Bright green ﬂ uorescence of microwave irradiation-synthesized Cdots as sensitive probe of iron (III)

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Mater. Res. Express6(2019)105703 https://doi.org/10.1088/2053-1591/ab3680

PAPER

Bright green ﬂ uorescence of microwave irradiation-synthesized Cdots as sensitive probe of iron (III)

I W L Lewa¹, H Sutanto^1,2 , A Subagio¹, I Marhaendrajaya¹and H Sugito¹

1 Department of Physics, Diponegoro University, Jl. Prof. Soedarto, SH, Semarang-50275, Indonesia

2 Central Laboratory of Research and Services Diponegoro University(CORES DU), Jl. Prof. Soedarto, SH, Semarang-50275, Indonesia E-mail:herisutanto@ﬁsika.undip.ac.id

Keywords:Cdots, bio imaging, bright Greenﬂuorescence, microwave irradiation

Abstract

Carbon nanodots

(Cdots)

are very attractive materials due to their

ﬂuorescence and great potential in

various

ﬁelds. Oneﬁeld that still needs to be developed is heavy metal ion detector. In this study, a

simple and cost efﬁcient

ﬂuorescent detector of Fe³⁺

was built. This material was synthesized by microwave irradiation method using citric acid and urea with puriﬁed water as the solvent to get the optimal concentration of urea in order to produce bright green

ﬂuorescence. Synthesized Cdots with

optimal concentration of urea emit bright green

ﬂuorescence under UV light radiation. This bright

green

ﬂuorescence was then used to detect Fe³⁺

. The

ﬂuorescence of this solution was quenched with

the addition of Fe

³⁺

due to transfer charges and exciton recombination. Optical characterization was carried out using UV–vis spectrophotometer, and

ﬂuorescence spectrophotometer. Results showed

two absorption peaks on Cdots; at 330 nm and 410 nm. Fluorescence analysis was performed using a beam of 532 nm produced emission at a wavelength of 590 nm. In addition, structural characterization was performed using FTIR, SEM and EDX.

Introduction

Carbon nanodots(Cdots)are zero-dimensional carbon material with a dimension of less than 10 nm. Cdots werefirst discovered by Xuet alin 2004 from the purification process of carbon nanotubes[1]. Cdots are spherical[2], non toxic[3]and have high water solubility[4]. Cdots can be used in several application areas such as biomedicine[5], LED[6], energy related applications[7,8], bioimaging[9], and sensors[10]. Cdots are very interesting material with theirfluorescence properties[11]and one of thefields that is being developed using this is sensors. Cdots are the right material choice to replace the commonly used probes. Sensor applications typically use quantum dots semiconductor materials such as CdS[12]. However, CdS is toxic and is not easily degraded in the environment. Cdots are an alternative substitute material that are effective because they are not toxic, compatible, and easily soluble in water[12].

Cdots can be synthesized using several methods that are divided into two categories of top down and bottom up. The top down method breaks large molecules into smaller ones. This method includes laser ablation[13], electrochemistry[14]and arc discharge[15]. Meanwhile, the bottom up method, which is also known as the chemical method, is the preparation of a material from small-sized materials. This method includes pyrolysis [16], hydrothermal[17]and microwave[18]. Microwave irradiation is one of the most widely used methods because it can reach certain heat in shortly, efficiently, fast, easily, and inexpensively. Improving thefluorescence properties of this material is an important aspect that should be considered. Various methods can be used such for this purpose, including surface passivation[19]. Passivation process uses organic materials containing an amine group to improvefluorescence. Fluorescence is caused by a surface energy trap that can be modified to get the properties that are suitable for certain applications. Surface modification method is appropriate for sensing applications[20]. Based on research by Sun and coworkers, the surface passivation process of non-luminescent Cdots derived from polyethylene glycol polymers(PEG)shows strong luminescence[20]. By using microwave

RECEIVED

31 May 2019

REVISED

7 July 2019

ACCEPTED FOR PUBLICATION

29 July 2019

PUBLISHED

7 August 2019

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irradiation, the passivation process can be carried out in one step, hence, microwave irradiation is the right method to synthesize Cdots[21].

