Effect of Surface Modification of Himalayan Nettle Fiber and Characterization of the Morphology, Physical and Mechanical Properties

2.1 Materials

The nettle grows in the Himalayan region of Nagaland (250-39′-47″ N, 940-38′-09″ E). The nettle plant is harvested from October to December, and it grows more than 3 meters tall in a Himalayan area above 1500–2000m, as shown in Figure 1. The fibers are found in a wide ring in the external section of the stalk, divided by collenchyma cells rather than in bundles. By dry weight, the stem contains 3.5–13.2% fiber. The moisture content of nettle is 16%, cellulose 68.10%, hemicelluloses 14.12%, lignin 10.45%, and pectin and gum 6.02% [6].

Figure 1

Himalayan nettle plant

2.2 FTIR Spectra analysis

The FTIR spectrum of the nettle fiber samples was analyzed using the ABB Bomen MB3000 spectrophotometer, which is used to analyze hydrogen bonds, the structure of natural fiber, and the chemical composition of nettle fiber. The near contact between fiber samples and the attenuated total reflectance (ATR) crystal was constructed by using a pressure clamp. In the range of 4000–600cm⁻¹, all spectra were collected with 32 scans and 4cm⁻¹ resolution [1,2,3].

2.3 Physical and Mechanical properties of nettle fiber

The physical and mechanical characteristics of water and dew retted nettle fiber, such as fiber length, diameter, fineness, tenacity, tensile strength, Young's modulus (E), and elongation break % were measured using the standard textile testing instrument, Unistretch 250, and a micrometer microscope. The total length of the nettle fiber sample used for testing was 120mm [4, 5].

2.4 Scanning Electron Microscopy

The morphology and structure of water and dew retted nettle fibers samples were observed by field emission SEM (JEOL JSM 6390) and an accelerating voltage of 5 to 10KV. The high-quality nettle fiber SEM images were collected at different magnifications (100,000x). Prior to SEM inspection, the samples were placed on aluminum stubs with carbon tape and then sputter coated with platinum and palladium to make them conductive [6,7,8].

2.5 Bacterial treatment of Nettle fiber

The water retting method produces a uniform length of high-quality fiber. The dry nettle fiber samples are soaked in cold water for 7–14 days. The retting trials were carried out in 10-liter plastic tanks at a temperature of 35 °C. As shown in Figure 2, the water was changed with fresh cold water to remove dirt and impurities, one with bacterial inoculum and the other a control sample. Over retting weakens the fiber strength, while under retting makes fiber separation difficult. As a result, retting time maintenance is critical. At the start of the process, spores were added to water tanks. A total of 16 water-retted fiber samples were collected, 8 of them retted with bacterial inoculum that degrades the pectin and lignin and eight control samples. After that, nettle bark is peeled and dried for 48hrs. The bark was rinsed in running water and beat with a wooden mallet to remove impurities and soften the fibers for 2 hours [4,5,6].

Figure 2

Water retting method for nettle fiber extraction

2.6 Fungi effect of Nettle fiber extraction

The dew retted nettle stems were harvested and uniformly spread in the fields where fungus, sunlight, and atmospheric air and dew caused the stem's cellular tissues and sticky compounds that wrap the fibers to break. For the dew retting process and colonization of fungi, warm places and Cellulose, pectinase, and xylanases are recommended. These are prevalent in locations with limited water resources. As retting organisms, fungi penetration is thought to be the most important enzymatic activity. In dew retting, Rhizomucor pusillus and Fusarium lateritium stood out for their strong lignin degradation, ability to attack noncellulosic cells without harming any cellulose, ability to penetrate the round surface of the stem, and effective fiber release from the core [4, 9]. During this process, soil and phyllosphere microorganisms proliferate on the plants, resulting in partial stem tissue disintegration and improved fiber quality, as shown in Figure 3.

