Effect of temperature on the size of biosynthesized silver nanoparticle: Deep insight into microscopic kinetics analysis

Hongyu Liu; Huan Zhang; Jie Wang; Junfu Wei

doi:10.1016/j.arabjc.2017.09.004

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Original article

13 (

); 1011-1019

doi:

10.1016/j.arabjc.2017.09.004

Effect of temperature on the size of biosynthesized silver nanoparticle: Deep insight into microscopic kinetics analysis

Hongyu Liu^⁎, Huan Zhang, Jie Wang, Junfu Wei

State Key Laboratory of Separation Membranes and Membrane Processes, Tianjin Polytechnic University, Tianjin 300387, PR China

School of Environmental and Chemical Engineering, Tianjin Polytechnic University, Tianjin 300387, PR China

⁎Corresponding author at: State Key Laboratory of Separation Membranes and Membrane Processes, Tianjin Polytechnic University, Tianjin 300387, PR China. liuhongyu77@126.com (Hongyu Liu)

Received: 2017-7-4, Accepted: 2017-9-6, Published: 2017-01-01

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

Lacking of microscopic insight into quantitative nucleation and growth kinetics analysis, the effect of temperature on particle size in wet chemical synthesis of metal nanoparticles is still not fully understood. Firstly, we investigated the influence of temperature on the nucleation kinetics constant k₁ and growth kinetics constant k₂. Based on the microscopic quantitative kinetics analysis, the influence of temperature on size of nanoparticles was discussed and concluded in detail. In order to test and verify the conclusions, synthesis of AgNPs under sufficient and insufficient Ag⁺ precursors respectively was carried out. Temperature exhibits different effect on the size of nanoparticles under sufficient and insufficient Ag⁺ precursors due to its impressively different influence on the nucleation kinetics constant k₁ and growth kinetics constant k₂. It is the first time to discuss the effect of temperature on size of nanoparticles in detail based on the microscopic quantitative kinetics analysis. Our work provides useful deep insight into microscopic kinetics analysis of the effect of temperature on size distribution of AgNPs.

Keywords

Microscopic kinetics

AgNPs

Nucleation

Growth

Particle size

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1 Introduction

Wet chemical synthesis of metal nanoparticles in liquid phase has achieved great success in recent years (Murphy et al., 2005; Gupta and Gupta, 2005; Cushing et al., 2004; Sun and Xia, 2002 ), including conventional chemical methods (Hyeon, 2003; Sau and Murphy, 2004) and novel biological methods (Sharma et al., 2009; Raveendran et al., 2003; Liu et al., 2012, 2013, 2014 ). Since, as generally accepted, the properties of nanoparticles, such as optical (Rechberger et al., 2003; Kelly et al., 2003; Pandey et al., 2014 ); magnetic (Pandey et al., 2014; Nadeem et al., 2016), catalytic (Cuenya, 2010; Zhang et al., 2017), optoelectronic (Cho et al., 2015) and thermal (Ceylan et al., 2006); are size and shape dependent (Cuenya, 2010), a great deal of effort has been put into size controlled synthesis of nanoparticles (Yu et al., 2016; Lv et al., 2016; Kwizera et al., 2016; Zhang et al., 2015; Dai et al., 2015 ). Process conditions, such as temperature, time, pH and concentration of reactants are the significant influencing factors on the size of nanoparticles (Sedighi and Montazer, 2016; Makhdoomi et al., 2015; Wang et al., 2010 ). This drives us to exert greater control on the reaction parameters. Gardea-Torresdey et al. (2003) reported that the shape and size of the nanoparticles synthesized using plants can be controlled and modulated by changing the pH. Chinnasamy et al. (2002) reported an extensive series of experiments for the spinel-structured CoFe₂O₄ designed to determine the effect of reaction temperature and reactant concentration on particle size.

