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Investigating the effect of N-doping on carbon quantum dots structure, optical properties and metal ion screening | Scientific Reports – Nature.com

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Abstract

Carbon quantum dots (CQDs) derived from biomass, a suggested green approach for nanomaterial synthesis, often possess poor optical properties and have low photoluminescence quantum yield (PLQY). This study employed an environmentally friendly, cost-effective, continuous hydrothermal flow synthesis (CHFS) process to synthesise efficient nitrogen-doped carbon quantum dots (N-CQDs) from biomass precursors (glucose in the presence of ammonia). The concentrations of ammonia, as nitrogen dopant precursor, were varied to optimise the optical properties of CQDs. Optimised N-CQDs showed significant enhancement in fluorescence emission properties with a PLQY of 9.6% compared to pure glucose derived-CQDs (g-CQDs) without nitrogen doping which have PLQY of less than 1%. With stability over a pH range of pH 2 to pH 11, the N-CQDs showed excellent sensitivity as a nano-sensor for the highly toxic highly-pollutant chromium (VI), where efficient photoluminescence (PL) quenching was observed. The optimised nitrogen-doping process demonstrated effective and efficient tuning of the overall electronic structure of the N-CQDs resulting in enhanced optical properties and performance as a nano-sensor.

Introduction

The demand for high-performance carbon quantum dots (CQDs) with a range of applications, including sensing has been steadily increasing. However, the synthesis of CQDs continues to face challenges including high costs, lengthy multistep processes, and the use of hazardous substances1,2. Recently, biomass-derived CQDs have attracted considerable attention, and are considered as an optimal and green approach to prepare efficient CQDs. Biomass and biomass waste (agriculture product, agricultural residue, municipal solid waste etc.) are abundant, high in carbon content (45–55%), and are an environmentally friendly renewable resource3. Therefore, the utilisation of biomass as carbon resources for nanomaterial synthesis is an eco-friendly process and expected to reduce the total synthetic cost4. Although a broad range of biomass materials have been employed in producing CQDs, generally, these synthetic routes faced problems associated with poor control of the CQDs particle size, quality, and homogeneity of the product5. In addition, the CQDs synthesised from biomass or biomass waste, commonly possess poor optical properties and a low PLQY. The doping of heteroatom such as (N, P, S) is one of the most common methods to improve the optical properties of biomass-derived CQDs6,7. However, the questions related to the origin of the optical improvement with optimised dosing of these heteroatoms still need to be answered. Furthermore, in most conventional methodologies, these doping processes result in a longer synthesis time and higher energy consumption8.

In this work, the continuous hydrothermal flow synthesis (CHFS) which is primarily water-based was employed; thus, it is considered the greenest and most promising synthesis method for making CQDs. Notably, the CHFS allows designing or tailoring of the nanoparticles for specific functions based on the nucleation and surface functional processes. The comparison between CHFS and the traditional hydrothermal process revealed that the CHFS consumed less energy and time, while producing a highly homogenous quality product9. Moreover, the continuous hydrothermal process can be employed in multi-purposes such as controlling the nucleation to control the particle size and the addition of surfactant coating or dopant without further post-treatments10. In this paper, we report the use of CHFS process, to successfully synthesise N-doped carbon quantum dots (N-CQDs) from glucose which is an abundant, readily available, cost-effective biomass carbon source; and ammonia is used as a nitrogen dopant. Synthesised N-CQDs with different concentrations of ammonia were used to explore the effect of the concentration of nitrogen dopant on the optical characteristics of CQDs. A range of characterisation techniques were employed to investigate the origin of the optical enhancement. The performance of the N-CQDs as chemical nanosensor was tested. Currently clean water resources are foremost among global challenges facing society today. A significant proportion of the worlds wastewater containing heavy metals as pollutants  is disposed untreated in to the environment11. Therefore, the application of the prepared N-CQDs as chemical sensor to detect chromium (VI) which is carcinogenic, hemotoxic, and genotoxic; the main source being industrial waste water, would be timely.

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Experimental work

Chemicals

Glucose, ammonia (32%), potassium chromate, and potassium dichromate were purchased from Fisher Scientific. The solutions of metal ions used for the sensing application experiments were prepared using nitrate (Ag+, Ce3+, Co2+, Cr3+, Ni2+, Fe3+), sulphate (Cu2+ and Fe2+), chloride (K+, Na+, Mg2+) and sodium (CrO42−, Cr2O72−, NO3, CH3COO, HCOO, SO42−, F, Cl, Br, I). These chemicals were purchased from Sigma-Aldrich and were used as received. 15 MΩ deionized H2O (ELGA Purelab) was used for all the experiments.

Equipment

UV–Vis spectrophotometry: Shimadzu UV-1800 was used to perform the absorption measurements (λ = 200 to 800 nm) using a quartz cuvette (10 mm).

Photoluminescence (PL) spectroscopy: The steady-state fluorescence spectra of NCQDs were measured with Shimadzu RF-6000 spectrofluorophotometer.