Previous studies have proven that Cdots can be used to detect heavy metals with the turn on/turn off fluorescence mechanism. One study by Zhanget alsynthesizes Cdots from melamine and g-C3N4by heating them for 2 h to detect Pb²⁺ions[22]. Another study by Kumaret alsynthesizes Cdots using the hydrothermal method for 7 h to detect Hg²⁺ions[23]. In this research, Cdots synthesis using microwave irradiation was carried out to obtain a material that has strong luminescence and can be used as a detector of Fe³⁺heavy metal ions. The precursors used here were citric acid as a source of carbon and urea as passivation agents and distilled water as solvent. Variations of urea concentration were made in order tofind the right formula to produce strong luminescence. Sensitivity tests for Fe³⁺heavy metal ions were also carried out. Further characterization includes using UV–vis spectrophotometer to observe absorbance spectrum,fluorescent spectrometer to observe emission spectrum of Cdots and FTIR to observe functional groups contained in the synthesized material.

Material and methods

A synthesis procedure for Cdots can be seen infigure1. Cdots were made of citric acid and urea using microwave irradiation method. Citric acid was used as a source of carbon, while urea was used as passivation agent with its amine group content. Purified water was used as solvent in the reaction. Two grams of citric acid were mixed with urea with varied concentration of 1 to 7 grams. The solvent for each solution was 60 ml of purified water.

Once the solution is homogenized, it was then irradiated using a microwave with power 450 W for 30 min until a blackish brown crust is formed. The crust was then taken and mashed into powder. Afterwards, the Cdots powder was dissolved in puriﬁed water with a concentration 100 ppm. This solution was then characterized and analyzed to determine its properties.

Results and discussion

Cdots synthesis

Theﬁrst step is synthesizing Cdots using microwave irradiation. The materials used were citric acid as a source of carbon and urea as a surface passivation agent. Physical processes occurring during synthesis are divides into 4 stages of dehydration, polymerization, carbonization and passivation²⁰. Dehydration reaction is the release of water content in the molecules that are reacting. The second step is polymerization. This is where reaction triggers spontaneous nucleation process that is followed by the formation of new longer bonds. The third step is carbonization in which inorganic carbon bonds are derived from citric acid²¹. Theﬁnal step is surface

passivation. This is where coating on the surface of Cdots by compounds of the amine functional groups

Figure 1.Sample preparationﬂowchart.

2

Mater. Res. Express6(2019)105703 I W L Lewaet al

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contained in urea takes place. Cdots surface without coating is not only exposed to contaminants, but also powerless because carbon and oxygen are endogenous to be able to react with organic molecules, hence, it can eliminate opto-electronic properties of Cdots. Therefore, coating is very important because it can maintain the stability of Cdots’physical properties and strengthenﬂuorescence. Surface passivation forms a thin insulating capping layer that can protect Cdots and increase theirﬂuorescence. There are various types of polymers or organic molecules that can be used as passivation agents as long as they do not contain chromophores from visible light to UV and they do not emit the same wavelength, as this may affect the original luminescence of Cdots[24].

Results obtained in this synthesis process are black solids, which were then dissolved in puriﬁed water for further observation. Upon observation using UV radiation with a wavelength of 280–300 nm it appeared that the Cdots emit green luminescence, as shown inﬁgure2below.

Theﬁgure shows that activated carbon(a)has no green luminescence, while Cdots produce green luminescence(b). This indicates change in optical properties when Cdots are changed into a quantum nano materials dimension.

Optical characterization

Optical characterization of Cdots was performed using UV-visible spectroscopy andﬂuorescence spectroscopy.

Absorption spectra of synthesized Cdots(ﬁgure3(a))showed two absorption peaks; at 330 nm and 410 nm.