With regard to the effect of reaction temperature, most of reports revealed that the size of nanoparticles become smaller with the increased temperature. For example, it was demonstrated by Fayaz et al. (2009) that at lower reaction temperature the size of the nanoparticles were increased whereas increases in temperature results decrease in size of nanoparticles. Khalil et al. (2014) synthesized silver nanoparticles using olive leaf extract and they reported that increasing of the reaction temperature led to a rapid reduction rate of the Ag⁺ ions and the subsequent homogeneous nucleation of silver nuclei-allowing for the formation of AgNPs with small size. As a result, it is generally accepted that high temperature is conducive to nucleation while low temperature is conducive to growth in the field of wet chemical nanoparticles synthesis.

Nevertheless, the discussions and conclusions are all based on the macroscopic experimental phenomena, and no microscopic insight into quantitative nucleation and growth kinetics of nanoparticles was taken into consider. In this work, the effect of temperature on nucleation and growth kinetics constants was discussed in detail at first. Based upon such discussions, the original effect of temperature on particle size was revealed and concluded. In addition, the conclusions were tested and verified by two group well-designed experiments.

2 Experiment

2.1

2.1 Materials and reagents

Silver nitrate (AgNO₃) of analytical grade were purchased from Sinopharm Chemical Reagent Co. Ltd, China and used directly without pretreatment. Cinnamomum Camphor (C. Camphor) leaf was manufactured from Shan Tou Chuang Mei Chinese Traditional Medicine Co. Ltd and deionized water was used in all experiments.

2.2

2.2 Preparation of C. Camphor aqueous extract

C. Camphor leaf was crushed into powder and then 1 g dosage was dispersed into deionized water in the flasks shaking in the shaker for 12 h at a rotation rate of 150 rpm at 30 °C. Then the mixtures in the flasks were filtered with filter paper and the precipitates were removed. The concentration of thus prepared filtrate was denoted as 10 mg/mL. The C. Camphor extract serves as both reducing and capping agents and main components (reducing sugars and flavonoids) are responsible for the bioreduction of the silver ions.

2.3

2.3 Measurement of kinetic constants

Measurement of kinetic constants k₁ and k₂ is the basic of the work. Firstly, as depicted in formula (F-1), we assume reduction of silver precursor $Ag (+)$ by reductants (R) as a reversible reaction in dynamic chemical equilibrium with an equilibrium constant $K_{c}$ . Simultaneously, crystallization would occur when free soluble silver atoms in liquid phase $Ag {(0)}_{l}$ were transformed into solid state $Ag {(0)}_{s}$ . Formula (F-2) indicates the typical phase transformation behavior of $Ag {(0)}_{l}$ into $Ag {(0)}_{s}$ via nucleation; growth of nuclei via interaction between the surface active site $s^{*}$ and $Ag {(0)}_{l}$ was shown in formula (F-3). $k_{01}$ and $k_{02}$ were overall nucleation and crystal growth rate constants, respectively.

(F-1)

Ag (+) + e^{-} \overset{K_{c}}{\leftrightarrow} Ag {(0)}_{l}

(F-2)

Ag {(0)}_{l} \overset{K_{01}}{\to} Ag {(0)}_{s}

(F-3)

Ag {(0)}_{l} + s^{*} \overset{K_{02}}{\to} Ag {(0)}_{s}

Eq. (1) would be obtained based on such assumptions above. Assuming the three formulas are pseudo-elementary reactions, then we have Eq. (2) that denotes the crystallization rate. Approximately, the concentration of the active sites $s^{*}$ is positively proportional to the total surface area of the AgNPs in the solution. Thus, Eq. (3) could be derived whereby s^∗ was denoted as a linear function of $Ag {(0)}_{s}$ with a constant $ε$ . Where, $M_{Ag}$ denotes the molar mass of silver, $ρ_{Ag}$ is the density of silver and $\overline{r}$ is the equivalent average radius of AgNPs. Meanwhile, Eq. (4) can be obtained based on the mass conservation law where ${[Ag (+)]}_{0}$ is the initial concentration of the gold precursor.