High-resolution transmission electron microscopy (HRTEM): NCQDs were diluted in isopropanol and applied onto a carbon holey mesh grid (Agar) and allowed to air dry. The samples were then imaged using JEM 2100 (Jeol, Japan) at an acceleration voltage of 200 kV and at a range of magnifications between 15 and 500 K. Representatives NCQDs samples (g-CQDs, N-0.25, N-1, N-5 and N-10) were imaged and analysed.

Fourier–transform infrared (FTIR) spectra was recorded using an IR Affinity-1S Fourier transform infrared spectrometer instrument.

Raman spectra of the prepared N-CQDs was measured with a Horiba LabRAM HR Evolution spectrometer with radiation at 633 nm.

An Edinburgh Instruments FLS1000 photoluminescence spectrometer was used to measure the PL lifetime and the PLQY of the samples. The lifetime was measured using a 375 nm pulsed laser, and the data was fitted with 3-exponentials after reconvolution with instrument response function. The absolute quantum yield (QYabs) of the samples were investigated by using integrating sphere accessory with a standard method. Then, the true fluorescence quantum yield (QYtrue) is calculated by using the Eq. (1) where a is the fraction of the re-absorbed area.

$$mathrmQY^mathrmtrue=fracmathrmQY^mathrmabs1-mathrma+mathrma.fracmathrmQY^mathrmabs100$$
(1)

X-ray photoelectron spectroscopy (XPS): an AXIS Ultra DLD (Kratos Surface Analysis) setup equipped with a 180° hemispherical analyser, using Al Kα1 (1486.74 eV) radiation produced by a mono-chromicized X-ray source at operating power of 300 W (15 kV × 20 mA), with spot size of 0.7 mm was used to record the XPS spectra. The partial charge compensation was achieved by using a flood gun operating at 1.52 A filament current, 2.73 V charge balance, and 1.02 V filament bias. The vacuum in the analysis chamber was at least 1 × 10−8 mbar.

Synthetic methodology

Continuous hydrothermal flow synthesis (CHFS) was employed to synthesize N-CQDs (Supplementary Fig. 1). The process consists of three feedstock streams; (i) glucose (with a concentration of 70 mg mL−1) which was used as carbon source, (ii) ammonia with varied concentrations from 0.25 M up to 10.0 M was used as an N-dopant, and (iii) supercritical water which is the key parameter of this reaction. Firstly, the deionized water (with the flow rate 20 mL min−1) was heated up to 450 °C, and the pressure was kept at 24.8 MPa by using a back-pressure regulator (BPR) during the experiment (this condition is previously reported by our group as the optimised environment for the CQDs synthesis)10. The reaction was conducted by injecting the two precursors into the engineered mixer labelled as the “Reactor” (Fig. S1). Here, the precursors were mixed with supercritical water, and the nano dots were produced (in fraction of seconds). The residence time (~ 1.8 s) of the reaction was controlled by the flow rate of the precursors; both glucose and ammonia were pumped at the same time into the reactor with 5 mL min−1 flow rate. The reaction mixture travelled through a cooler to the BPR, and was collected for further treatments. The obtained solutions from the CHFS reaction mixtures were filtered using a 0.2 µm alumina membrane; subsequently, the solutions were continuously dialysed using a 30 kDa membrane in a tangential filtration unit. The cleaned solutions were freeze-dried, and the obtained average yield was 10.68 mg ml−1.

The CQDs samples synthesised from [glucose] = 70 mg mL−1 and ammonia with varied concentrations (0.25 M, 0.5 M, 0. 75 M, 1.0 M, 2.5 M, 5.0 M, 7.5 M and 10.0 M), were denoted as N-0.25, N-0.5, N-0.75, N-1, N-2.5, N-5, N-7.5, and N-10, respectively; g-CQDs was synthesised from the same source (glucose) but without nitrogen doping. The fluorescent photographs of the samples are shown in Fig. S2.

pH stability testing

The solutions with pH ranging from 1 to 13 were prepared using varying concentrations of NaOH (initial concentration 1.0 M) and HCl (1.0 M) solutions which were then diluted to the required pH. A dilute solution of N-CQDs (optical density, OD = 0.1) in deionised water was prepared. Following that, 100 μL of this diluted N-CQDs solution was added to a 3000 μL of each solution prepared at thedesired pH level (range 1–13). A pH meter was used to measure the corresponding pH values. The fluorescence spectra of these solutions were recorded using a Shimadzu RF-6000 Spectro fluorophotometer.

Chromium (VI) ion-sensing experiments

The detection of Cr (VI) ion experiment was conducted with various metal ions (as reported above), each prepared with a concentration of 50 ppm. In a typical experiment, 100 μL, N-CQDs (0.1 OD) was added to the 3.0 mL aqueous metal ion solution. The fluorescence spectrum of mixture solutions was measured using a Shimadzu RF-6000 Spectro fluorophotometermeas. The fluorescence lifetime was investigated to achieve a deeper understanding of the quenching mechanism using an Edinburgh Instruments FLS1000 spectrophotometer.

