Curtis Berlinguette


Research Classification

Combinatorial Chemistry

Research Interests

CO2 conversion and utilization
clean energy
advanced solar cells
electrochromic windows
dynamic windows
hydrogen fuels production
robotics and automation
machine learning / artificial intelligence

Relevant Degree Programs


Research Methodology

electrolyzer technologies
solar cell fabrication
transient spectroscopy


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Postdoctoral Fellows

Graduate Student Supervision

Doctoral Student Supervision

Dissertations completed in 2010 or later are listed below. Please note that there is a 6-12 month delay to add the latest dissertations.

Efficient, carbon-neutral hydrogenation using a palladium membrane reactor (2021)

Hydrogenation is a class of chemical manufacturing widely used for applications including fine chemicals, food, fertilizer, and fuels. Conventional thermochemical hydrogenation requires large amounts of hydrogen gas and heat derived from fossil fuel combustion to enable reaction. This process is highly carbon intensive. In this thesis, I present the electrocatalytic palladium membrane reactor (ePMR) as a technology that can reduce this carbon footprint by producing hydrogenated chemicals using water and renewable electricity. In this architecture, reactive hydrogen atoms are produced from water electrolysis on one side of a palladium membrane. These hydrogen atoms are then transported through the membrane to react with an unsaturated bond of a substrate on the other side. This technology eliminates the use of hydrogen gas and fossil fuels, and operates under ambient temperatures and pressures.In this thesis, I first demonstrate the utility of the ePMR to pair two organic reactions. Electrochemical synthesis generally forms a useful product at one electrode and a waste product at the other electrode. The palladium membrane acts as a physical barrier between the two electrodes, enabling optimized reaction conditions of two reactions simultaneously. I also investigate the effect of catalyst surface area, applied current, and electrolyte on reaction selectivity in the ePMR.I then focus on reducing the palladium content in an ePMR through a supported palladium membrane design. I show that a thin layer of palladium (20-fold reduction in palladium content compared to palladium foil membranes (25 μm) often used in the ePMR. The supported membrane design enables faster 1-hexyne hydrogenation rates than palladium foil and provides a strategy for designing cost-effective and potentially scalable membranes.Finally, I show that furfural (an important biomass derivative) can be hydrogenated into higher value products, furfuryl alcohol and tetrahydrofurfuryl alcohol at selectivities >84%. I also compare the ePMR to conventional electrochemical hydrogenation reactors. I find that furfural hydrogenation in the ePMR proceeds at higher selectivity, suppresses side product formation, and lowers operating voltages. This work presents an opportunity to decarbonize a >350,000 ton year-1 hydrogenation industry.

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Toward carbon-neutral hydrogenation using a palladium membrane reactor (2021)

The full abstract for this thesis is available in the body of the thesis, and will be available when the embargo expires.

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Electrocatalytic CO2 conversion in flow reactors (2020)

Electrochemical reduction of CO₂ to value-added liquid fuels and chemical feedstocks is a sustainable approach to off-peak electricity utilization. The propagation of a CO₂ value chain through capture-conversion technology is bottlenecked by a lack of systems capable of catalytic CO₂ conversion with the efficiency, selectivity, robustness, and economic viability relevant to industry. The design of a CO₂ electrolyzer that can operate at current densities (J) > 200 mA/cm² , Faradaic efficiencies (FE) > 85%, voltages 50%). I deploy a bipolar membrane which allows the use of non-corrosive conditions on either electrode, thereby prolonging cell lifetime.I then detail the design and use of an analytical device to compare the voltages for different CO₂ flow reactor architectures to identify which cell components should be optimized to most effectively lower the overall cell voltage. Analysis of the voltages across the components of three different flow reactor configurations highlights that the reactions at the anodes and cathodes are relatively efficient and that much of the voltage loss occurs at the membran. These results illuminate that a better understanding of membranes and the membrane-catalyst interface is needed.Finally, I demonstrate the incorporation of a molecular catalyst into a CO₂ flow reactor for efficient conversion of CO₂ to CO. Molecular catalysts are known to have high activity for the CO₂ reduction reaction but typically at low rates of conversion (i.e., 150 mA/cm² and FE > 85%).

