Parametric investigations on the influence of nano-second Nd3+:YAG laser wavelength and fluence in synthesizing NiTi nano-particles using liquid assisted laser ablation technique

Accepted Manuscript Title: Parametric investigations on the influence of nano-second Nd 3+ : YAG Laser wavelength and fluence in Synthesizing NiTi Nano-particles using Liquid assisted Laser Ablation Technique Author: Nandini Patra K. Akash S. Shiva Rohit Gagrani H. Sai Pranesh Rao V.R. Anirudh I.A. Palani Vipul Singh PII: DOI: Reference:

S0169-4332(16)00109-4 http://dx.doi.org/doi:10.1016/j.apsusc.2016.01.072 APSUSC 32304

To appear in:

APSUSC

Received date: Revised date: Accepted date:

3-7-2015 20-12-2015 8-1-2016

Please cite this article as: N. Patra, K. Akash, S. Shiva, R. Gagrani, H.S.P. Rao, V.R. Anirudh, I.A. Palani, V. Singh, Parametric investigations on the influence of nanosecond Nd 3+ : YAG Laser wavelength and fluence in Synthesizing NiTi Nano-particles using Liquid assisted Laser Ablation Technique, Applied Surface Science (2016), http://dx.doi.org/10.1016/j.apsusc.2016.01.072 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

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Highlights:

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Influence of laser wavelengths ( 1064 nm, 532 nm and 355 nm) and fluences (40 J/cm2, 30 J/cm2 and 20 J/cm2) on generation of underwater laser ablated NiTi nanoparticles • Particle size range of 140-10 nm was generated at varying laser wavelengths • The alloy formation of NiTi nanoparticles was confirmed from XRD and TEM analysis where the crystalline peaks of NiTi, Ni4Ti3 and Ni3Ti were observed from XRD • Formation efficiency of NiTi nanoparticles was maximum at 1064 nm wavelength and 40 J/cm2 fluence

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Parametric investigations on the influence of nano-

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second Nd 3+: YAG Laser wavelength and fluence in

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Synthesizing NiTi Nano-particles using Liquid

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assisted Laser Ablation Technique

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Nandini Patra1, Akash K. 2, S. Shiva 2, Rohit Gagrani 2, Sai Pranesh Rao H. 2,

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Anirudh V. R. 2, Palani I. A. 1, 2, Vipul Singh1

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Centre for Material Science and Engineering, Indian Institute of Technology, Indore,

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Mechatronics and Instrumentation lab, Discipline of Mechanical Engineering,

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Madhya Pradesh, Pin-453441, India

Indian Institute of Technology, Indore, Madhya Pradesh, Pin-453441, India

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Abstract:

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*[email protected], [email protected]

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This paper investigates the influence of laser wavelengths and laser fluences on the

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size and quality of the NiTi nanoparticles, generated through underwater solid state

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Nd:YAG laser ablation technique. The experiments were performed on Ni55%-

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Ti45% sheet to synthesize NiTi nano-particles at three different wavelengths (1064

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nm, 532 nm and 355 nm) with varying laser fluences ranging from 20-40 J/cm2.

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Synthesized NiTi nano-particles were characterized through SEM, DLS, XRD, FT-IR,

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TEM and UV-Vis spectrum. It was observed that, maximum particle size of 140 nm

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and minimum particle size of 10 nm were generated at varying laser wavelengths. The

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crystallinity and lattice spacing of NiTi alloy nanoparticles were confirmed from the

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XRD analysis and TEM images, respectively.

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Keywords: NiTi nanoparticle, under water laser ablation, Nd: YAG laser, laser

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wavelength, structural analysis, formation efficiency.

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1. Introduction:

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Previous researchers have investigated various synthesizing techniques for

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nanoparticles owing to their potential applications in different fields of technology

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and life such as electronics, mechanics, energy creation, storage [1] and medical [2,

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3].