Limits of detection (LOD) and limits of quantification (LOQ)

The sensitivity of the N-CQDs sensor for Cr (VI) was investigated by evaluating their LOD and LOQ. For that, Cr (VI) ion solutions with various concentrations of 300 ppm, 200 ppm, 100 ppm, 50 ppm, 30 ppm, 10 ppm, 5 ppm, 2 ppm, 1 ppm and 0.5 ppm were first prepared. Then, 100 μL of N-CQDs were added to 3.0 mL of the prepared Cr (VI) ion solutions. The fluorescence spectra were recorded to estimate the LOD and LOQ by using Stem-Volmer graphs, LOD = 3σ/Ksv, LOQ = 10σ/Ksv, where Ksv is the slope of the graph, and σ is the error of the intercept.

Results and discussion

HRTEM images of N-CQDs (representative N-0.25 sample) show that the as-synthesized N-CQDs are spherical (Fig. 1a,c) with particle size ranging from 1.78 to 6.50 nm. The Gaussian distribution (Fig. 1b) of a sample of 150 particles shows the mean particle size of 4.60 ± 0.87 nm. In addition, the N-CQDs possess a crystalline structure as indicated by graphite lattice d-spacing of 0.22 nm (Fig. 1d). Similar features were also observed for the other samples g-CQDs, N-1, N-5 and N-10 analysed via TEM (Fig. S3).

Figure 1

HRTEM images of N-CQDs at different magnification and scale: (a) 20 nm, (c) 10 nm, (b) particle size Gaussian distribution histogram, (d) graphitic core lattice. The N-CQDs have commonly a particle size of 4.60 ± 0.87 nm.

To determine the nature of the functionalisation, the synthesised N-CQDs were investigated using the Fourier transform infrared (FTIR) spectroscopy. The samples were classified into two groups:(i) N-CQDs with a lower concentration of ammonia (from N-0.25 to N-1) and (ii) with a higher concentration of ammonia (from N-2.5 to N-10). The FTIR spectra (Fig. 2) showed that all N-CQDs have hydrophilic groups on their surface such as O–H (hydroxyl) corresponding to the peak at 3389 cm−1 and N–H (3263 cm−1), thus confirming their good solubility in the water. In addition, vibrations of C–H (2950 cm−1), C=O (1581 cm−1), C–N (1435 cm−1) and C–O (1080 cm−1) bonds were also observed in each sample13,14,15. The comparison of the FTIR spectra (Fig. S4) of the samples showed that increasing N-doping (ammonia concentration, from N-0.25 to N-1) displayed a diminishing stretch in vibration for C–O bond at 1080 cm−1. While the group of samples with a higher concentration of ammonia (N-2.5 to N-10) showed a sharp vibration of C–N bond at 1435 cm−1.

Figure 2
figure 2

FTIR spectra of N-CQDs with a lower concentration of ammonia (from N-0.25) and higher concentration of ammonia (N-10).

To achieve a deeper understanding of the surface characterisation of the N-CQDs and also to investigate the chemical composition of N-CQDs, X-ray photoelectron spectroscopy (XPS) was employed. The resultant XPS spectra shown in Fig. 3 were deconvoluted using Voigt functions (Lorentzian and Gaussian widths) with a distinct inelastic background for each component16. A minimum number of components is used to obtain a convenient fit. The binding energy scale was calibrated to the C 1s standard value of 284.6 eV. The atomic composition has been determined by using the integral areas provided by the deconvolution procedure normalized at the atomic sensitivity factor (Table S1). The XPS spectrum of the N-CQDs displays three typical peaks C1s (285.0 eV), N1s (399.0 eV), and O1s (531.0 eV). The fitted C1s spectrum was deconvoluted into four components, corresponding to carbon in form of C=C/C–C bonds (~ 284.4 eV), C–O/C–N (~ 285.8 eV), C=O (~ 287.3) and O=C–OH (~ 288.4 eV)17. Whilst, the N1s band showed three peaks after deconvolution which are 398.8 eV, 399.6 eV and 400.8 eV, representing pyridinic N, N–H and amide C–N, respectively18.

Figure 3
figure 3

Representative XPS spectra of N-CQDs showing the lowest (N-0.25) and highest (N-10) nitrogen doped samples. The spectra display three typical peaks C1s (285.0 eV), N1s (399.0 eV), and O1s (531.0 eV). The deconvoluted N1s band showed three peaks representing pyridinic N, N–H and amide C–N.

The content of each nitrogen doping species (pyridinic, pyrrolic and graphitic) are identified and quantified from the XPS spectra of NCQDs with the purpose of understanding their influence over the optical and chemical properties (Table S2). As commonly reported, the fluorescent property of CQDs can be enhanced by using nitrogen-doping. However, only the nitrogen bonded to carbon can improve the emission19. Also, a larger ratio of N/C was observed for N-CQDs samples synthesised with a higher concentration of ammonia (Table S1). The O1s region contains three peaks at 530.9 eV, 532.2 eV and 533.3 eV for C–OH/C–O–C, C=O, H–O–H, respectively20. In addition, the oxygen content is also a key parameter in the N-CQDs emission as it can maintain the balance between sp2 and sp3-carbon atoms21. Therefore, Raman spectroscopy was employed to investigate the disorder in the carbon bonding arrangement of N-CQDs.