(1)

[Ag {(0)}_{l}] = K_{c} \cdot [R] \cdot [Ag (+)]

(2)

\frac{d [Ag {(0)}_{s}]}{dt} = k_{01} [Ag {(0)}_{l}] + k_{02} [s^{*}] [Ag {(0)}_{l}]

(3)

s^{*} = \frac{3 M_{Ag}}{ρ_{Ag} \overline{r}} [Ag {(0)}_{s}] = ε [Ag {(0)}_{s}]

(4)

{[Ag (+)]}_{0} = [Ag (+)] + [Ag {(0)}_{l}] + [Ag {(0)}_{s}]

The sum of Eqs. (1)–(4) gives the crystallization fraction $x$ in Eq. (5) with $α = \frac{K_{c} R}{K_{c} R + 1}$

(5)

x = \frac{[Ag {(0)}_{s}]}{{[Ag (+)]}_{0}} = 1 - \frac{k_{02} ε {[Ag (+)]}_{0} + k_{01}}{k_{02} ε {[Ag (III)]}_{0} + k_{01} e^{α (k_{01} + k_{02} ε {[Ag (+)]}_{0}) t}}

Let $k_{1} = α k_{01}$ and $k_{2} = α ε k_{01} {[Ag (+)]}_{0} k_{02}$ , and then Eq. (5) could be transformed into Eq. (6) through which the crystallization fraction $x$ could be denoted as a function of the reaction time t, with two kinetic parameters, i.e., $k_{1}$ the apparent overall nucleation rate constant and $k_{2}$ the apparent overall growth rate constant, The unit of $k_{1}$ and $k_{2}$ is $s^{- 1}$ . For convenience, thereafter Eq. (6) was referred to as redox–crystallization model according to its derivative mechanism. Specifically, for fitting of the Abs-t profiles by the R–C model (Finney and Finke, 2008; Polte et al., 2010; Zhou et al., 2013 ); Eq. (6) could be further transformed into Eq. (7).

(6)

x = 1 - \frac{k_{2} + k_{1}}{k_{2} + k_{1} s^{(k_{1} + k_{2})} t}

(7)

A_{t} = A_{\max} \cdot (1 - \frac{k_{2} + k_{1}}{k_{1} s (k_{2} + k_{1}) t + k_{2}})

The Abs-t profiles achieved by recording the absorbance at 423 nm by UV–vis spectroscopy were found to be sigmoidal in shape shown as Fig. 1. The concentration of AgNO₃ is 0.125 mM and C. Camphor aqueous extract is 10 mg/mL. More detailed measurement methods of nucleation rate constant k₁ and growth rate constant k₂ can be found in our previous work (Zhou et al., 2013, 2014).

Fitting of the Abs-t profiles by R–C model for silver nanohydrosol.

2.4

2.4 Synthesis of AgNPs

2.4.1

2.4.1 Under sufficient Ag⁺ precursor

In a typical synthesis of AgNPs under sufficient Ag⁺ precursors, a flask filled with 100 mL AgNO₃ solution (2 mM) was preheated in an oil bath (equipped with magnetic stirring) at different temperature for 5 min. Feed solution of C. Camphor aqueous extract (10 mg/mL) was injected into the flask through a syringe pumps at addition rate of 20 mL/h.

2.4.2

2.4.2 Under insufficient Ag⁺ precursor

In a typical synthesis of AgNPs under insufficient Ag⁺ precursors, a flask filled with C. Camphor aqueous extract (10 mg/mL) was preheated in an oil bath (equipped with magnetic stirring) at different temperature for 5 min. Feed solution of 100 mL AgNO₃ solution (2 mM) was injected into the flask through a syringe pumps at addition rate of 20 mL/h.