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reversible transition between austenite and crystal phases under temperature and

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stress [4, 5, 6, 7] effects. This attractive functional material is used in industrial

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applications for its high strength, high corrosion resistance, ductility, low

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manufacturing cost, good electrical and mechanical properties [6, 8]. Earlier studies

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had shown that the properties of liquid assisted laser ablated NiTi nanoparticle differs

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from bulk due to its ability to synthesize different morphologies of nanoparticles [9].

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It also has wide applications in medical science where it adsorbed to implant surfaces

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as nanocoatings [10]. It was used as a biocompatible material for the replacement of

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structural components inside the human body [3]. Anne Hann et al. had investigated

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the laser ablated NiTi-nano-particles for the cell extension over nanoparticle coating

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where cells were adhered to nano surfaces coated with nanoparticles [11].

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Barcikowski et al. [12] had synthesized NiTi nano-particles to determine the bio-

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compatibility with human adipose-derived stem cells. Tomi Smausz et al. had

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investigated the core-shell nature of NiTi nano-particles where the core-shell

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nanostructures were fabricated by laser ablation method. This has broad range of

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applications in the field of electronics, magnetism, optics and catalysis [13]. Based on

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the applications it is clear that a clean, impurity free technique is required to generate

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NiTi nanoparticles with varying crystal quality and sizes. Under water laser ablation

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is an emerging technique for synthesizing pure nanoparticles. Few literatures are

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available on under water laser ablation to generate nanoparticles thorough pico and

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femto-second lasers. However limited reports are available on under water laser

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ablation on NiTi target by using nano-second Nd: YAG laser.

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NiTi shows unique shape-memory and super elastic properties due to their

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In this research an attempt has been made to investigate the influence of laser

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wavelengths (1064 nm, 532 nm and 355 nm) and fluences (range: 20-40 J/cm2) on

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size and morphology of as generated NiTi nano particles, which haven’t been reporter

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elsewhere. The colloidal solutions of NiTi nanoparticles in de-ionized water were

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collected and samples were prepared for further characterization. The surface

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morphology and particle size distribution were investigated through SEM and DLS

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analysis. The crystallanity and the oxidation characteristics of the generated

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nanoparticles were examined using XRD, TEM and FT-IR analysis. The nanoparticle

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formation efficiency was investigated and discussed using UV-VIS analysis.

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2. Experimental Specification:

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Figure 1 shows the schematic layout of the experimental setup.

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nanosecond pulsed laser (Quanta Ray-INDI) with a frequency of 10 Hz and pulse

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duration of 5-8 ns was used to ablate the NiTi target. Laser wavelengths of 1064, 532

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and 355 nm were generated by using KDP crystal. The NiTi nanoparticles were

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generated using NiTi thin sheets (Nitinol 55 - 55% Ni and 45% Ti; dimension:

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8×8×0.15 mm3), placing at the bottom of the petri dish filled with 10 mL (3 mm water

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layer above the sheet) of de-ionized water. Laser beam generated by the Nd:YAG

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laser was reflected at an angle of 90o with the help of a dichroic mirror and focused on

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the surface of the target by using a converging lens (f = 30 cm). The laser beam radius

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of 0.25 mm was measured using a burn paper and a microscope (Toolmakers

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microscope, Carmar Technology Co. Ltd.) at 30X magnification. The energy of the

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laser pulse was measured using a power meter (Newport 842-PE) and the laser

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fluences were calculated as 40 J/cm2, 30 J/cm2 and 20 J/cm2. Each process was

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typically performed for 45 minutes (27000 pulses) at room temperature (25oC).

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The as generated nanoparticles were separated from the colloidal solution by

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evaporating the solution on a glass slide (10×10×1 mm) which was kept on a hotplate

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(90o C). The particle size distributions and shape characterizations were investigated

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using SEM (Supra 55, Zeiss), DLS (SZ-100) and TEM analysis. The oxidation

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behaviour was investigated by FT-IR (Tensor 27, Bruker) analysis. The phase

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transformations and absorption capacities were investigated by XRD (Rigaku

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SmartLab), and UV-Vis (Varian Cary 100) spectrum, respectively.