The Raman spectra (Fig. S5) of the N-CQDs exhibited typical graphitic features consisting of the D mode (at 1368 cm−1) related to symmetry transformation by the defects, and the G band (at 1586 cm−1), which is assigned to the graphitic core sp2 (graphite-like) bonds. This is not surprising as the HRTEM images of N-CQDs showed a typical lattice spacing of graphite (see Fig. 1d). When comparing the Raman spectra between N-CQDs, at first glance, those spectra look similar, a common ratio ID/IG of 0.95 revealed a balance between the sp2 and sp3 bonds in the N-CQDs structure. This is different from g-CQDs where an ID/IG ratio of 0.83 was observed and assigned to the carbon core (sp2 bonds)10. This is probably attributed to the changes introduced by the nitrogen doping resulting in the transformation of C–C (sp2 bonds) into the sp3 bonding between N, O and C.

Optical properties of N-CQDs

The absorption spectra of the as-prepared N-CQDs measured using UV–Vis spectrophotometry are shown in Fig. 4. The N-CQDs samples have a strong peak around 265 nm and a shoulder around 295 nm (Fig. 4a). The 265 nm absorption peak is characteristics of π–π* transitions of the graphitic core (C=C or C–C) of sp2 domains present in the sp3 environment, and the 295 nm is attributed to n–π* (C=O) transitions and C–N/C=N bonds22,23. For comparison, the absorption spectrum of CQDs without nitrogen doping was also measured. It is noted that the absorption peaks related to N-CQDs are red-shifted compared to g-CQDs (synthesised from the same source glucose but without nitrogen doping), Fig. 4b. These transitions, are observed at 225 nm = π–π* (graphitic core), and 280 nm = n–π* transitions (C=O)10. Therefore, the absorption peak observed at 295 nm in the case of the N-CQDs is due to the formation of the C–N/C=N bonds related to the doping effect caused by the presence of graphitic nitrogen24,25.

Figure 4
figure 4

(a) UV–Vis absorption spectra of (a) N-CQDs and (b) g-CQDs without nitrogen doping. The presence of C–N/C=N bonds is observed at 295 nm.

The photoluminescence (PL) spectra of as-prepared N-CQDs were measured using a range of different excitation wavelengths as shown in Fig. 5. The PL emission of each sample clearly showed the excitation-dependent PL which is beneficial for a variety of applications such as biosensors, bio-images, or LED devices26,27. The PL emission peaks shifted when different excitation wavelengths were applied, and each sample exhibited an optimal excitation wavelength. Overall, the PL study revealed interesting optical properties of the N-CQDs. Firstly, the PL results are consistent with previous reports where the excitation dependent emission phenomenon of CQDs was observed28. Secondly, the maximum excitation wavelengths varied from 360 to 320 nm with the concentration of ammonia.

Figure 5
figure 5

Photoluminescence spectra of CQD with and without nitrogen doping measured using excitation wavelengths in the range of 300 to 500 nm, (a) g-CQDs (without nitrogen doping); (b) N-0.25; (c) N-2.5, (d) N-10.

However, the mechanisms behind the excitation dependent properties of CQDs is not clear. One of the most comprehensive and broadly accepted mechanism in interpreting the excitation-dependent PL of the CQDs is the quantum confinement effect also known as the size effect14,21,28,29. In general, the CQDs possess broad particle size distributions which leads to a range of different energy gaps and is the reason for the variation of emission wavelengths30,31. But herein, HRTEM image data analyses confirmed that the increased amount of nitrogen doping did not contribute to an increase in the particle size for the as prepared samples. Therefore, the observed red-shift character can be ascribed to the radiative recombination of e−h pairs hosted in the sp2 clusters32. Aside from the quantum confinement effect, surface states theory is rather broadly adopted to interpret the excitation-dependent PL behaviour of CQDs33,34,35. UV–Vis absorbance showed that the peak of the N-CQDs at 265 nm is related to the π–π* transition, which suggests the existence of a large number of π-electrons. The surface electronic states can conjugate with these π-electrons as a results of the surface oxidation which result in the modification of the electronic structure of the N-CQDs34,36.

To interpret the mechanism of this effect, the PL lifetime and PLQY of N-CQDs were measured. The obtained results (Table 1) showed an increase in both PL lifetime and PLQY upon nitrogen doping and the highest values of lifetime and PLQY were obtained for (left[Nright]ge 7.5 M). The obtained PLQY value of 9.6%(pm) 0.9 for N-10 is an significant improvement compared to g-CQDs which showed PLQY of < 1%10. These results are comparable to the literature (shown in Table S3), where CQDs and N-CQDs were synthesised via different methodologies.

Table 1 The photoluminescence quantum yield (PLQY), average lifetime, 1/e lifetime, radiative (kr) and non-radiative (knr) rates of N-CQDs.

The radiative rate (kr) and non-radiative rate (knr) were calculated by using the Eq. (2) and (3) 37.

$$k_r=fracPhi tau _1/e$$
(2)
$$Phi =frack_rk_r+k_nr$$
(3)

where (Phi) is PLQY of N-CQD and (tau _1/e) corresponds to the lifetime when fluorescence drops 1/e of its initial value.