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A palladium membrane reactor for organic transformations (2019)

Hydrogenation reactions are a widely-used class of catalytic transformations but the reactions require high-pressure H₂ gas and specialized equipment for safe handling. Hydrogenation with protons as a hydrogen source (electrocatalytic hydrogenation, ECH) overcomes this challenge but the substrate scope is limited to reactants that can be solubilized in protic conditions. In this thesis, a palladium membrane reactor is used to perform hydrogenation reactions with protons in any desired solvent. Palladium is semi-permeable for monoatomic, reduced hydrogen atoms so protons can be reduced at one side of the palladium, diffuse through the membrane and hydrogenate an unsaturated substrate on the other side of the palladium. The palladium membrane separates electrochemistry from hydrogenation, eliminating the solubility challenge of ECH. In this thesis, I first study hydrogen absorption into palladium. Hydrogen absorption is difficult to quantify because hydrogen is light and has minimal electron density. I demonstrate that coulometry can be an accurate technique to quantify hydrogen absorption when an electrochemical flow cell is used. The flow cell improves the selectivity of coulometry and enables quantification of absorbed hydrogen for a number of different palladium sample types. I then demonstrate the use of a palladium membrane reactor to pair two organic reactions together. Electrochemical reactions often form one product of value and one waste product. The palladium membrane acts as a dense barrier between the anode and cathode, enabling reaction of two organic substrates simultaneously. I also compare palladium membrane reactions to ECH reactions. I find that hydrogenation with a palladium membrane reactor increases reaction rates, changes the possible product distribution and lowers operating voltages. Finally, I study the use of the palladium membrane reactor for deuteration. Deuterated pharmaceuticals are of growing interest because of their increased half-lives. I find that the membrane reactor forms C–D bonds from an inexpensive and reusable D₂O starting material. The method has high site-selectivity and deuterium incorporations, and can be incorporated into a drug synthesis pathway.

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Driving chemistry at photoelectrodes and electrodes (2019)

Photoelectrochemical and electrochemical cells drive redox reactions by electricity with and without light, respectively. Water splitting is a widely-studied electrolytic reaction, where oxygen and hydrogen are produced at the anode and cathode, respectively. This technology, however, is limited by the relatively low value of products. The anodic production of oxygen usually requires a significantly higher electrical potential than the theoretical potential and actually holds very little economic value. The product of cathode reaction, hydrogen, may also be a poor target product because the hydrogen made by water electrolysis costs twice as much as the hydrogen extracted from fossil fuels in most markets. Therefore, a better selection of reactant and target product is required to make a value-added photoelectrochemical or electrochemical reaction.I show herein that the challenges for anode reaction in a photoelectrochemical cell can be overcomed by two strategies: lowering the amount of electricity required to produce oxygen; or simply driving alternative chemistry that forms products with higher value than oxygen. A bismuth vanadate (BiVO₄) photoanode is used to develop these two strategies. The photoelectrochemical activity of BiVO₄ is improved (i.e. a lower potential is required to drive water oxidation) by exposure to ultraviolet light radiation. I then use this BiVO₄ photoanode to drive alternative anodic reaction, organic oxidation, and generate organic products that are more valuable than oxygen. A variety of organic transformations are demonstrated on BiVO₄ photoanode, including alcohol oxidation, C-H oxidation and lignin decomposition.I also study an alternative cathode reaction, CO₂ reduction, to replace hydrogen evolution reaction. I demonstrate that pairing cathodic CO₂ reduction with anodic organic oxidation in a single electrochemical cell can make valuable carbon products on both electrodes. I also question a presupposition in many previous CO₂ reduction studies that CO₂ is the best (or even the only) carbon species for cathodic reduction. The direct reductions of bicarbonate and carbonate into CO are demonstrated in an electrochemical flow cell without CO₂ gas feed, which bypasses the energy-intensive step to first thermally extract CO₂ gas in carbon capture and utilization process and suggests bicarbonate/carbonate might be a better cathode reactant than CO₂.

