR) detectors based on voltage-controlled oscillators (VCOs) have been attracting attention, mainly due to the possibility of integrating the whole ESR spectrometer onto a single printed circuit board at relatively low cost while maintaining a performance comparable to commercial solutions. We present an experimental setup where the signal is detected as a change in VCO oscillation amplitude, along with in-depth theoretical analysis of the novel readout scheme.
Novel electron spin resonance (ESR) detectors based on voltage-controlled oscillators (VCOs)...