Table 1 and Fig. 6 shows that when a higher concentration of ammonia was used, the non-radiative rates significantly reduced. This is due to surface coating activities of the nitrogen functional group which led to enhanced PLQY38. In addition, the lower non-radiative constant suggested that N-CQDs possess an efficient recombination process which led to an observation of nanosecond scale PL lifetime. These recombination processes suggested strong coupling of excited core states with the surface state. Thus confirming that the π-electron systems affect the surface electronic state leading to the modification of the overall electronic structure of N-CQDs36,39.

Figure 6
figure 6

(a) PLQY and non-radiative rate (GlU = g-CQDs), (b) PL lifetime of g-CQDs and N-CQDs. The analysis revealed an increase in both PL lifetime and PLQY upon nitrogen doping and the highest values of lifetime and PLQY were obtained for [N] ≥ 7.5 M.

The stability of CQDs for a broad pH range is essential for sensing applications. Therefore, PL of the N-CQDs in pH solution was measured to establish the relationship between the pH level and the emission intensity. N-CQDs showed fluorescence stability in a broad pH range from 2 to 11. For example, the fluorescence intensity of sample N-0.25 (Fig. 7a,b) was dramatically reduced by ~ 60% at pH  1, ~ 35% at pH  12 and ~ 40% at pH  13; and there were slight decreases at pH  11 (~ 12%).

Figure 7
figure 7

pH effect on the emission intensity of N-CQDs. Representative samples selected to show the highest and lowest [N] doping levels: (a,b) N-0.25, (c,d) N-10.

The diminishing fluorescent intensity behaviour of N-CQDs in strongly acidic and alkali media, noticeable also for samples with high content of nitrogen (for example, sample N-10, Fig. 7c,d). This can be related to protonation/deprotonation of the surface functional groups which causes surface charge disruption13. Whilst H-bonding is eliminated by deprotonation in basic conditions which can cause irregular energy levels resulting in the reduction of the N-CQDs fluorescence40. In addition, H+ can introduce surface defects on CQDs by breaking the passivated OH shell resulting in PL decreasing and a redshifted spectrum41. Indeed, as shown in Fig. 7c, a 20 nm red shift was also noted for the N-CQD in the strong acidic condition (pH  1). We have previously assigned this to the prominent emissions deriving from the graphitic core10.

Chromium (VI) ion-sensing

The N-CQDs were investigated for ion-sensing applications for a series of cations and anions (Fig. 8 and Fig. S6) including chromium (VI) ion (CrO42−/Cr2O72−) which is a major anthropogenic pollutant in industrial wastewater and soils11. The obtained results indicated that N-CQDs are highly sensitive and showed high selectivity towards hexavalent chromium in comparison to a series of other cations and anions.

Figure 8
figure 8

Selectivity of the N-CQDs based chemo-sensor.

To identify the sensitivity, limits of detection (LOD) and limits of quantification (LOQ) of N-CQDs were determined by measuring the fluorescent emission quenching as a function of Cr (VI) concentration (Fig. 9a). The reduction in emission intensity with the increase in concentrations of chromium was observed (Fig. 9b) i.e. there is a correlation between them. This correlation was fitted with a linear equation (y=mx+c), where slope m gives the value of quenching constant Ksv and c is the intercept. The LOD and LOQ were determined using the following equations: LOD = 3σ/Ksv, LOQ = 10σ/Ks, respectively, where σ is the standard error of the intercept. The plotted Stern–Volmer graph for N-10 in Fig. 9b was fitted with y = 0.0238x + 0.026 (R2 = 0.9999) which gave a quenching constant value of Ksv = 0. 0238 and intercept of 0.026. The LOD of 0.955 ppm and LOQ of 3.182 ppm were obtained with a standard error of the intercept of 0.0076. The calculated LOD and LOQ for all the samples are shown in Fig. 10. Our results showed a significant improvement compared to previously reported research10 where LOD of  3.62 ppm and LOQ of 11.6 ppm) were reported for g-CQDs. In addition, the obtained results are also comparable to other reported literature (Table S4).

Figure 9
figure 9

The effect of concentration in the PL intensity of N-10: (a) Stem–Volmer graphs as a function of (log(F0/F) versus Cr (VI) concentration (b).

Figure 10
figure 10

(a) Spectral overlap of the normalized UV–Vis absorption bands for the Cr (VI) ions (dash black) and the synthesised N-CQDs (green line), and the excitation spectrum (λem = 420 nm) (red line) and emission spectrum (λext = 340 nm) (blue line) of the N-CQDs. (b) LOD and LOQ of N-CQDs.

To understand the quenching mechanism, the change in PL lifetime of N-CQDs in various ion solutions were studied. The mechanism for this fluorescence quenching behaviour in the presence of Cr (VI) can be assigned to Inner Filter Effect (IFE) which is a physical phenomenon that occurs in a sensing system when the absorption spectrum of the absorber has an overlap with that of excitation and/or emission of the fluorescence leading to the reduced fluorescent emission intensity13. The IFE quenching is not related to the radiative and non-radiative transitions in the CQD, thus the intrinsic fluorescence emission is not changed in the presence of the quencher molecule42.