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Photodeposited functional thin films (2019)

The conversion of electrical energy derived from clean, renewable, and intermittent sources such as wind and solar into transportable and storable fuels is a means of matching energy supply and demand. Effective electrocatalysts can facilitate these conversions in an economical manner. Our group has developed photodeposition techniques for synthesizing amorphous thin-film metal oxide electrocatalysts. The thicknesses of amorphous metal oxide films were determined by cross-sectional scanning electron microscopy (SEM) and X-ray fluorescence spectroscopy (XRF). XRF measurements recorded on the films provided a strong linear correlation with the thicknesses determined by cross-sectional SEM. The electrochemical surface area (ECSA) determined by double-layer capacitance measurements did not universally show a linear relationship with film thicknesses. These results highlight the limitations of using ECSA to determine electrocatalyst film thickness. The noninvasive XRF technique is demonstrated to be a superior method for reporting on the thickness and loadings of thin metal oxide films. XRF measurements were made on iron-nickel oxy/hydroxide (FeNiOx) films that are widely known to mediate the oxygen evolution reaction at modest current densities (10 mA cm-²). These measurements enabled the determination of the electrochemical stability and metal composition of these electrocatalyst films when subjected to sustained electrolysis in strong base at a current density J = 200 mA cm-². Most of the iron in the film was liberated during the first 24 h of electrolysis and deposited on the cathode. These results show that one must account for the instability of this mixed-metal composition when drawing structure-property relationships and when considering the scale-up of electrocatalysts.Finally, modifications to the photodeposition technique are demonstrated that enables access to metal and metal alloy thin films. Silver and copper are widely studied metals for catalyzing the CO₂ reduction reaction (CO₂RR), yet studies of Ag-Cu alloys are rare due to the immiscibility of the metals. I report that our photodeposition procedure provides access to Ag-Cu alloys at ambient pressures and temperatures. Our photodeposition procedure is shown to furnish metastable alloys with ~10 atomic weight % (at-%) copper incorporated into the silver lattice. These results provide proof that photodeposition can be used to access kinetic phases of alloys.

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The design of hole-transport materials to stabilize the performance of perovskite solar cells (2019)

Over six decades of photovoltaic research have led to the emergence of a highly efficient technology called perovskite solar cells (PSCs). Despite the recent sharp rise in power conversion efficiencies (PCEs) of this technology, PSCs have not yet been deployed at scale owing in part to the unsatisfactory stability of devices. The stability issues are due to the light absorbing layers being susceptible to dissolution and the hole-transport material (HTM) layers undergoing morphological changes under real life conditions. This dissertation seeks to suppress mechanisms of PSC degradation through the design of HTMs.I designed a series of five structurally similar HTMs to study the effect of triphenylamine (TPA) location and number on the thermal stability (i.e., glass transition temperature, Tg) of the HTM layer. My studies demonstrate that where the TPA units are positioned about a spiro-carbon core can shift the Tg upwards of 30 °C. I designed HTMs that can be electrochemically and thermally polymerized to yield an encapsulation layer for the PSC. I demonstrated that the polymerized HTM layer decreases film wettability and can be incorporated into a PSC device.I interrogated a series of three structurally analogous donor-acceptor (D-A) architectures (i.e., monopodal, bipodal and tripodal architectures) to determine the role of molecular structure on the hole mobility of HTMs. From these experiments, I learned that “monopodal” D-A architectures yielded the highest hole mobilities because of the low computed reorganization energy, small polaron stabilization energy and hole extraction potential associated with this HTM.Overall, I demonstrated three mechanisms to suppress either the degradation of the photoactive perovskite layer, the morphological changes to the HTM layer or the instability caused by additives in HTM films. I suggest future design principles to yield stable PSC devices towards the commercialization of this technology.

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Master's Student Supervision

Theses completed in 2010 or later are listed below. Please note that there is a 6-12 month delay to add the latest theses.

