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Research Papers

Morphology and Crystallographic Characterization of Nickel Nanowires—Influence of Magnetic Field and Current Density During Synthesis OPEN ACCESS

[+] Author and Article Information
Mahendran Samykano

Department of Nanoengineering,
Joint School of Nanoscience
and Nanoengineering,
North Carolina A&T State University,
2907 East Lee Street,
Greensboro, NC 27401
e-mail: mahendran.samkano@gmail.com

Ram Mohan

Department of Nanoengineering,
Joint School of Nanoscience
and Nanoengineering,
North Carolina A&T State University,
2907 East Lee Street,
Greensboro, NC 27401
e-mail: rvmohan@ncat.edu

Shyam Aravamudhan

Department of Nanoengineering,
Joint School of Nanoscience
and Nanoengineering,
North Carolina A&T State University,
2907 East Lee Street,
Greensboro, NC 27401
e-mail: saravamu@ncat.edu

1Corresponding author.

Manuscript received April 25, 2014; final manuscript received July 14, 2014; published online August 19, 2014. Assoc. Editor: Hsiao-Ying Shadow Huang.

J. Nanotechnol. Eng. Med 5(2), 021005 (Aug 19, 2014) (7 pages) Paper No: NANO-14-1036; doi: 10.1115/1.4028026 History: Received April 25, 2014; Revised July 14, 2014

This paper presents results and discussion from a comprehensive morphological and crystallographic characterization of nickel nanowires synthesized by template-based electrodeposition method. In particular, the influence of magnetic and electric field (current density) conditions during the synthesis of nickel nanowires was studied. The structure and morphology of the synthesized nanowires were studied using Helium ion microscopy (HIM) and scanning electron microscopy (SEM) methods. The HIM provided higher quality data and resolution compared to conventional SEM imaging. The crystallographic properties of the grown nanowires were also studied using X-ray diffraction (XRD). The results clearly indicated that the morphological and crystallographic properties of synthesized nickel nanowires were strongly influenced by the applied magnetic field and current density intensity during the synthesis process.

FIGURES IN THIS ARTICLE
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One-dimensional (1D) magnetic nanostructures have received enormous attention for their numerous applications that includes high-density magnetic storage, sensors and in Nano/Micro electromechanical (NEMS/MEMS) systems. A number of methods and processing conditions have been used to synthesize 1D nanostructures of various sizes, morphology, and composition that have resulted in exciting and fundamentally different configurations [1,2]. Template-based electrodeposition is one such method used to synthesis 1D metallic nanostructures. However, the effect of the synthesis parameters, especially, magnetic field and current density used during the synthesis process on the morphology, crystal orientation and crystal grain size have not been well-understood. In the present paper, the structure and morphology of the synthesized Nickel (Ni) nanowires are analyzed using HIM, which provides much higher resolution compared to the conventional SEM. This results in higher qualitative imaging and nanostructure resolution compared to the SEM characterization. The morphological characteristics of the synthesized nanowires and their differences due to the process parameter variations (current density and applied magnetic field) are also presented and discussed in this paper.

Currently, there are two major approaches to synthesize 1D nanostructures, namely, “bottom-up” and “top-down” approaches. In the “bottom-up” approach, the formation of 1D nanostructures are via crystallization, where the evolution of a solid from a vapor, liquid, or solid phase involves two fundamental steps of nucleation and growth. As the concentration of the building units (atoms, ions, or molecules) of a solid becomes sufficiently high, they aggregate into small nuclei or clusters through homogeneous nucleation. Thus, with a continuous supply of the building blocks, these nuclei will serve as seeds for further growth to form larger nanostructures. In comparison, in “top-down” approach, the formation of the 1D nanostructures are from the attrition of the bulk material to nanometer sized 1D structures using techniques such as lithography [3], focused ion beam [4], or electrospinning [5]. Xia et al. [2] in their review article have discussed quite extensively both these approaches and identified the six strategies to synthesis 1D nanostructures. The six strategies are divided into two groups, with the first five strategies falling under “bottom-up” approach and the last one is the “top-down” approach. The six nanostructure synthesis strategies identified are: (1) growth dictated by anisotropic crystallographic structure of solid, (2) growth confined by liquid droplet as in the vapor–liquid–solid process, (3) growth directed through the use of template, (4) growth kinetically controlled provided by capping reagent, (5) growth through self-assembly of 0D nanostructures, and (6) size reduction of a 1D microstructure [2].