As illustrated in Fig. 10a, the N-CQDs excitation and emission bands (λex = 340 nm and λem = 420 nm) overlapped with the chromate (CrO42−) anions absorption bands at 372 nm. Moreover, CrO42− shows a second absorption band at 274 nm that also overlaps with the N-CQDs most intense absorption band at 265 nm. Further, the fluorescence lifetime of N-CQDs did not change with the addition of Cr (VI) (Fig. S7 and Table S5) which provides an evidence that the IFE is the mechanism for the fluorescence quenching phenomenon. There is a downtrend of N-CQDs in the LOD and LOQ results (Fig. 10b). The LOD decreased from 4.9 ppm for sample N-0.25 to 0.95 ppm for sample N-10, while the LOQ improved from 16.3 ppm to 3.18 ppm. These results revealed that nitrogen doping enhanced the fluorescent properties of CQDs resulting in higher PLQY which then leads to the improvement in LOD and LOQ and consequently the sensing performances.

Conclusions

In conclusion, efficient N-CDQs were synthesised using biomass precursors (glucose) and ammonia via the CHFS process. The synthesized N-CQDs possess excellent optical properties with a PLQY of ~ 10% and showed excellent pH stability (for pH 2 to 11). The synthesized N-CQDs were tested as a chemical sensor for Cr (VI) ion and the LOD value of 0.95 ppm and LOQ value of 3.18 nm were obtained. The fluorescence lifetime studies confirmed Inner Filter Effect (IFE) as the mechanism for the quenching behaviour of the nano-sensing. Hence, this work presented a novel, rapid, single-step and green approach for nanomaterials synthesis in general and carbon quantum dots in particular which then can be used for a range of different applications.

Data availability

The datasets used and/or analysed during the current study are available from the corresponding author on reasonable request. For the purpose of open access, the authors have applied a Creative Commons attribution (CC BY) licence to any author accepted manuscript version arising.

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Acknowledgements

SK, MTS, KGN and IAB would like to acknowledge LSBU for all the financial support provided in the completion of this research work. IAB and AN would like to acknowledge funding through the Core Program 21N/2019 and the Project ELI_17/2020 (granted by the Institute of Atomic Physics) of the National Institute of Materials Physics.

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K.N.G. carried out the experimental work; I.B.: Raman analysis; A.N.: XPS analysis; N.P.P.: facilitated access to TEM facilities, R.G.: TEM characterisation; S.T., A.R. and M.T.S. supported with TRPL analysis; S.K.: principal investigator; K.N.G, M.T.S. and S.K. wrote the paper. All authors reviewed the manuscript.

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Nguyen, K.G., Baragau, IA., Gromicova, R. et al. Investigating the effect of N-doping on carbon quantum dots structure, optical properties and metal ion screening.
Sci Rep 12, 13806 (2022). https://doi.org/10.1038/s41598-022-16893-x

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  • Published: 15 August 2022

  • DOI: https://doi.org/10.1038/s41598-022-16893-x

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The total solar eclipse in North America could shed light on a persistent puzzle about the sun – Phys.org

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The total solar eclipse in North America could shed light on a persistent puzzle about the sun

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The path of eclipse totality passes through Mexico, the US and Canada. Credit: NASA’s Scientific Visualization Studio

A total solar eclipse takes place on April 8 across North America. These events occur when the moon passes between the sun and Earth, completely blocking the sun’s face. This plunges observers into a darkness similar to dawn or dusk.

During the upcoming eclipse, the path of totality, where observers experience the darkest part of the moon’s shadow (the umbra), crosses Mexico, arcing north-east through Texas, the Midwest and briefly entering Canada before ending in Maine.

Total solar eclipses occur roughly every 18 months at some location on Earth. The last that crossed the US took place on August 21 2017.

An international team of scientists, led by Aberystwyth University, will be conducting experiments from near Dallas, at a location in the path of totality. The team consists of Ph.D. students and researchers from Aberystwyth University, Nasa Goddard Space Flight Center in Maryland, and Caltech (California Institute of Technology) in Pasadena.

There is valuable science to be done during eclipses that is comparable to or better than what we can achieve via space-based missions. Our experiments may also shed light on a longstanding puzzle about the outermost part of the sun’s atmosphere—its corona.

The sun’s intense light is blocked by the moon during a total solar eclipse. This means that we can observe the sun’s faint corona with incredible clarity, from distances very close to the sun, out to several solar radii. One radius is the distance equivalent to half the sun’s diameter, about 696,000km (432,000 miles).

Measuring the corona is extremely difficult without an eclipse. It requires a special telescope called a coronagraph that is designed to block out direct light from the sun. This allows fainter light from the corona to be resolved. The clarity of eclipse measurements surpasses even coronagraphs based in space.

We can also observe the corona on a relatively small budget, compared to, for example, spacecraft missions. A persistent puzzle about the corona is the observation that it is much hotter than the photosphere (the visible surface of the sun). As we move away from a hot object, the surrounding temperature should decrease, not increase. How the corona is heated to such high temperatures is one question we will investigate.