Design of anion exchange membranes for electrochemical carbon dioxide reduction to carbon monoxide (2021)

Electrochemical CO₂ reduction technologies provide a platform for transforming renewable electricity, water, and waste CO₂ into synthetic building blocks (e.g., CO) and chemicals. However, CO₂ electrolyzers are not yet available in the market due to poor efficiencies at high reaction rates. Emerging CO₂ electrolyzers containing an anion exchange membrane (AEM) offer promise in overcoming this challenge, but limited design principles exist for AEMs in CO₂ electrolysis application. This thesis reports on my investigation of the designs of AEMs that improve CO₂ electrolyzer performance for CO production.I first interrogate two analogous AEM designs to determine the effect of AEM functional group on product selectivity, cell voltage, and stability. This relationship between the membrane and CO₂ electrolyzer performance has not yet been established at reaction rates greater than 10 mA/cm². I demonstrate that an imidazolium-based AEM achieves a higher cell performance than a trimethylamine analog at reaction rates up to 100 mA/cm². I find that the low water uptake (i.e., water content) and improved chemical stability of an imidazolium group are contributing factors that lead to increased performance for CO production.I explore further how AEM water uptake and thickness, and cathode hydrophobicity impact the amount of water transported to the cathode. Water serves as a proton source for the CO₂ reduction reaction to CO, but excess water at the cathode (i.e., flooding) can block the pores of catalytic sites and impede mass transport of reactants and products. Theoretical simulations predict that flooding will occur at reaction rates greater than 750 mA/cm², but this thesis demonstrates that cathode flooding is an issue at merely 200 mA/cm². I find that thin, low water uptake AEMs paired with hydrophobic cathodes mitigate cathode flooding and improve product selectivity and cell voltage for CO production.

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Quantifying doping of hole-transport materials in solid-state solar cells (2021)

Solid-state dye-sensitized solar cells (ssDSSCs) convert renewable solar energy into electricity by separating electrons and holes. This function of charge separation is achieved by two fundamental layers: the hole transport material (HTM) and the electron transport layer (ETL). The poor stability and reproducibility of these layers is a current impediment to the commercialization of this technology. Doped-HTMs in particular suffer from poor reproducibility due to atmospheric conditions affecting doping, and in many cases, unnecessarily large amounts of dopants are added leading to reduced stability. These issues stem from a lack of a standardized protocol for HTM doping in lab-scale research.I developed a standard protocol to quantify the effective doping of HTMs to increase reproducibility and stability. I demonstrate this technique with state-of-the-art HTM 2,2′,7,7′-tetrakis[N,N-di(4-methoxyphenyl)amino]-9,9′-spirobifluorene (Spiro) and indirect oxidant lithium bis (trifluoromethylsulfonyl)imide (LiTFSI). This technique can be extended to quantify the effective doping of other HTM/dopant combinations which will enable optimized doping for ssDSSCs.I fabricated ssDSSCs with varied component composition, device architectures, and material deposition methods to understand the roles of different TiO₂ ETLs and their effects on power conversion efficiency (PCE). The PCE increased with the addition of a compact-TiO2 blocking layer which obstructs deleterious electron recombination pathways. Moreover, it was discovered that the use of TiO₂ clusters as an interlayer and the compact-TiO₂ have a synergistic improvement on PCE. Overall, I demonstrated the optimization of TiO₂ layers and quantified HTM oxidation to improve solid-state solar cell technologies. I suggest future experiments to develop our understanding of dopants and the necessary processing conditions to obtain stable high efficiency solid-state solar cells.

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High-temperature high-pressure calorimetry for studying thermochemical energy storage materials (2019)

Metal hydrides that can hydrogenate and dehydrogenate reversibly at high-temperature and high-pressure are considered candidate materials for thermochemical energy storage (TES). The thermodynamic and kinetic properties of these metal hydrides are poorly defined due to the limitation of the measurement techniques at high-temperature and high pressure. This thesis describes a custom-designed high-temperature and high-pressure calorimeter for studying gram-scale heterogeneous chemical reactions that expands the limits of TES research. Chapter 2 outlines the physical design and fabrication details of the calorimeter. The calorimeter was demonstrated operating up to at least 1232 °C while under pure hydrogen pressures up to 33 bar with simultaneous in-situ calorimetric and pressure measurements. A finite element analysis (FEA) model was constructed using COMSOL Multiphysics to aid the experimental design. Chapter 3 outlines a thermal analysis algorithm that is modelled with a lumped-element model. The chemical enthalpy can be estimated using this algorithm along with the power and temperature profile data from this calorimeter. The model was verified using an aluminum heat of fusion experiment, as well as an exothermic process simulation to obtain a fitting accuracy of over 99%. Chapter 4 summarizes this work and offers future directions of the research that can be conducted using this instrument.