2.5

2.5 TEM characterization of the AgNPs

TEM observations were performed using an electron microscope (Tecnai F30, FEI; Netherlands) with an accelerating voltage of 300 kV. The samples were prepared by dipping the copper grid in the silver hydrosol (2 mL), and then put into a vacuum drier to allow water to evaporate. The particle solutions were not diluted. In addition, the size distributions were obtained by measuring and counting the particles in the TEM image with the assistance of SigmaScan Pro 4.

3 Results and discussion

3.1

3.1 Effect of temperature on kinetic constant

As generally accepted in the previous published literatures, high temperature is conducive to nucleation while low temperature is conducive to growth in the field of wet chemical nanoparticle synthesis. The reason is that the particle size would get smaller with the increasing reactive temperature. In other words, nanoparticles with larger size can be obtained at relatively lower temperature. Therefore, it is concluded that nanoparticles could grow better and larger at lower temperature, and that is “low temperature is conducive to growth”. However, it is observed that the total reaction rate is increased with the increasing reactive temperature. Accordingly, it is concluded that high temperature is conducive to nucleation. Based on the above conclusions, it could be deduced that the nucleation rate constant k₁ would become larger with increasing reaction temperature, while the growth rate constant k₂ would get smaller with increasing reaction temperature.

Nevertheless, it is confirmed by our experiment that the fact is different. The effect of temperature on k₁ and k₂ are achieved through experimental measurement and the results are shown in Fig. 2. As shown in Fig. 2(a), growth rate constant k₁ increases slightly when temperature was raised from 70 to 80 °C, while it rises sharply when temperature exceed 80–90 °C. Accordingly, k₁ indeed gets larger with increasing reaction temperature, and it become sensitive to temperature under high high-temperature region. However, as shown in Fig. 2(b), growth rate constant k₂ also gets larger with increasing reaction temperature, and the growth rate increases almost linearly to reaction temperature. Therefore, the variation tendency of k₂ is contrary to the deduction that k₂ would get smaller with increasing reaction temperature from the practice that nanoparticles with larger size are obtained at relatively lower temperature. We propose that there are two key points to explain this phenomenon. One is the abrupt change of k₁ when temperature was enhanced over a special value (80 °C in this work), and another is whether the amounts of precursors are sufficient or not. Due to the sharply increase of k₁ at high temperature (80–90 °C), lots of Ag⁺ precursors nucleate becoming crystal nucleus. At this stage, if the amounts of precursors are sufficient, the precursors would grow faster on the nucleus on account of the increased k₂ at high temperature. Nevertheless, if the amounts of precursors are insufficient, there are fewer precursors for growth. As a result, size of the nanoparticles still gets smaller in spite of the increased k₂ at high temperature. In order to confirm the standpoint discussed above, two groups of experiments are designed as follows.

(a) Nucleation rate constant k1 and (b) growth rate constant k2 under different temperatures.

3.2

3.2 Synthesis of AgNPs under sufficient Ag⁺ precursors

In a typical synthesis of AgNPs under sufficient Ag⁺ precursors, AgNO₃ solution is excess to C. Camphor aqueous extract. Accordingly, Ag⁺ precursors could grow on the crystal nucleus abundantly, and the nanoparticles could grow bigger without limit. TEM images and corresponding size distribution of the AgNPs synthesized under sufficient precursors at different temperature are shown in Fig. 3. It indicates that the average diameter of AgNPs synthesized under 70–90 °C is 7.8 ± 2.3 nm, 9.8 ± 3.9 nm, 12.8 ± 4.1 nm, 15.3 ± 3.7 nm and 17.6 ± 4.5 nm, respectively. Accordingly, it is easily figured out from Fig. 3 that the size of AgNPs under sufficient precursors increases with the increased temperature gradually. The increasing tendency is shown in Fig. 4, indicating that it is almost a linear increase of particle size. Moreover, by comparing of Fig. 4 with Fig. 2(b), it is found that the increase of particle size almost has the same trend with the increase of the growth rate constant k₂ under sufficient precursors. Therefore, it could be concluded that the increase of particle size with enhanced temperature is caused by the increase of k₂ when precursors are sufficient. In this condition, the particle size is not influenced by the nucleation rate constant k₁, and k₁ only effect on the amounts of nanoparticles. Schematic illustration for kinetic-controlled biosynthesis of AgNPs under insufficient Ag⁺ precursors is shown in Scheme 1.