These absorption peaks could be associated withπ→π^*transition of C=C bond and n→π^*transition of C=O bond, respectively. These are transitions of carbonyl and oxygen containing compounds. These results corresponds to several study before[25,26]. Figure3(a)shows the effect of adding urea that causes a decrease in absorption intensity from the sample. This is possible as the more nitrogen levels contained in urea, the less Cdots absorption is because of lower levels of citric acid and more predominant nitrogen levels. Furthermore, surface functional groups also play an important role in determining the absorption wavelength of Cdots.

Thefluorescence spectrum shows a peak at a wavelength of 590 nm. At a concentration of 1 gram, 2 g and 3 g of urea, there is an increase influorescence intensity. Fluorescence that occurs in Cdots is caused by the presence of surface passivation process by passivation agents. The passivation process results in surface energy trap that enables emission stability and hence, improvedfluorescence of Cdots. This is because of the quantum

Figure 2.(a)Activated carbon, and(b)Cdots illuminated by UV radiations, and(c)non-illuminated Cdots.

Figure 3.Optical characterization of Cdots(a)absorbance spectra, and(b)ﬂuorescence spectra.

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confinement effect of the emission energy trap on particles, where the ratio between the surface and volume of particles affects passive particles[20].Fluorescence intensity of Cdots saturated at a variation of 4 g urea kept on decreasing until the concentration reaches 7 g of urea. The reason is that at a concentration of 4 g, the level of urea is more dominant than citric acid as a carbon source. So it is estimated that the number of carbon bonds decreases and this results in reducedfluorescence intensity. The effect of concentration is very important for the fluorescent properties of Cdots. Emissions from strong surface energy levels are caused by changes in

concentration[27].

Structural characterization

In addition to optical characterization, characterization using SEM, EDX and FTIR were also carried out. SEM is used to see the topography of this material. Fromﬁgure4(a)we can see that cdots are irregularly shaped with a rough surface. While previous research stated that cdots have spherical shape and uniform size[28]. This is because cdots tend to agglomerate and poses a problem for characterization. EDX used to analyze the elements that exist in the material. Fromﬁgure4(b)we can see that the material consists of 100% carbon element.

Meanwhile, FTIR was used to determine the functional group of synthesized material.

FTIR analysis is used to determine the functional groups contained in Cdots[29]. Fromfigure5we can see that cdots shows transmitance band at 3307 cm⁻¹correspond to O–H bond , C≡C bond at 2111 cm⁻¹and transmitance band 1635 cm⁻¹correspond to C=O and C=C bonds . These results show the same results according to previous research explain that the functional group of Cdots contain O–H at wave numbers 3100–3400 cm⁻¹and function group C=O at 1600–1770 cm⁻¹[30]. Results of FTIR measurement show no significant differences with urea variation. Cdots will be more stable and hidrofility increases if there are O–H and N–H groups[31].

Figure 4.(a)SEM image from the sample produced at 10,000 magniﬁcation, and(b)EDX results showing 100% carbon atoms.

Figure 5.FTIR measurement from citric acid and urea.

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Fe³⁺ions detection

The Fe³⁺ions detection test was carried out tofind out changes influorescence properties of Cdots when some heavy metal solutions were added. Observations show that Cdotsfluorescence changes with the addition of heavy metals ions solution, as can be seen infigure6.

It can be seen infigure6(a)that when given a standard solution of Cr⁶⁺and Pb²⁺fluorescence of cdots remained constant. But it was different when Cdots were given a solution of Fe³⁺, as thefluorescence began to quench. This can be proven by observing PL spectrum shown infigure6(b). It is easy to see in the spectrum that when compared to other metal ions, Fe³⁺shows more quenched effect with decrease in the emission spectrum.

Therefore, we can conclude that Cdots synthesized from citric acid and urea are sensitive to Fe³⁺ion solutions.

Quenchedﬂuorescence of cdots are caused by several functional groups on the their surface. These include hydroxyl and carboxyl groups that are capable to selectively respond to Fe³⁺ions. The mechanism of this ﬂuorescence turning off stems from charge transfer and controlled exciton recombination[26,32].