We have two main scientific instruments. The first of these is Cip (coronal imaging polarimeter). Cip is also the Welsh word for “glance,” or “quick look.” The instrument takes images of the sun’s corona with a polariser.

The light we want to measure from the corona is highly polarized, which means it is made up of waves that vibrate in a single geometric plane. A polarizer is a filter that lets light with a particular polarization pass through it, while blocking light with other polarizations.

The Cip images will allow us to measure fundamental properties of the corona, such as its density. It will also shed light on phenomena such as the solar wind. This is a stream of sub-atomic particles in the form of plasma—superheated matter—flowing continuously outward from the sun. Cip could help us identify sources in the sun’s atmosphere for certain solar wind streams.

Direct measurements of the magnetic field in the sun’s atmosphere are difficult. But the eclipse data should allow us to study its fine-scale structure and trace the field’s direction. We’ll be able to see how far magnetic structures called large “closed” magnetic loops extend from the sun. This in turn will give us information about large-scale magnetic conditions in the corona.

The second instrument is Chils (coronal high-resolution line spectrometer). It collects high-resolution spectra, where light is separated into its component colors. Here, we are looking for a particular spectral signature of iron emitted from the corona.

It comprises three , where light is emitted or absorbed in a narrow frequency range. These are each generated at a different range of temperatures (in the millions of degrees), so their relative brightness tells us about the coronal temperature in different regions.

Mapping the ‘s temperature informs advanced, computer-based models of its behavior. These models must include mechanisms for how the coronal plasma is heated to such high temperatures. Such mechanisms might include the conversion of magnetic waves to thermal plasma energy, for example. If we show that some regions are hotter than others, this can be replicated in models.

This year’s eclipse also occurs during a time of heightened solar activity, so we could observe a coronal mass ejection (CME). These are huge clouds of magnetized plasma that are ejected from the sun’s atmosphere into space. They can affect infrastructure near Earth, causing problems for vital satellites.

Many aspects of CMEs are poorly understood, including their early evolution near the sun. Spectral information on CMEs will allow us to gain information on their thermodynamics, and their velocity and expansion near the sun.

Our eclipse instruments have recently been proposed for a space mission called moon-enabled solar occultation mission (Mesom). The plan is to orbit the moon to gain more frequent and extended eclipse observations. It is being planned as a UK Space Agency mission involving several countries, but led by University College London, the University of Surrey and Aberystwyth University.

We will also have an advanced commercial 360-degree camera to collect video of the April 8 eclipse and the observing site. The video is valuable for public outreach events, where we highlight the work we do, and helps to generate public interest in our local star, the sun.

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Mar 30: An Australian Atlantis and other lost landscapes, and more… – CBC.ca

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Quirks and Quarks54:00An Australian Atlantis and other lost landscapes, and more…


On this week’s episode of Quirks & Quarks with Bob McDonald: 

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Archaeologists identify a medieval war-horse graveyard near Buckingham Palace 

Quirks and Quarks9:04Archaeologists identify a medieval war-horse graveyard near Buckingham Palace

We know knights in shining armour rode powerful horses, but remains of those horses are rare. Now, researchers studying equine remains from a site near Buckingham Palace have built a case, based on evidence from their bones, that these animals were likely used in jousting tournaments and battle. Archaeologist Katherine Kanne says the bone analysis also revealed a complex, continent-crossing medieval horse trading network that supplied the British elite with sturdy stallions. This paper was published in Science Advances.

University of Exeter researchers analyzed horse skeletons found near Buckingham Palace and conducted isotope tests on teeth to find out more about the animals’ origins. (University of Exeter)

In an ice-free Arctic, polar bears are dining on duck eggs — and gulls are taking advantage

Quirks and Quarks9:22In an ice-free Arctic, Polar bears are dining on duck eggs — and gulls are taking advantage

Researchers using drones to study ground-nesting birds in the Arctic have observed entire colonies being devastated by marauding polar bears that would normally be out on the ice hunting seals, except the ice isn’t there. What’s more, now they’re enabling a second predator — hungry gulls that raid the nests in the bears’ wake. Andrew Barnas made the observations of this “gull tornado” by following around polar bears in East Bay Island in Nunavut. The research was published in the journal Ecology and Evolution.

Aerial video of a polar bear on grassy, rocky terrain with white birds circling nearby.
A polar bear storms eider duck nests on East Bay island in Nunavut, while herring gulls follow closely behind to snack on any remaining eggs. (Submitted by Andrew Barnas)

A NASA mission might have the tools to detect life on Europa from space

Quirks and Quarks8:05A NASA mission might have the tools to detect life on Europa from space

NASA’s Europa Clipper mission, due to launch this fall, is set to explore the jewel of our solar system: Jupiter’s moon, Europa. The mission’s focus is to determine if the icy moon, thought to harbour an ocean with more water than all of the water on Earth, is amenable to life. However, postdoctoral researcher Fabian Klenner, now at the University of Washington, demonstrated how the spacecraft may be able to detect fragments of bacterial life in a single grain of ice ejected from the surface of the moon. The study was published in the journal Science Advances.