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Cobalt tris(2,2'-bipyrimidine) redox mediators generate high dye-sensitized solar cell photovoltages (2018)

Dye-sensitized solar cells (DSSCs) are promising, cost-effective technologies used to harness solar energy for electricity. Previous efforts to improve the solar-to-electricity conversion efficiency have primarily focused on sensitizer engineering and photocurrent generation. Alternatively, the efficiency can be increased by tuning the redox potential of the charge mediator to maximize the photovoltage in the device. This work describes the implementation of a new cobalt mediator (Co-bpm) with an exceptionally positively shifted redox potential of 1.07 V vs NHE in the DSSC. The best-performing device showed one of the highest reported DSSC photovoltages. The poor solubility of Co-bpm in MeCN was a major obstacle that was overcome by testing a variety of electrolyte solvent systems and counterions. Notwithstanding, Co-bpm mediator-based devices exhibited low photocurrents and low power conversion efficiencies despite the high voltages.A comparative study was then performed to elucidate how the positively shifted redox potential affect the photocurrent in Co-bpm mediator-based devices. Three cobalt analogs [Co-(bpm-DTB), Co-bpy and Co-(bpy-DTB)] of varying redox potentials were studied alongside Co-bpm to determine the trend between redox potential, device performance, and recombination lifetime. The redox potentials of the cobalt analogs were tuned by installing tert-butyl substituents and varying the number of nitrogen atoms in the ligand. A positive shift in the redox potentials correlated to a linear increase in photovoltage and non-linear decrease in photocurrent in DSSCs. A low quasi-Fermi level (EF,n) at open-circuit conditions and a short electron lifetime (Tn) in device containing Co-bpm indicate that a significant loss of electrons from TiO₂ via recombination pathways is one key factor that contribute to the poor photocurrent and overall device performance.

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Interfacial Halogen Bonding Boosts the Photovoltage of the Dye-Sensitized Solar Cell (2016)

A series of donor-bridge-acceptor (D-π-A) compounds, differing only by the identity of two halogen atoms substituted on the triphenylamine (TPA, donor), were synthesized and characterized for insight into the regeneration reactions within dye-sensitized solar cells (DSSCs) [Dye-X⁺/TiO₂(e-) + I− → Dye-X/TiO₂ + I₂•−]. The structures of each series conformed to a molecular scaffold bearing a TPA donor, thiophene spacer, and acrylic acid unit as the anchoring group. In Chapter 2, each Dye-X (X = F, Cl, Br, and I) was immobilized on a TiO₂ surface to investigate how the halogen substituents affect the reaction rate between the light-induced charge-separated state, TiO₂(e−)/Dye-X⁺, with iodide in solution. Transient absorption spectroscopy showed progressively faster reactivity towards nucleophilic iodide with more polarizable halogen substituents: Dye-F
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Methods for Reducing the Capital Costs of Electrolyzers for Hydrogen Generation (2016)