Figure 3

A) Dew retting B) Water retting nettle fiber

3.1 Chemical composition analysis

During water and dew retting process, bacterial and fungi formation degraded fiber lignin in the nettle fiber stems. The cellulose, hemicellulose, and lignin content in the raw nettle was 65.27%, 9.53% and 3.7% respectively. The degradation of lignin and hemicellulose was observed at 2.8% and 8.4% for bacterial method and 2.1% and 7.3% for dew process. The change in values reflects the increase in fiber softness and cellulose content 86.4% and 84% shown in Figure 4. Both bio-organisms improved the color and fineness of the fiber to their maximum ability in 30 days. There was no visible change in color until 30 days elapsed. The samples that incubated for 30 and 45 days showed no significant difference in lignin breakdown [10].

Figure 4

A) Cellulose (B) hemicellulose (C) Lignin (D) Physical properties

3.2 Physical and Mechanical Properties

The nettle fiber length was measured using a calibrated centimeter scale. The raw fiber length measured up to 250cm. After treatment, the fiber length measured 200cm for water retted fibers and 175cm for dew retted fibers. The microbial treatment methods could increase fiber fineness up to 58 dtex and reduce fiber diameter from 40 mm to 32 mm, as shown in Figure 5 (D). From Table.1, the tenacity of microbial treated nettle fiber decreased over raw nettle from 45.72 to 38.20 cN\tex. This reduction in tenacity could be related to the selective removal of lignin, which causes microfibril compaction and lowers the tensile strength of bio-softened nettle. Notice that from Table 1. The tensile strength and elongation breaks improved in treated nettle compared to raw nettle. The raw fiber had a 2.86% elongation, but the fiber treated with fungi had a 3.32% elongation, and the fiber treated with bacteria had a 3.80% elongation. As a result, softening did not degrade the fiber quality [12,13,14]. This enhancement in tensile properties is likely to improve fiber spinnability and strengthen nettle yarn's ability to withstand being woven.

Figure 5

FTIR spectrum analysis of Nettle fiber

3.3 FTIR analysis of treated nettle fiber

The hydroxyl (OH) form of cellulose, lignin, and hemicellulose had a strong peak observed between 3500–3300cm⁻¹ that is specific to compounds. The peak at 2878–2746cm⁻¹ was representative of the stretching vibration of CH found in cellulose and hemicellulose the band at 1620cm⁻¹ may be linked to the presence of water in the fibers. The peak at 1636cm⁻¹ was indicative of hemicellulose's carboxyl group [12].

The CH2 deformation vibrations in lignin and pectin symmetric bending of the cellulose are related to the absorption band at 1450cm⁻¹. The bending vibrations of the CH and CO vibration of the aromatic rings’ methyl and methylene groups in cellulose bands measured at 1273cm⁻¹ and 1196cm⁻¹, respectively. The CO and OH stretching vibrations of the polysaccharide in cellulose were related to the intense peak vibrations detected at 1026cm⁻¹. Finally, the creation of the glycosidic area is defined by the peak CH deformation in the cellulose bond structure between 895cm⁻¹ and 897cm⁻¹ [11,12,13].

3.4 SEM analysis of treated nettle fiber

The water and dew treated nettle fiber surface morphologies are shown in Figure 6. After biological treatment, the surface morphologies visibly changed. In comparison to raw nettle fibers, treated nettle fibers have a distinct degree of protrusion. The SEM figures show the nettle yarn's twisting mechanism at the breaking point is smooth. The presence of protrusions in treated nettle fibers contributes to the tensile characteristics by improving the mechanical connection between the fiber and the matrix during tensile loading [14]. A nettle fiber matrix, which is made up of hemicellulose, lignin, and pectin (which have various characteristics), becomes highly anisotropic. The existence of the gradient in the radial direction indicates that the anisotropy of the matrix may have imparted a twisting moment on the fibers.

Figure 6

SEM images of treated nettle fiber