Out of the six strategies mentioned above, the growth-directed process through the use of template is one of the simplest and preferred strategies to produce 1D nanostructures. This method is relatively straightforward as the template serves as a scaffold within or around which a different material can be generated in situ, and shaped into a 1D nanostructure with the morphology complementary to the template used [2]. Among the different template synthesis strategies, the most successful methods are the step edges [6], channels in porous material [7,8], self-assembled molecular structures [9], and templating against existing nanostructures [10]. The synthesis of 1D nanostructures inside the channel of porous materials were pioneered by Huczko, Martin, and several others [7,8]. In this method, the porous material (template) serves as a scaffold in which the desired 1D nanostructures are deposited in situ inside the channel. The different porous templates that have been employed in the past include anodized alumina oxide (AAO) [8,11], radiation track etch polymer membrane (Polycarbonate) [8], nanochannel glass [12], mica [13], mesoporous silica [14], and block copolymers [15]. As shown in Fig. 1, the mechanism of filling the template can be performed using techniques such as electrodeposition [16], sol–gel [17], chemical vapor deposition [18], and pressure injection method [19]. In all of these cases, the 1D nanostructure shape, structure, and morphology is complementary of the template. In addition, the properties of these nanostructures are also directly related to the template properties such as channel dimensions, relative channel orientation, channel size distribution, and channel surface roughness. These methods are known for their simplicity, high-throughput, and cost effectiveness, which allows for complex topology present on surface of the template to be formed in single additive step. The major drawback of these methods especially electrodeposition is that the 1D nanostructures are usually polycrystalline and the quantities produced in each run is limited [2]. It is also worth mentioning here that it is possible to synthesize single-crystalline 1D nanostructures using template method by employing tight process control [20].

As stated earlier, in this paper, we investigate the structure and morphology of Ni nanowires synthesized under varying processing conditions. Ni nanowires are of interest because of their potential applications as high-density data storage and in magnetic sensors [16]. To date, a number of synthesis and characterization methods have been employed to study Ni nanowires. Specifically, the effect of electrodeposition process parameters such as solution pH, bath temperatures, current and additives on the growth and morphology of the Ni nanowires has been investigated [21-24].

In an electrodeposition process, crystallization of electrodeposited metal is influenced not only by the composition and concentration of the electrolyte but also by the operating conditions such as current density, temperature, electrolyte pH, and agitation. The effect of current density on the structure of the electrodeposit is particularly significant as it principally changes the cathodic potential. In general, the current density over a cathode will vary from point to point during electrodeposition. The current tends to be low in recesses, vias, and cavities and high on protruding points depending on the current travel distance, which in turn determine the quality of the final electrodeposit [25]. In addition, the electrodeposition process is a mass-transport limited process. Application of an external magnetic field during electrodeposition can increase this mass transport and thus change the properties of the electrodeposited layers. It is generally accepted that the primary influence of an external magnetic field is due to the Lorentz force that acts on the moving electrolyte ions. As suggested by Tabakovic et al. [26] and later verified by Aravamudhan et al. [21], this force induces a convective flow of the electrolyte near the template surface. This effect on the electrodeposition process is known as the magnetohydrodynamic (MHD) effect. This process in turn causes a decrease in the thickness of the diffusion layer and therefore an increase in the mass-transport of active species (ions). In order to control the properties of the electrodeposit, it is important to understand the effect of external magnetic field during the electrochemical processes. In previous works, external magnetic fields have been applied during the synthesis process to control structural and magnetic properties of 1D nanostructures [21,22]. It has been observed that external magnetic field can induce changes in surface morphology and preferential growth direction in case of Ni or Ni–Fe grains [21,27]. However, the influence of external magnetic field, along with the electric field (current density) and their coupled effect on the morphology, crystallographic orientation, and crystal size are yet to be studied in detail. In this paper, we will investigate the effect of external magnetic field, electric field (current density) and their combined effect on the morphology, crystallographic orientation, and grain size of Ni nanowires embedded inside the nanochannels of anodic alumina oxide (AAO) membrane.