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The Nd:YAG

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3. Results:

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The effects of laser wavelengths and fluences on the size and morphology of NiTi

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alloy nanoparticles are discussed in the following sections.

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The SEM and DLS analysis of NiTi alloy nanoparticles synthesized at 1064 nm using

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three different fluences (40 J/cm2, 30 J/cm2, and 20 J/cm2) are presented in Figure 2

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(a,c,e) and figure 2 (b,d,f) respectively. DLS gives hydrodynamic particle size

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distributions where the average particle size of 47 nm (Figure 2a) from SEM and

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particle size distribution range of 26-76 nm (Figure 2b) from DLS were observed at

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40 J/cm2 laser fluence. With the reduction of laser fluence to 30 J/cm2, the average

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particle size of 76 nm was observed (Figure 2c) and particle sizes were in the range of

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44-120 nm (Figure 2d). At 20 J/cm2 laser fluence, the average particle size of 85 nm

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(Figure 2e) and particle size distribution range of 56-121 nm (Figure 2f) was

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observed.

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3.2: Investigations on influence of 532 nm laser wavelength:

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The average particle size of 42 nm (Figure 3a) and particle size distribution range of

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20-73 nm (Figure 3b) were observed for the laser fluence of 40 J/cm2. Further

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reducing the laser fluence to 30 J/cm2, the observed average particle size of 72 nm is

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shown in Figure 3c and size distribution range of 49-111 nm is shown in Figure 3d.

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The average particle size of 79 nm (Figure 3e) and particle size distribution range of

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45-140 nm (Figure 3f) were observed at 20 J/cm2 laser fluence.

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3.3: Investigations on influence of 355 nm laser wavelength:

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The same investigation was done at a wavelength of 355 nm. The average particle

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size of 35 nm (Figure 4a) and the respective particle size distribution range of 10-79

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nm (Figure 4b) were observed at laser fluence of 40 J/cm2. Further decreasing the

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laser fluence to 30 J/cm2, an average particle size of 38 nm (Figure 4c) and particle

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size distribution range of 20-63 nm (Figure 4d) were observed. Average particle size

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of 68 nm (Figure 4e) and respective particle size distribution range of 38-110 nm

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(Figure 4 f) were observed at a reduced fluence to 20 J/cm2. Based on the above

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analysis, the average size and size variation of the nanoparticles have been tabulated

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in Table 1 where the effect of different laser wavelengths and fluences on average

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size of the nanoparticles are analysed. The particle size distribution data generated

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from software (ImageJ) and DLS can be comparable and is tabulated in the table

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(Table 1).

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From the table, it was observed that the average size of nanoparticles prepared at 1064

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nm wavelength is comparable with the nanoparticles prepared at 532 nm wavelength.

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However, the 355 nm wavelength has a capability to generate nanoparticles less than

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15 nm. Discussions on structural analysis of these nanoparticles are as follows.

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Figure 5 shows different structural phases of NiTi at different laser wavelengths and

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fluences. The crystalline peak of NiTi (020) was observed (Figure 5a) for the samples

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prepared at 1064 nm laser wavelength with three different fluences. The additional

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peak of Ni4Ti3 (220) was observed at 20 J/cm2 laser fluence. The similar procedures

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were followed to prepare the samples at 532 nm (Figure 5b) laser wavelenth with

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three different fluences. The crystalline peaks of NiTi (020) and Ni3Ti (102) were

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observed at 40 J/cm2 laser fluence. Peaks of NiTi (020), Ni3Ti (102) and Ni4Ti3 (220)

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were observed at 30 J/cm2 and the peaks of Ni3Ti (102) and Ni4Ti3 (220) were

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observed at 20 J/cm2. Further decreasing the laser wavelength to 355 nm (Figure 5c),

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the crystalline peaks of Ni4Ti3 (220) and Ni3Ti (102) were observed for the samples

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prepared at three different laser fluences. The additional peak of NiTi (020) was

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observed for the sample prepared with laser fluence of 20 J/cm2.