Amorphous phases of metal oxide thin films are of interest to the Berlinguette group because they mediate the oxygen evolution reaction more efficiently than crystalline phases of the same compositions. One goal of this thesis is to develop a technique to implement amorphous metal oxide thin films in a membrane electrode assembly (MEA) by depositing these highly active thin films on solid polymer electrolyte membranes. Chapter 2 outlines the implementation of amorphous iridium oxide (a-IrOx) into a catalyst-coated membrane (CCM) to study amorphous thin film electrocatalysts in MEAs. Current densities of 10 mA cm-² were reached at relatively low overpotentials (~ 400 mV) for amorphous CCMs produced using the decal transfer method. This electrochemical response compares closely to that of amorphous iridium electrodeposited on conductive glass (10 mA cm-² at η = 430 mV). The second goal of this thesis is to lower the capital costs of alkaline electrolyzer units by using plastic as a surrogate for metal in field-flow plates. This achievement was demonstrated by electroplating nickel onto 3D-printed plastic flow-field plates. The test cells containing these metal-coated plastic components matched the performance of conventional metal components, despite containing 60-fold less metal. Chapter 4 summarizes this work and offers future directions of the research conducted for this thesis.

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Amorphous Electrocatalysts Formed by Near-Infrared-Driven Decomposition (2015)

The splitting of water into hydrogen and oxygen is widely viewed as the most sustainable option for storing energy produced by intermittent renewable energy sources such as solar or wind. Economically feasible large-scale deployment of this type of system requires the discovery of efficient electrocatalysts, particularly for the kinetically slow oxygen evolution reaction (OER). Transition metal oxides are the most durable and active water oxidation catalysts, and there is a growing body of evidence showing amorphous metal oxide films mediate the OER more efficiently than the crystalline phases of the same compositions. Notwithstanding, there is a limited set of fabrication methods available for making amorphous films, particularly in the absence of a conducting substrate. I introduce herein a scalable preparative method for accessing oxidized and reduced phases of amorphous films that involves the efficient decomposition of molecular precursors, including simple metal salts, by exposure to near-infrared (NIR) radiation. The NIR-driven decomposition process provides sufficient localized heating to trigger the liberation of the ligand from solution-deposited precursors on substrates, but insufficient thermal energy to form crystalline phases. This method provides access to state-of-the-art electrocatalyst films, as demonstrated herein for the electrolysis of water, and extends the scope of usable substrates to include non-conducting and temperature-sensitive platforms. Because crystalline ruthenium oxide is one of the most efficient electrocatalysts in acidic media, it would be highly advantageous to be able to readily access the amorphous phase of the material. I also document two facile preparation techniques for accessing amorphous ruthenium oxide, a state-of-the-art electrocatalyst. The formation of amorphous ruthenium oxide films is triggered by the decomposition of a film of spin-cast molecular ruthenium precursors on conducting glass by either ultraviolet (UV) and near infrared (NIR) light.

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Controlling Electron Transfer at Sensitized TiO? Surfaces (2015)

A series of three bis-tridentate ruthenium(II) complexes containing one cyclometalating ligand with terminal triphenylamine (TPA) substituents have been synthesized and characterized for insight into electron transfer reactions at TiO₂ surfaces. The structure of each complex conforms to a molecular scaffold formulated as [Ru(II)(TPA-2,5-thiophene-pbpy)(H₃tctpy)] (pbpy = 6-phenyl-2,2’-bipyridine; H₃tctpy = 4,4’,4”-tricarboxy-2,2’:6’,2”-terpyridine), where an electron-donating group (EDG) or an electron-withdrawing group (EWG) is installed about the anionic ring of the pbpy ligand and methyl groups surrounding the TPA-thiophene bridge. Modification of the anionic ring of the pbpy chelated with EDGs and EWGs enables the modulation of the Ru(III)/Ru(II) redox potential over 140 mV. This property offers the opportunity to turn on and off intramolecular hole transfer. Pulsed light laser excitation of the sensitized thin film resulted in rapid excited state injection and in some cases hole transfer to TPA [TiO₂(e⁻)/Ru(III)−TPA → TiO₂(e⁻)/Ru(II)−TPA・⁺. The rate constants for charge recombination of [TiO₂(e⁻)/Ru(III)−TPA → TiO₂/Ru(II)−TPA and TiO₂(e⁻)/Ru(II)−TPA・⁺ → TiO₂/Ru(II)−TPA] were drastically affected by modification of the bridging unit and can be modulated over 5.2 – 6.2×10⁵ s ⁻¹ and 1.7 – 5.1×10⁴ s⁻¹ respectively.

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