In this present work, 1D Nickel (Ni) nanowire arrays were prepared by electrodeposition of Ni ions into the pores of Anopore® alumina oxide (AAO) membranes with a pore diameter of 200 nm (Whatman, Germany). The alumina membranes were thoroughly cleaned with de-ionized water and dried prior to use. A film of aluminum with approximate thickness around 100 nm was deposited on one side of the membrane (using Kurt J. Lesker, PVD 75) to serve as the working electrode. This was followed by the electrodeposition of Ni into the template from a sulfamate-based electrolyte bath using the commercially available pre-prepared solution (SN-10). A magnet with known magnetic field intensity was placed close to the template (with magnetic field parallel to nanowire growth) during deposition process. As the stoichiometry of the Ni nanowires are significantly affected by current density, solution pH, agitation conditions, temperature, external magnetic field, solution additives, and deposition time, all the parameters were maintained constant during the synthesis except for the external magnetic field and current density. Table 1 lists the deposition parameters used in the present work. All electrodeposition was carried out for 3 h at a temperature of 25  °C. After the electrodeposition process, the alumina membrane was cleaned with de-ionized water and then dissolved in NaOH to obtain freestanding Ni nanowires.

The structure and morphology of the grown Ni nanowires were analyzed using an HIM (Carl Zeiss Orion Plus) and SEM (Carl Zeiss Auriga). HIM is a relatively new imaging technology based on a helium ion beam. This technique has several advantages over the traditional SEM. In particular, the HIM has very high scanning resolution compared to SEM. HIM with a very high source brightness and short De Broglie wavelength, produces images with significantly higher resolution and qualitative data than a traditional SEM [28]. In addition, the conventional SEM suffers from several performance limitations, specifically, under many circumstances the image resolution are limited by sample interaction volume rather than the actual focused spot size, which degrades the image resolution. The HIM does not suffer from this effect as the excitation volumes are much smaller than that of the SEM [29]. Thus, HIM can be effective for morphological study with enhanced precision and resolution compared to SEM. Furthermore, very limited prior works currently exist on the HIM morphological study of 1D nanostructures. The energy dispersive spectroscopy (EDS, Oxford Instruments) was used to investigate the composition of the grown nanowires. XRD was used to determine the crystallographic structure of the electrodeposited Ni nanowires. The XRD was performed using Rigaku Smartlab X-ray Diffractometer with a monochromatized Cu Kα (λ = 15.4 nm) in a grazing incident arrangement. In subsequent sections, the morphology, composition, and crystallographic characteristics of the synthesized Nickel nanowires under varying process conditions are presented.

HIM and SEM.

Carl Zeiss Orion Plus HIM and Carl Zeiss Auriga SEM were used to image the synthesized Nickel nanowires. The goal was to study the structure and morphology of Ni nanowires synthesized at two different current densities with/without two different external magnetic fields. Figures 2 and 3 show the HIM and SEM images of grown Ni nanowires with and without external magnetic field at the two current densities of 5 mA·cm−2 and 11 mA·cm−2. The HIM and SEM images are shown side by side. Figures 2(a) and 2(b) show the HIM and SEM images of the synthesized Ni nanowires electrodeposited at a current density of 5 mA·cm−2 and magnetic field of 0G (Gauss). The HIM and SEM images at the same current density and magnetic field of 3817G are shown in Figs. 2(c) and 2(d), while Figs. 2(e) and 2(f) show HIM and SEM images at the magnetic field of 5756G. The corresponding HIM and SEM images for the current density of 11 mA·cm−2 and magnetic fields of 0G, 3817G, and 5756G are shown in Figs. 3(a)3(f).