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3.5: FT-IR measurements:

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The results of FT-IR spectroscopic analysis for the samples prepared at three different

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wavelengths (1064 nm, 532 nm and 355 nm) are shown in Figure 6a, 6b, and 6c. The

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NiTi sample was measured as a KBr pallet in the 400 to 4000 cm-1 spectral range at a

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resolution of 4 cm-1. A broad band at 3400-3421 cm−1 was observed which is related 6

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to stretching hydroxyl (O-H), representing the water as moisture [14]. The band at

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2334-2359 cm-1 and 1615 cm-1 were assigned to the stretching vibrations of surface

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hydroxyl (–OH) groups and another band around 1280 cm-1 was due to the bending

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vibration of the H−O−H bonds [15,16]. The main peak was observed at around 1384-

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1421 cm-1 which can be attributed to the Ti-O bond in the samples prepared at three

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different wavelengths [17]. The peak around 1031-1054 cm-1 may be due to

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characteristics O-O stretching vibration [18]. The peak between 700 and 875 cm-1 was

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assigned to the Ti-O stretching bands [14].

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Figure 7 shows the TEM images for the sample prepared at 1064 nm wavelength and

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40 J/cm2 fluence. Different sizes of nanoparticles are observed in Figure 7a and

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minimum particle size of 10 nm is observed in Figure 7b. It was investigated from

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those images that the shapes of the nanoparticles were almost spherical and it was in

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crystalline form. The calculated d spacing between adjacent lattice planes in texture of

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nanoparticle (Figure 7b) can be compared with the theoretical d spacing of Bragg’s

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plane.

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4. Discussion:

4.1 Influence of laser wavelengths:

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The effect of different laser wavelengths on average size of nanoparticles were

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examined from SEM images (Figure 2, Figure 3 and Figure 4). It was observed (Table

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1) that the average size of NiTi nanoparticles synthesized at 355 nm wavelengths is

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smaller than nanoparticles generated at 532 nm and 1064 nm wavelengths. As the

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absorption co-efficient of NiTi is higher at 355 nm wavelength, so the intensity of

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absorption peak is higher than 532 and 1064 nm wavelength. The photon energy of

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355 nm is higher. So the average size of nanoparticles prepared at 355 nm is smaller

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compared to higher wavelengths [19]. All the nanoparticles synthesized at 1064 nm

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wavelength by varying laser fluences (40 J/cm2, 30 J/cm2, and 20 J/cm2), shows the

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crystalline peak of NiTi (020) (Figure 5a). The crystalline nature of the NiTi

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nanoparticle can be further confirmed from the TEM images (Figure 7b). This was

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verified using Bragg’s d spacing calculations (Figure 5a and Figure 7b). Based on the

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above investigations, we confirm the formation of NiTi alloy nanoparticles in

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crystallographic nature [20, 21]. The additional peak of Ni4Ti3 (220) (Figure 5a) was

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observed at laser fluence of 20 J/cm2, which could be due to the low energy barrier

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required [22] for the formation of such intermediate phase. Due to less absorption at

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1064 nm wavelength, it leads to less temperature distribution throughout the

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surrounding work material [23]. Previous studies reported the formation of Ni4Ti3

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phase at lower ageing temperature and shorter ageing time [24, 25]. Thus it can be

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concluded that the nanoparticles can form in different crystal structures [26]. Similar

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investigations were done at 532 nm wavelength (Figure 5b). The peaks of Ni3Ti (102)

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and Ni4Ti3 (220) were observed for the sample prepared at 20 J/cm2 fluence. Further

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increasing the fluence to 30 J/cm2, the phases of NiTi (020), Ni4Ti3 (220) and Ni3Ti