The silhouette of the spacecraft is flying over a brightly pink, blue and orange tinted moon with lots of darker coloured veins underneath with a slightly eclipsed Jupiter looming in the backdrop.
Scientists think under Europa’s icy shell, there is a global, saltwater ocean with twice the volume of Earth’s oceans combined. (NASA/Jet Propulsion Laboratory/Caltech)

Pollution is preventing pollinators from recognizing floral plants by scent

Quirks and Quarks7:50Pollution is preventing pollinators from finding plants by scent

Our polluted air is transforming floral scents so pollinators that spread their pollen can no longer recognize them. In a new study in the journal Science, researchers found that a certain compound in air pollution reacts with the flower’s scent molecules so pollinators — like the hummingbird hawk-moths that pollinate at night — fail to recognize them. Jeremy Chan, a postdoctoral researcher at the University of Naples, said the change in scent made the flowers smell “less fruity and less fresh.”

A huge insect that looks like a hummingbird hovers over a vibrant pink flower with its long antenna inside one of the blooms.
Scientists found that a hummingbird hawk-moth’s ability to recognize the smell of flowers is hampered by air pollution. (Thomas Kienzle/AFP/Getty Images)

An Australian Atlantis and underwater archeological remains in the Baltic 

Quirks and Quarks17:14An Australian Atlantis and underwater archeological remains in the Baltic

During the last ice age, sea levels were more than 100 metres lower than they are today, which means vast tracts of what are currently coastal seafloor were dry land back then. Geologists and archaeologists are searching for these lost landscapes to identify places prehistoric humans might have occupied. These included a country-sized area of Australia that could have been home to half a million people. Archaeologist Kasih Norman and her colleagues published their study of this now-drowned landscape in Quaternary Science Reviews

Another example is an undersea wall off the coast of Northern Germany that preserves an underwater reindeer hunting ground, described in research led by Jacob Geersen, published in the journal PNAS.

a black-and-white depiction of a small group of caribou walking between a low stone wall and an ocean coastline.
An artist’s representation of caribou being directed by a hunters’ stone wall, as it would have appeared 8-11,000 years ago, before rising sea levels left it 20m below the surface of the Baltic Sea. (Michał Grabowski)

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Solar eclipse April 8 – South Grey News

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March 28, 2024

Graphic: Appalachian Mtn Club

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Grey Bruce Public Health is urging residents to resist the temptation to look directly at the sun during the upcoming solar eclipse and take steps to safeguard their visual health during this relatively rare celestial event.

On April 8, 2024, parts of southern and eastern Ontario will experience a total solar eclipse for the first time since 1925. Grey-Bruce will be outside of the so-called Path of Totality — a narrow area where the moon will completely block out the sun — but will still experience a partial eclipse.

The eclipse is expected to begin at about 2 pm and continue until 4:30 pm The eclipse will peak around 3:20 pm.

It is never safe to stare directly at the sun, but it may be tempting to do so during a solar eclipse.

Looking directly at the sun during an eclipse can cause retinal burns, blurred vision, and/or temporary or permanent loss of visual function, according to the Ontario Association of Optometrists. Damage to the eyes can occur without any sensation of pain.

Grey Bruce Public Health advises the following:

  • Do not look directly at the sun without proper eye protection during the solar eclipse. Looking at even a small sliver of the sun before or after the eclipse without proper eye protection can harm vision.
  • Keep a close eye on children and other vulnerable family members during the eclipse to ensure they do not inadvertently look up at the sun without proper eye protection.
  • To safely view the eclipse, ISO-certified eclipse glasses that meet the ISO 12312-2 international safety standard must be worn. Ensure these glasses are in good condition, without any wrinkles or scratches, and that they fully cover the entire field of vision. Put on the glasses when looking away from the sun, then look at the eclipse. Look away from the sun before taking the glasses off.
  • Regular sunglasses or homemade filters will not protect the eyes.
  • It is not safe to view the eclipse through a camera/phone lens, telescope, binoculars, or any other optical device.

Other ways to safely experience the solar eclipse include watching a livestream of the event or creating and using an eclipse box or pinhole projector.

Anyone experiencing temporary vision loss or blurred vision during or after the eclipse should speak with their eye care professional or healthcare provider as soon as possible.

Anyone experiencing blindness (immediate or delayed) after viewing the eclipse must seek emergency care immediately.

More information on the upcoming eclipse is available on the GBPH website.


At South Grey News, we endeavour to bring you truthful and factual, up-to-date local community news in a quick and easy-to-digest format that’s free of political bias. We believe this service is more important today than ever before, as social media has given rise to misinformation, largely unchecked by big corporations who put profits ahead of their responsibilities.

South Grey News does not have the resources of a big corporation. We are a small, locally owned-and-operated organization. Research, analysis and physical attendance at public meetings and community events requires considerable effort. But contributions from readers and advertisers, however big or small, go a long way to helping us deliver positive, open and honest journalism for this community.

Please consider supporting South Grey News with a donation in lieu of a subscription fee and let us know that our efforts are appreciated. Thank you.

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