TEM images and corresponding size distribution of the AgNPs synthesized under sufficient precursor at different temperature (a) 70 °C, (b) 75 °C, (c) 80 °C, (d) 85 °C and (e) 90 °C.

Particle diameter of AgNPs synthesized under sufficient precursors at different temperature.

Schematic illustration for kinetic-controlled biosynthesis of AgNPs under sufficient Ag+ precursors.

3.3

3.3 Synthesis of AgNPs under insufficient Ag⁺ precursors

In a typical synthesis of AgNPs under insufficient Ag⁺ precursors, AgNO₃ solution is insufficient and C. Camphor aqueous extract is excess. As a result, nucleation and growth would compete with each other for Ag⁺ precursors. As shown in Fig. 2(a), nucleation rate constant k₁ increases slightly when temperature was raised from 70 to 80 °C, while it rises sharply when temperature exceed 80–90 °C. By comparison with Fig. 2(b), growth rate constant k₂ increases almost linearly to reaction temperature. As calculated by Eqs. (8)–(11), k₁ increases 1.17 times and k₂ increases 1.77 times as temperature was raised from 70 to 80 °C. Therefore, growth would take advantages to nucleation at this stage. As a result, it could be deduced that size of the nanoparticles would get a little bigger as temperature was raised from 70 to 80 °C. Nevertheless, k₁ increases 4.57 times but k₂ only increases 1.64 times when temperature was raised from 80 to 90 °C. Accordingly, the sharply increased k₁ would lead to an explosive nucleation which would consume lots of Ag⁺ precursors. As a result, growth would be restricted duo to lack of Ag⁺ precursors. It could be deduced that size of the nanoparticles would get evidently smaller in spite of the increased k₂ when temperature was raised from 80 to 90 °C.

(8)

k_{1} (80 ° C) / k_{1} (70 ° C) = 1.17

(9)

k_{2} (80 ° C) / k_{2} (70 ° C) = 1.77

(10)

k_{1} (90 ° C) / k_{1} (80 ° C) = 4.57

(11)

k_{2} (90 ° C) / k_{2} (80 ° C) = 1.64

TEM images and corresponding size distribution of the AgNPs synthesized under insufficient precursors at different temperature are shown in Fig. 5. It indicates that the average diameter of AgNPs synthesized under 70–90 °C is 4.6 ± 1.3 nm, 5.0 ± 0.8 nm, 5.3 ± 1.3 nm, 3.5 ± 0.8 nm and 2.7 ± 0.4 nm, respectively. The variation tendency is shown in Fig. 6, and it could be easily figured out from Fig. 6 that size of AgNPs increases slightly from 70 to 80 °C while it decreases sharply from 80 to 90 °C. Accordingly, the result is in good agreement with the deduction discussed above. It could be concluded that the decrease of size at high temperature is result from the sharply increased k₁ leading to a lack of precursors for growing under insufficient precursors. Schematic illustration for kinetic-controlled biosynthesis of AgNPs under insufficient Ag⁺ precursors is shown in Scheme 2.

TEM images and corresponding size distribution of the AgNPs synthesized under insufficient precursors at different temperature (a) 70 °C, (b) 75 °C, (c) 80 °C, (d) 85 °C and (e) 90 °C.

Particle diameter of AgNPs synthesized at different temperature under insufficient precursors.

Schematic illustration for kinetic-controlled biosynthesis of AgNPs under insufficient Ag+ precursors.