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(102) were observed. Finally the peaks of Ni3Ti (102) and NiTi (020) were observed

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at 40 J/cm2 fluence. This transformation of phases might be due to the higher photons

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energy at lower wavelengths which leads to rapid transformations of crystal phases

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[27]. Previous investigations reported about phase transformation of NiTi to

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intermediate phase of Ni4Ti3 and finally to Ni3Ti with longer ageing time at

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equilibrium [25, 28]. Such transformations were clearly observed at 532 nm (Figure

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5b) wavelengths. The reasons to observe the NiTi (020) phase at 40 J/cm2 and 30

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J/cm2 fluences, might be due to the energy barrier. At higher ageing temperature and

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longer ageing time, Ni3Ti phase was appeared which was observed at higher fluences

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[24, 25]. A single material may have several distinct solid states which form separate

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phases [29, 30]. Thus it can be concluded that different phases has different energy

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levels. The material either takes up or releases energy when it undergoes a phase

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transition. Phase transition turns the material from one phase to another by crossing

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the energy barrier [22].

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Similar investigations were done at 355 nm wavelength. Here we observed the

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formation of Ni4Ti3 and Ni3Ti (Figure 5c) phases in all the samples prepared at three

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different laser fluences. NiTi phase was observed at 20 J/cm2. This might be because

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of the energy barrier [22]. NiTi has higher absorption at 355 nm wavelength which

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influences the temperature distribution throughout the surrounding material than

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higher wavelengths [23]. This might be one possible reason to observe the phases of

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Ni4Ti3 and Ni3Ti for longer ageing temperature [25]. Based on the above analysis at

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different wavelengths, it can be concluded that the alloy formation of NiTi

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nanoparticles with different crystal phases were observed.

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Though the oxidation of nanoparticles were not observed from XRD analysis which

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might be due the noise in XRD data. But the peaks of Ti-O bond were observed

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(Figure 6) from FT-IR spectroscopy analysis for the samples prepared at three

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different wavelengths. This confirms the formation of TiO2 as a sharp peak was

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observed at around 1384 cm-1 which is attributed to the Ti-O bond [17].

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The effect of three different laser fluences on average size and size variation of

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nanoparticles were examined from the SEM images (Figure 2, Figure 3 and Figure 4).

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Based on the analysis from Table 1, it was investigated that the average size of

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nanoparticles were smaller and the formation of nanoparticles increases at higher

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fluences. Thus it increases the concentration of colloidal solution [19].

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During a single laser pulse the nanoparticles are excited due to the absorbance of

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photons. The light absorption at higher fluence leads to generate smaller size of

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nanoparticles, However it was observed that the average particle size was less at

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higher fluences, but there were particles which were as large as 100 nm. This might

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be due to the type of nucleation process during ablation [31, 32]. The direct

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nucleation of particles acting as growing centres for the incoming species which

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contribute to varying size distribution [32]. The range of size variation was less at 355

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nm wavelength than higher wavelengths which might be due to the low

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agglomeration rate of nanoparticles [32, 33] at that wavelength.

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4.3 Influence of absorption co-efficient for nanoparticle formation:

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It was observed that the ablation of NiTi target was increasing with increasing the

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laser fluence [1]. Figure 8 shows the amount of ablated target material for 45 mins

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with respect to laser fluences for three different laser wavelengths. The ablation

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versus the laser fluence is not linear and the slope increases with increasing the

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fluence. The ablation depth is influenced by the absorption depth of the material [34]

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for different wavelengths of light. Thus the ablation depth is the function of beam

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energy, pulse duration and wavelength. NiTi has higher absorption in UV region than 9

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in visible and IR region of light [35]. It was also observed that the laser ablation

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efficiency (Figure 8) was increasing with increasing the laser wavelength [32]. This

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might be due to the higher absorption at 355 nm wavelength leads to heat transfer

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throughout the surrounding work material [23, 34]. It is expected to have higher heat

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conduction at 355 nm wavelength than 532 nm and 1064 nm [23]. Thus the less

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absorption at 1064 nm leads to higher ablation [23]. The above explanation was

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justified with Uv-Vis spectrum analysis (Figure 9) where it was observed that NiTi

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alloy nanoparticle has more absorption at 355 nm than 532 and 1064 nm wavelength.