Branched growth, wire breakage, and significantly different surface roughness were noticed on all synthesized Ni nanowires. The branched growth observed on the grown nanowires is primarily due to the morphology of the AAO template. The cross-sectional image of the AAO template, as shown in Fig. 4 clearly shows the pore branching, which subsequently results in nanowire branching during the electrodeposition process. The breakages of the nanowires are primarily attributed to the centrifugation process, which is used to clean and isolate the nanowires. Next, the surface roughness of the synthesized nanowires at different process conditions was compared using HIM and SEM. The surface characteristics of the synthesized nanowires due to the application of external magnetic field are clearly visible from the HIM images. At low current density and without any external magnetic field, a rough surface morphology with uneven nanowire growth is observed (Fig. 2(a)). With the application of an external magnetic field, the nanowire surface roughness is observed to have been quite significantly reduced. It is important to mention that it is because of the use of HIM imaging such higher resolution images and surface characterization data could be obtained. The helium ion beam is capable of producing 2–8 secondary electrons for each incoming helium ion, thus creating a better signal with higher contrast compared to high yield secondary electron in SEM [28,29]. The nanowires are also found to be straighter with the external magnetic field compared to no external magnetic field due to the compactness factor and uniformity of the obtained nanostructure. The comparison of the Nickel nanowire morphology presented in Figs. 2 and 3 also indicates that at a higher current density, the surface roughness is observed to be reduced even without the external magnetic field than at a lower current density. The nanowire surface is observed to become even more smoother, when both higher current density and magnetic field are applied, which is in agreement with prior work by Aravamudhan et al. [21] and Rabia et al. [30]. The enhancement of surface morphology, as shown in Figs. 2 and 3, is attributed to the increase in mass transport and decrease in diffusion layer thickness near the electrode/template surface due to the large Lorentz force also known as MHD [30,31].

The Ni nanowires deposited in AAO membrane were found to be 220 ± 30 nm in diameter. The diameter was found to be slightly larger than the template pore size due to the tendency of Ni to become oxidized. The average length of the grown nanowires was found to be 10 ± 5 μm.

EDS.

We also performed a quantitative EDS analysis to determine the elemental composition of the Ni nanowires by randomly dispersing them on a SEM sample holder. The results are summarized in Table 2. The EDS analysis demonstrated that the nanowires were composed of primarily Nickel with weight percentage above 85% for all the samples. A small percentage of oxygen is seen on the spectra indicating the existence of thin oxide layer on the Nickel nanowires. The presence of carbon on the spectra can be attributed to the carbon tape placed on the SEM holder.

XRD.

XRD based on grazing incident [32] technique (Rigaku Smartlab X-ray Diffractometer) was used to study the crystal structure and preferred orientation of the Ni crystals at different process conditions. The XRD analysis was performed prior to dissolving the AAO membrane with NaOH. In this analysis, the AAO membrane with pores filled with Ni nanowires were treated as a thin film to obtain the XRD spectra. The obtained XRD spectra were normalized and the instrumental error was subtracted to compare the results. Figs. 5(a) and 5(b) show the presence of multiple XRD peaks, which suggests that the grown nanowires are polycrystalline in nature. This indeed is an attribute of template-based synthesis method. Significant differences in the Ni crystalline structure are observed from the XRD spectra due to the incorporation of magnetic field and current intensity variations during synthesis. Fig. 5(a) presents the superimposed XRD spectra obtained for the electrodeposition of Ni on the AAO membrane at 5 mA·cm−2 current density and different magnetic fields–0G (solid line), 3817G (dashed line), and 5756G (dotted line). In the absence of magnetic field during synthesis, a strong peak of (1 1 1) Ni plane with other lower peaks of (2 0 0) and (2 2 0) Ni were observed. A preferred crystal orientation at (1 1 1), along with other peaks indicates the polycrystalline nature of the synthesized 1D Nickel nanowires. In comparison, when an external magnetic field was applied, the Ni crystal with (2 0 0) plane becomes more dominant instead of the (1 1 1) plane. This clearly indicates that there are changes in the crystal structure of the grown Nickel nanowires in the presence of external magnetic field. In addition, the HIM images (Figs. 2 and 3) also show significant morphological differences with and without the applied magnetic field.

Figure 5(b) presents the superimposed XRD spectra obtained for electrodeposition of Ni in the AAO membrane at a higher current density of 11 mA·cm−2 and external magnetic fields–0G (solid line), 3817G (dashed line), and 5756G (dotted line). In the absence of external magnetic field, a strong peak of (1 1 1) Ni plane with other lower peaks of (2 0 0) and (2 2 0) was observed. In comparison, when an external magnetic field was applied, the crystal orientation at (2 0 0) and (2 2 0) planes was found to have decreased further than with no external magnetic field. This observation may suggest that the crystals preferred orientation is along (1 1 1) direction at high current density and magnetic field, which is different than what was observed at lower current density, suggesting that the magnetic field may have a lesser dominant effect compared to the current density. This effect can also be observed from HIM and SEM images (Figs. 2 and 3), where the nanowire morphology at higher current density is vastly improved even without an external magnetic field. These observations may need further detailed analysis including investigations using TEM and selected area electron diffraction (SAED).