Conclusions

A synthesis of Cdots has been successfully carried out using the microwave irradiation method of citric acid and urea via microwave irradiation process. The synthesized Cdots show bright greenfluorescence and are sensitive to Fe³⁺ions. Therefore, it can be concluded that the addition of urea increasesfluorecence. Nonetheless, Cdots saturate at some point and have reduced the intensity. The most appropriate concentration of citric acid-urea that produce the strongestfluorescence is at a concentration 2:3. Cdotsfluorescence is quenched upon administration of a standard solution of Fe³⁺ion. This quenching mechanism is caused by the respons of carboxyl and hydroxyl functional groups with Fe³⁺ions that reside on the surface of Cdots.

Acknowledgments

The authors would like to thank Diponegoro University for funding this research in 2019.

ORCID iDs

H Sutanto https://orcid.org/0000-0003-3404-0337

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Bright green fluorescence of microwave irradiation-

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Bright green ﬂuorescence of microwave irradiation-synthesized Cdots as sensitive probe of iron (III)

^(Article)

, , , ,

Department of Physics, Diponegoro University, Jl. Prof. Soedarto, SH, Semarang, 50275, Indonesia

Central Laboratory of Research and Services, Diponegoro University (CORES DU), Jl. Prof. Soedarto, SH, Semarang, 50275, Indonesia

Abstract

Carbon nanodots (Cdots) are very attractive materials due to their ﬂuorescence and great potential in various ﬁelds.

One field that still needs to be developed is heavy metal ion detector. In this study, a simple and cost efficient fluorescent detector of Fe was built. This material was synthesized by microwave irradiation method using citric acid and urea with purified water as the solvent to get the optimal concentration of urea in order to produce bright green fluorescence. Synthesized Cdots with optimal concentration of urea emit bright green fluorescence under UV light radiation. This bright green fluorescence was then used to detect Fe . The fluorescence of this solution was quenched with the addition of Fe due to transfer charges and exciton recombination. Optical characterization was carried out using UV-vis spectrophotometer, and fluorescence spectrophotometer. Results showed two absorption peaks on Cdots; at 330 nm and 410 nm. Fluorescence analysis was performed using a beam of 532 nm produced emission at a wavelength of 590 nm. In addition, structural characterization was performed using FTIR, SEM and EDX. © 2019 IOP Publishing Ltd.

SciVal Topic Prominence

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Author keywords

bio imaging bright Green ﬂuorescence Cdots microwave irradiation

Indexed keywords

Engineering controlled terms:

Heavy metals Iron compounds Irradiation Metabolism Metal ions Meteorological instruments Microwave irradiation Spectrophotometers Urea

Engineering uncontrolled terms

Bio-imaging Cdots Fluorescence spectrophotometer Green ﬂuorescence Optical characterization Optimal concentration Structural characterization UV-Vis spectrophotometers

Engineering main heading:

Fluorescence

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Not every article in a journal is considered primary research and therefore "citable", this chart shows the ratio of a journal's articles including substantial research (research articles, conference papers and reviews) in three year windows vs. those documents other than research articles, reviews and conference papers.

Documents Year Value

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Ratio of a journal's items, grouped in three years windows, that have been cited at least once vs. those not cited during the following year.

Documents Year Value

Uncited documents 2014 0 Uncited documents 2015 117 Uncited documents 2016 391 Uncited documents 2017 627

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0 0.3 0.6 0.9 1.2 1.5

2014 2015 2016 2017 2018

0 2k 4k

2014 2015 2016 2017 2018

0 0.7 1.4

2014 2015 2016 2017 2018

12 18 24 30

2014 2015 2016 2017 2018

0 2k 4k

2014 2015 2016 2017 2018

0 2k 4k

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(29)

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2014-present Materials Research Express doi:10.1088/issn.2053-1591

Online ISSN: 2053-1591

Bright green ﬂ uorescence of microwave irradiation-synthesized Cdots as sensitive probe of iron (III)

Bright green ﬂ uorescence of microwave irradiation-synthesized Cdots as sensitive probe of iron (III)