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Conclusion:

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Nano-second Nd:YAG under water laser ablation is a convenient way to generate

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pure nanoparticles. Laser wavelengths and fluences have an important role in

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controlling the size of the nano-particle. Increase in laser wavelength results in bigger

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particle size whereas increase in laser fluence form smaller sizes of particles.

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Minimum average particle size of 35 nm was observed for the wavelength of 355 nm

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and fluence of 40 J/cm2. The XRD plots at different wavelengths and fluences had

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shown the crystalline peaks of Ni4Ti3, Ni3Ti and NiTi. Alloy form of NiTi was

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observed from XRD and TEM images. The oxidation formation was observed from

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FT-IR spectroscopy. It was investigated that the formation efficiency of nano-

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particles was more at higher wavelengths and higher fluences. Based on UV-Vis

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spectroscopy, the optical absorption capacity of NiTi nanoparticles was high in ultra-

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violet region than in visible and IR region. It can be concluded that, less than 15 nm

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size of NiTi alloy nanoparticle was observed from this investigation.

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Acknowledgement:

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The authors are grateful to the Centre for Material Science and Engineering

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department, Mechanical Engineering department and Sophisticated Instrumentation

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Centre (SIC) of IIT Indore, India for the financial support to carry out the above

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investigations. The authors are also grateful to Kyushu University, Japan for the TEM

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measurements.

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440 Appendix:

443

us

442 1. Figure Captions:

445

an

444

Figure 1: Block diagram of experimental setup

M

446 447

Figure 2: SEM(a,c,e) and DLS(b,d,f) images of nanoparticle generation at 1064 nm

448

wavelength with fluences of (a, b) 40 J/cm2, (c, d) 30 J/cm2 and (e, f) 20 J/cm2

d

449

Figure 3: SEM (a,c,e) and DLS(b,d,f) images of nanoparticle generation at 532 nm

451

wavelength with fluences of (a, b) 40 J/cm2, (c, d) 30 J/cm2 and (e, f) 20 J/cm2

452

Ac ce pt e

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453

Figure 4: SEM (a,c,e) and DLS(b,d,f) images of nanoparticle generation at 355 nm

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wavelength with fluences of (a, b) 40 J/cm2, (c, d) 30 J/cm2 and (e, f) 20 J/cm2

455 456

Figure 5: XRD plots of nanoparticles for the laser wavelength of (a) 1064 nm, (b) 532

457

nm and (c) 355 nm with different fluences of 40 J/cm2, 30 J/cm2 and 20 J/cm2

458 459

Figure 6: FT-IR spectrum at different laser wavelength of (a) 1064 nm, (b) 532 nm

460

and (c) 355 nm

461 462

Figure 7: TEM images of nanoparticles with (a) different sizes and (b) minimum size

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of 10 nm

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Figure 8: Variation of the mass of the target versus laser pulse fluence

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Figure 9: Absorbance spectrum of NiTi naoparticle prepared at 40J/cm2

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2. Table Caption:

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Table 1: Average size and size variation of nanoparticles at different laser

503

wavelengths and fluences comparing the results obtained from software and DLS.

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Table 1:

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Wavelength (nm)

Fluence (J/cm2)

Avg. Particle size (nm) (Software/DLS)

Range of 505 506 nanoparticle size (Software/DLS) 507

40 30 20

42/47 74/76 82/85

22-60/26-76508 31-112/44-120 509 55-114/56-121

532

40 30 20

39/42 66/72 71/76

32-50/20-73 50-93/49-111 43-115/45-140

355

40 30 20

33/35 39/38 55/68

8-60/10-79 16-62/20-63 28-95/38-110

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