X-Band Single Chip Integrated Pulsed Electron Spin Resonance Microsystem.

We report on the design and characterization of a single chip integrated pulsed electron spin resonance detector operating at 9.1 GHz. The microsystem consists of an excitation microcoil, a detection microcoil, a low noise microwave preamplifier, a mixer, and an intermediate frequency (IF) amplifier. The chip area is about 0.7 mm2. To exemplify its possible applications, we report the results of single pulse, Rabi nutation, Hahn echo, two echoes, Carr-Purcell, and inversion recovery echo experiments performed on 0.02 and 0.05 nL samples of α, γ-bisdiphenylene-ß-phenylallyl (BDPA) and 1% BDPA in polystyrene (BDPA:PS) at room temperature. The measured spin sensitivity is about 8 × 107 spins/Hz1/2 on a sensitive volume of about 0.1 nL. The microsystem power consumption is less than 100 mW, the radio frequency (RF) input bandwidth is 8.8 to 9.8 GHz, the IF output bandwidth is DC to 350 MHz, and the deadtime is less than 30 ns.

Single-Chip Dynamic Nuclear Polarization Microsystem.

Integration of the sensitivity-relevant electronics of nuclear magnetic resonance (NMR) and electron spin resonance (ESR) spectrometers on a single chip is a promising approach to improve the limit of detection, especially for samples in the nanoliter and subnanoliter range. Here, we demonstrate the cointegration on a single silicon chip of the front-end electronics of NMR and ESR detectors. The excitation/detection planar spiral microcoils of the NMR and ESR detectors are concentric and interrogate the same sample volume. This combination of sensors allows one to perform dynamic nuclear polarization (DNP) experiments using a single-chip-integrated microsystem having an area of about 2 mm2. In particular, we report 1H DNP-enhanced NMR experiments on liquid samples having a volume of about 1 nL performed at 10.7 GHz(ESR)/16 MHz(NMR). NMR enhancements as large as 50 are achieved on TEMPOL/H2O solutions at room temperature. The use of state-of-the-art submicrometer integrated circuit technologies should allow the future extension of the single-chip DNP microsystem approach proposed here up the THz(ESR)/GHz(NMR) region, corresponding to the strongest static magnetic fields currently available. Particularly interesting is the possibility to create arrays of such sensors for parallel DNP-enhanced NMR spectroscopy of nanoliter and subnanoliter samples.

200 GHz single chip microsystems for dynamic nuclear polarization enhanced NMR spectroscopy.

Dynamic nuclear polarization (DNP) is one of the most powerful and versatile hyperpolarization methods to enhance nuclear magnetic resonance (NMR) signals. A major drawback of DNP is the cost and complexity of the required microwave hardware, especially at high magnetic fields and low temperatures. To overcome this drawback and with the focus on the study of nanoliter and subnanoliter samples, this work demonstrates 200 GHz single chip DNP microsystems where the microwave excitation/detection are performed locally on chip without the need of external microwave generators and transmission lines. The single chip integrated microsystems consist of a single or an array of microwave oscillators operating at about 200 GHz for ESR excitation/detection and an RF receiver operating at about 300 MHz for NMR detection. This work demonstrates the possibility of using the single chip approach for the realization of probes for DNP studies at high frequency, high field, and low temperature.