We further analyzed the XRD data to determine the crystal size of each sample using Scherrer equation shown in Eq. (1); Ref. [32]. The result of these calculations is summarized in Table 3. Table 3 indicates that the crystal size increases as the current density increases and with a higher magnetic field. The measured standard deviation of the crystal size is very small which signifies the measured crystal size is precise.

This observation may due to enhanced nucleation of active species during the electrodeposition caused by combined effect of increased current density and applied magnetic field. The observed change in crystal size verifies that the application of magnetic field enhances the convective flow and its ionic mass transport near the template. The enhancement of mass transport also affects the deposition rate and reduces the diffusion controlling process. Since the diffusion processes control grain growth, a different model of grain growth is expected when a magnetic field is imposed during electrodeposition [33]. This model of grain growth with magnetic field may have resulted in increased crystal size. In our future efforts, we will study the mechanical and magnetic properties of the Ni nanowires synthesized under the above-mentioned varying process conditions.

We have presented in this paper our findings on the morphological, crystallographic properties and crystal size changes of Ni nanowires as a function of (a) current density (5 mA·cm−2 and 11 mA·cm−2) and (b) applied magnetic field intensity (0G, 3817G, and 5756G). Both these process parameters have been found to influence the surface roughness, crystal orientation and crystal size of the electrodeposited Ni nanowires. The morphology of the nanowires showed significant improvement, from rough wall surface to smoother surface as the current density and magnetic field are increased. HIM was found to provide clearer and better picture of the morphological changes when compared to SEM images. We also found that the preferred orientation of Ni crystals changes due to the application of external magnetic field. In addition, variation in the current density and magnetic field also influenced the crystallite size. The morphological and crystallographic structure changes may largely be attributed to the MHD phenomena, which in turn causes an increase in ionic mass transport and decrease in diffusion layer thickness near the electrode or template surface.

We would like to thank the Joint School of Nanoscience and Nanoengineering, North Carolina A&T State University and Analytical Instrumentation Facility, North Carolina State University for the use of XRD facility. This work was supported by Joint School of Nanoscience and Nanoengineering (JSNN), North Carolina A&T State University and Universiti Malaysia Pahang, Ministry of Education, Malaysia. Financial support in part from Office of Naval Research is also acknowledged.

 

 Nomenclature
  • AAO =

    anodic alumina oxide

  • FWHM =

    full width half maximum

  • HIM =

    helium ion microscope

  • MHD =

    magnetohydrodynamic

  • SAED =

    selected area electron diffraction

  • SEM =

    scanning electron microscope

  • TEM =

    transmission electron microscope

  • XRD =

    X-ray diffraction

  • 1D =

    one-dimensional

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References

Chen, J., Wiley, B. J., and Xia, Y., 2007, “One-Dimensional Nanostructures of Metals: Large-Scale Synthesis and Some Potential Applications,” Langmuir, 23(8), pp. 4120–4129. [CrossRef] [PubMed]
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Figures

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Fig. 1

Processing flow for template-based synthesis

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Fig. 2

HIM (left) and SEM (right) images of nanowires grown at current density 5 mA·cm−2 and external magnetic field of, (a) and (b) 0G, (c) and (d) 3817G, and (e) and (f) 5756G

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Fig. 3

HIM (left) and SEM (right) images nanowires grown at current density 11 mA·cm−2 and external magnetic field of, (a) and (b) 0G, (c) and (d) 3817G, and (e) and (f) 5756G

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Fig. 4

Cross section of AAO template

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Fig. 5

XRD pattern of the Ni nanowires deposited in alumina membranes at various magnetic field and current density, (a) 5 mA·cm−2 and (b) 11 mA·cm−2 (in both Figs. 5(a) and 5(b)), solid line indicates for 0G, dashed line indicates for 3817G and dotted line for 5756G magnetic field

Tables

Table Grahic Jump Location
Table 1 Deposition process parameters during synthesis
Table Grahic Jump Location
Table 2 Average EDS elemental composition of Ni nanowires
Table Grahic Jump Location
Table 3 Crystal size calculation of deposited Ni nanowires at various growth conditions

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