4 Conclusion

In summary, we demonstrated that high temperature is conducive to both nucleation and growth since both nucleation rate constant k₁ and growth rate constant k₂ are enhanced at high temperature. k₁ increases slightly when temperature was raised from 70 to 80 °C, while it rises sharply when temperature exceed 80–90 °C. However, k₂ increases almost linearly to reaction temperature. Accordingly, if the precursors are sufficient, the increase of particle size almost has the same trend with the increase of k₂. The particle size is not influenced by k₁, and k₁ only influence the amounts of nanoparticles. While, under insufficient precursors, an explosive nucleation would consume lots of Ag⁺, so growth would be restricted duo to lack of Ag⁺ precursors. Size of AgNPs increases slightly from 70 to 80 °C while it decreases sharply from 80 to 90 °C. It could be concluded that the decrease of size at high temperature is result from the sharply increased k₁ instead of the decreased k₂.

Acknowledgements

This work was supported by The Science and Technology Plans of Tianjin (16PTSYJC00110), The Science and Technology Supporting Plans of Tianjin (No. 15ZCZDSF00880), The National Natural Science Foundation of China (No. 51678409, No. 51578375, No. 51378349, No. 51308390, No. 51478461).

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Introduction

Experiment

Materials and reagents
Preparation of C. Camphor aqueous extract
Measurement of kinetic constants
Synthesis of AgNPs
TEM characterization of the AgNPs

Results and discussion

Effect of temperature on kinetic constant
Synthesis of AgNPs under sufficient Ag+ precursors
Synthesis of AgNPs under insufficient Ag+ precursors

Conclusion

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[1] Ceylan A., Jastrzembski K., Shah S.I., . Enhanced solubility Ag-Cu nanoparticles and their thermal transport properties. Metall. Mater. Trans. A. 2006;37A:2033-2038.
[Google Scholar]

[2] Chinnasamy C.N., Jeyadevan B., Perales-Perez O., Shinoda K., Tohji K., Kasuya A., . Growth dominant co-precipitation process to achieve high coercivity at room temperature in CoFe(2)O(4) nanoparticles. IEEE T. Magn.. 2002;38:2640-2642.
[Google Scholar]

[3] Cho E.C., Huang J.H., Li C.P., Chang-Jian C.W., Lee K.C., Huang J.H., . The optoelectronic properties and applications of solution-processable titanium oxide nanoparticles. Org. Electron.. 2015;18:126-134.
[Google Scholar]

[4] Cuenya B.R., . Synthesis and catalytic properties of metal nanoparticles: Size, shape, support, composition, and oxidation state effects. Thin Solid Films. 2010;518:3127-3150.
[Google Scholar]

[5] Cushing B.L., Kolesnichenko V.L., O'Connor C.J., . Recent advances in the liquid-phase syntheses of inorganic nanoparticles. Chem. Rev.. 2004;104:3893-3946.
[Google Scholar]

[6] Dai J., Yang X.Y., Hamon M., Kong L.Z., . Particle size controlled synthesis of CdS nanoparticles on a microfluidic chip. Chem. Eng. J.. 2015;280:385-390.
[Google Scholar]

[7] Fayaz A.M., Balaji K., Kalaichelvan P.T., Venkatesan R., . Fungal based synthesis of silver nanoparticles-An effect of temperature on the size of particles. Colloids Surf., B. 2009;74:123-126.
[Google Scholar]

[8] Finney E.E., Finke R.G., . Nanocluster nucleation and growth kinetic and mechanistic studies: A review emphasizing transition-metal nanoclusters. J. Colloid Interf. Sci.. 2008;317:351-374.
[Google Scholar]

[9] Gardea-Torresdey J.L., Gomez E., Peralta-Videa J.R., Parsons J.G., Troiani H., Jose-Yacaman M., . Alfalfa sprouts: A natural source for the synthesis of silver nanoparticles. Langmuir. 2003;19:1357-1361.
[Google Scholar]

[10] Gupta A.K., Gupta M., . Synthesis and surface engineering of iron oxide nanoparticles for biomedical applications. Biomaterials. 2005;26:3995-4021.
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