A broadband single-chip transceiver for multi-nuclear NMR probes

Grisi, Marco; Gualco, Gabriele; Boero, Giovanni

doi:10.1063/1.4916206

Cited by 55 publications

(37 citation statements)

References 29 publications

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“…With this approach, the B 1 amplitude could be reduced to an arbitrarily low value using an integrated variable attenuator. Furthermore, this approach would also allow for the implementation of pulsed mode single-chip ESR detectors, where the B 1 field could be pulsed using an integrated switch and the free induction decay or echo signal could be amplified and downconverted using an integrated microwave amplifier, a mixer, and an IF amplifier (an architecture already demonstrated for NMR spectroscopy at frequency below 1 GHz [58]). However, compared with the frequency detection, such a more conventional and versatile approach based on a signal amplitude detection requires more complex integrated circuitry and it might not necessarily allow to achieve better spin sensitivities at 10 GHz and above.…”

Section: Discussion and Outlookmentioning

confidence: 99%

Single-chip electron spin resonance detectors operating at 50 GHz, 92 GHz, and 146 GHz

Matheoud

Gualco

Jeong

et al. 2017

Journal of Magnetic Resonance

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We report on the design and characterization of single-chip electron spin resonance (ESR) detectors operating at 50GHz, 92GHz, and 146GHz. The core of the single-chip ESR detectors is an integrated LC-oscillator, formed by a single turn aluminum planar coil, a metal-oxide-metal capacitor, and two metal-oxide semiconductor field effect transistors used as negative resistance network. On the same chip, a second, nominally identical, LC-oscillator together with a mixer and an output buffer are also integrated. Thanks to the slightly asymmetric capacitance of the mixer inputs, a signal at a few hundreds of MHz is obtained at the output of the mixer. The mixer is used for frequency down-conversion, with the aim to obtain an output signal at a frequency easily manageable off-chip. The coil diameters are 120μm, 70μm, and 45μm for the U-band, W-band, and the D-band oscillators, respectively. The experimental frequency noises at 100kHz offset from the carrier are 90Hz/Hz, 300Hz/Hz, and 700Hz/Hz at 300K, respectively. The ESR spectra are obtained by measuring the frequency variations of the single-chip oscillators as a function of the applied magnetic field. The experimental spin sensitivities, as measured with a sample of α,γ-bisdiphenylene-β-phenylallyl (BDPA)/benzene complex, are 1×10spins/Hz, 4×10spins/Hz, 2×10spins/Hz at 300K, respectively. We also show the possibility to perform experiments up to 360GHz by means of the higher harmonics in the microwave field produced by the integrated single-chip LC-oscillators.

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Section: Discussion and Outlookmentioning

confidence: 99%

Single-chip electron spin resonance detectors operating at 50 GHz, 92 GHz, and 146 GHz

Matheoud

Gualco

Jeong

et al. 2017

Journal of Magnetic Resonance

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“…The electronic setup was identical to the one described in details in ref. 21. All experiments employing the single-chip probe were performed with a repetition time of 2 s, a π/2 pulse length of 2.5 μs, and an acquisition time of 400 ms.…”

Section: Methodsmentioning

confidence: 99%

“…( d ) Photographs of the integrated microchip and microcoil (details in Ref. 21). ( e ) Schematic representation of the single ovum probe in section view.…”

Section: Figurementioning

confidence: 99%

“…NMR spectroscopy of sub-nL biological samples is both a volume and concentration limited problem, setting severe constraints on the required spin sensitivity. Here we employ a recently developed single-chip integrated inductive NMR probe21 entirely realized with a commercially accessible complementary-metal-oxide-semiconductor (CMOS) technology, where the combination of a low noise transceiver and a multilayer microcoil allows for high spin sensitivities in sub-nL volumes (Fig. 1d).…”

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confidence: 99%

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NMR spectroscopy of single sub-nL ova with inductive ultra-compact single-chip probes

Grisi

Vincent

Volpe

et al. 2017

Sci Rep

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Nuclear magnetic resonance (NMR) spectroscopy enables non-invasive chemical studies of intact living matter. However, the use of NMR at the volume scale typical of microorganisms is hindered by sensitivity limitations, and experiments on single intact organisms have so far been limited to entities having volumes larger than 5 nL. Here we show NMR spectroscopy experiments conducted on single intact ova of 0.1 and 0.5 nL (i.e. 10 to 50 times smaller than previously achieved), thereby reaching the relevant volume scale where life development begins for a broad variety of organisms, humans included. Performing experiments with inductive ultra-compact (1 mm2) single-chip NMR probes, consisting of a low noise transceiver and a multilayer 150 μm planar microcoil, we demonstrate that the achieved limit of detection (about 5 pmol of 1H nuclei) is sufficient to detect endogenous compounds. Our findings suggest that single-chip probes are promising candidates to enable NMR-based study and selection of microscopic entities at biologically relevant volume scales.