Carbon nanodots

are very attractive materials due to their

various

simple and cost efﬁcient

was built. This material was synthesized by microwave irradiation method using citric acid and urea with puriﬁed water as the solvent to get the optimal concentration of urea in order to produce bright green

optimal concentration of urea emit bright green

green

. The

the addition of Fe

due to transfer charges and exciton recombination. Optical characterization was carried out using UV–vis spectrophotometer, and

two absorption peaks on Cdots; at 330 nm and 410 nm. Fluorescence analysis was performed using a beam of 532 nm produced emission at a wavelength of 590 nm. In addition, structural characterization was performed using FTIR, SEM and EDX.

Introduction

Material and methods

Results and discussion

Conclusions

Acknowledgments

ORCID iDs

References

Bright green fluorescence of microwave irradiation-

synthesized

by Agus Subagio

6 %

SIMILARITY INDEX

3 %

INTERNET SOURCES

5 %

PUBLICATIONS

4 %

STUDENT PAPERS

1 2 %

2 1 %

3 1 %

4 < 1 %

5 < 1 %

Bright green fluorescence of microwave irradiation-synthesized

link.springer.com

Internet Source

Sachin Kadian, Gaurav Manik, Ashish Kalkal, Manjinder Singh, Rishi Pal Chauhan. "Effect of sulfur doping on fluorescence and quantum yield of graphene quantum dots: an

experimental and theoretical investigation", Nanotechnology, 2019

Publication

Fu-Gen Wu, Xiaodong Zhang, Xiaokai Chen, Wei Sun, Yan-Wen Bao, Xian-Wu Hua, Ge Gao, Hao-Ran Jia. "Chapter 3 Quantum Dots for

Cancer Therapy and Bioimaging", Springer Nature, 2018

Publication

Submitted to Thammasat University

Student Paper

nanoscalereslett.springeropen.com

Internet Source

Li, Panpan, Lei Huang, Youjie Lin, Leo Shen, Qi

6 < 1 %

7 < 1 %

8 < 1 %

9 < 1 %

10 < 1 %

Chen, and Wangzhou Shi. "Printable

temperature-responsive hybrid hydrogels with photoluminescent carbon nanodots",

Nanotechnology, 2014.

Publication

Submitted to University of Wisconsin - Stout

Student Paper

Hongzhen Liu, Xin Zhao, Fei Wang, Yunpeng Wang, Liang Guo, Jingjing Mei, Cancan Tian, Xiaotian Yang, Dongxu Zhao. "High-Efficient Excitation-Independent Blue Luminescent Carbon Dots", Nanoscale Research Letters, 2017

Publication

Submitted to Queen's University of Belfast

Student Paper

Anil Kumar, M R, H P Nagaswarupa, K S

Anantharaju, K Gurushantha, C Pratapkumar, S C Prashantha, T R Shashishekar, H

Nagabhushana, S C Sharma, Y S Vidya, B Daruka Prasad, C S Vivek Babu, and K R

Vishnu Mahesh. "Banyan latex: a facile fuel for the multifunctional properties of MgO

nanoparticles prepared via auto ignited

combustion route", Materials Research Express, 2015.

Publication

11 < 1 %

Jing-Hui Zhang, Aping Niu, Jing Li, Jian-Wei Fu, Qun Xu, De-Sheng Pei. "In vivo characterization of hair and skin derived carbon quantum dots with high quantum yield as long-term bioprobes in zebrafish", Scientific Reports, 2016

Publication

/0

Bright green fluorescence of microwave irradiation-synthesized

Instructor

Document details

Bright green ﬂuorescence of microwave irradiation-synthesized Cdots as sensitive probe of iron (III)

6 ^%

3 ^%

5 ^%

4 ^%

1 2 ^%

2 1 ^%

3 1 ^%

4 < 1 ^%

5 < 1 ^%

6 < 1 ^%

7 < 1 ^%

8 < 1 ^%

9 < 1 ^%

10 < 1 ^%

11 < 1 ^%