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“…The electronic setup is noticeably similar to the one described in detail in Ref. [30]. In this realization, the RF sources, DAQ, and TTL pulses are generated by a modified Tecmag Scout console, whose GUI is used to manage the experimental parameters.…”

Section: Methodsmentioning

confidence: 99%

NMR microsystem for label-free characterization of 3D nanoliter microtissues

Grisi¹,

Conley²,

Rodriguez³

et al. 2020

Preprint

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11Performing chemical analysis at the nanoliter (nL) scale is of paramount importance for 12 medicine, drug development, toxicology, and research. Despite the numerous methodologies 13 available, a tool for obtaining chemical information non-invasively is still missing at this scale.14 Observer effects, sample destruction and complex preparatory procedures remain a necessary 15 compromise 1 . Among non-invasive spectroscopic techniques, one able to provide holistic and 16 highly resolved chemical information in-vivo is nuclear magnetic resonance (NMR) 2,3 . For its 17 renowned informative power and ability to foster discoveries and life-saving applications 4,5 , 18 efficient NMR at microscopic scales is highly sought after 6-10 , but so far technical limitations 19 could not match the stringent necessities of microbiology, such as biocompatible handling, ease 20 of use, and high throughput. Here we introduce a novel microsystem, which combines CMOS 21 technology with 3D microfabrication, enabling nL NMR as a platform tool for non-invasive 22 spectroscopy of organoids, 3D cell cultures, and early stage embryos. In this study we show its 23 application to microlivers models simulating non-alcoholic fatty liver disease (NAFLD), 24 demonstrating detection of lipid metabolism dynamics in a time frame of 14 days based on 117 25 measurements of single 3D human liver microtissues. 26 27 28 29Nuclear magnetic resonance (NMR) is a powerful spectroscopic tool for non-invasive 30 investigations of the chemistry in intact living matter 2,3 . In the last decades, NMR has been a 31 key enabler for several lifesaving diagnostic applications 4,5 as well as groundbreaking 32 fundamental research on animal and human bodies 11,12 . However, due to limitations of the 33 current commercial hardware, magnetic resonance cannot be routinely applied to in-vivo and 34 in-vitro studies at the nanoliter (nL) scale, typical of microorganisms and cell cultures. Indeed, 35 micro-NMR is a longstanding technical challenge, and numerous researchers have proposed 36 methods to achieve it, mainly using micro solenoids 6,7 , planar micro coils 8 , magic angle coil 37 spinning (MACS) probes at ultra-high fields 9 , reaching sample volume sizes of about 10 nL. 38More recently, NMR spectroscopy of eggs of microorganisms having a volume of just 0.1 nL 39 was reported in a relatively weak field strength of 7 T. Such advancement was possible thanks 40 to a novel approach based on complementary metal-oxide semiconductor (CMOS) microchips 41 that delivered high sensitivity, robustness, and a local and easily accessible sensing region 10 . 42All these works pushed NMR to the nL range, but sample handling issues and a high level of 43 complexity remained an obstacle to high throughput studies with sufficient statistics, essential 44 for biology, preventing widespread adoption. In this work we present an innovative device that 45 combines the advantages of CMOS-based NMR probes with an unprecedented ease of use, 46 allowing investigations of nL biological entit...

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A broadband single-chip transceiver for multi-nuclear NMR probes

Cited by 55 publications

References 29 publications

Single-chip electron spin resonance detectors operating at 50 GHz, 92 GHz, and 146 GHz

Single-chip electron spin resonance detectors operating at 50 GHz, 92 GHz, and 146 GHz

NMR spectroscopy of single sub-nL ova with inductive ultra-compact single-chip probes

NMR microsystem for label-free characterization of 3D nanoliter microtissues

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