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Article

Impact of Micro- and Nanocellulose Coating on Properties of Wool Fabric by Using Solution Blow Spinning

by
Yi Zhang
,
Abu Naser Md Ahsanul Haque
and
Maryam Naebe
*
Institute for Frontier Materials, Deakin University, 75 Pigdons Road, Geelong, VIC 3216, Australia
*
Author to whom correspondence should be addressed.
Fibers 2024, 12(12), 107; https://doi.org/10.3390/fib12120107
Submission received: 16 October 2024 / Revised: 21 November 2024 / Accepted: 2 December 2024 / Published: 5 December 2024
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Abstract

:
This study investigates the impact of micro- and nanocellulose coatings on the properties of wool fabrics using the solution blow spinning technique. The objective is to assess how varying cellulose sizes influence key fabric attributes, including physical properties, UV-shielding ability, air permeability and water vapour permeability, with a focus on their practical applications. Coating with microcrystalline cellulose (MCC) was found to increase the air permeability of fabric significantly, whereas coating with cellulose nanocrystals (CNCs) enhanced water vapour permeability and reduced pore size. The air permeability could relate to the breathability, and water vapour permeability could relate to the comfortability. Coated fabric with both sizes of cellulose could have different applications, like pollen filtration and printable cloth, and further functionality could be achieved by modifying the cellulose structure. This research establishes a platform for the effective application of cellulose coatings on wool fabric, offering promising advancements for textile performance and sustainability.

1. Introduction

Textile coating is an increasingly expanding area that has gained significant research interest in the recent past. Different coatings can achieve varied functionalities on textile substrates, such as fire retardancy [1], UV-shielding ability [2] and self-cleaning [3], which depend on their usage. Manufacturing of textile coating products is also observing an increasing trend. In 2023, the global textile coatings market was valued at approximately USD 4.19 billion, with expectations to grow at a compound annual growth rate (CAGR) of 4.3% from 2024 to 2030 [4].
Currently, the most effective coating materials used are thermoplastics, such as polyurethane, polyvinyl chloride (PVC), acrylics, nylon, polyolefins, etc. [5]. However, all these materials either need hazardous solvents (such as DMF) in the fabrication process or create problems after application [6]. For example, the coating by synthetic plastics will cause the release of microplastics [7]. In this regard, bio-based sustainable materials are more desirable to replace the thermoplastic polymers in the textile coating.
Cellulose is a plant-based material and usually is biocompatible, nontoxic and biodegradable. Nanocellulose has already been accepted as a coating material for fabrics as it could enhance the mechanical and other functional properties, such as anti-UV, antibacterial and resistance to degradation [8,9]. Cellulose, including micro- and nanocellulose, e.g., cellulose nanocrystals (CNCs), has abundant hydroxyl groups, which are favourable for chemical modification, making them ideal for achieving varied functionalities [9,10,11,12]. Several techniques have been employed to modify CNCs, such as atom transfer radical polymerisation, reversible addition–fragmentation chain transfer, ring-opening polymerisation and nitroxide-mediated polymerisation, resulting in a range of functionalities suitable for textiles [13]. CNCs have been used to coat synthetic fabrics, such as polyester and polyamide, to understand the adhesion between the structure of CNCs and the polymers. The result shows that the coating by CNCs can increase the strength of the fabric and reduce the water and air permeability [14]. CNCs have also been used to coat fabrics made from natural fibres, such as cotton [15] and silk [16]. For example, Fan et al. [17] modified CNCs with copper ions and applied them on cotton fabric, achieving 99.9% bacterial resistance. Though CNCs have a lot of advantages, microcrystalline cellulose (MCC) is also attractive as it could require lower energy and chemical use in the manufacturing process compared to CNCs [18]. Also, with its large size, the cellulose particle could easily form a film on the surface of fabrics.
For the consideration of the fabric to be coated, wool contains approximately 97% keratin, a fibrous protein, which can form physical bonds with cellulose [19,20]. The unique structure of wool is different from other fibres, such as cotton or polyester, but interaction with cellulose has the potential to alter fabric properties, such as water vapour transmission and porosity, and could be beneficial in the moisture management [21]. Though there are few studies on the coating of cotton and polyester with nanocellulose and chitosan [22], there is no study based on the micro- or nanocellulose coating of wool fabric.
In this paper, we provided a controllable coating method for the wool fabric by using micro- and nano-sized cellulose. The adhesions between cellulose and wool fabric have been studied. We chose the solution blow spinning (SBS) method as a technique to coat wool, since this is rapid and efficient and an increasingly popular technique for fabricating nanofibres. SBS works by spraying a polymer solution through a small nozzle, with the help of high-velocity air or gas, and the fibres are formed as the solvent evaporates. This is contactless and can produce a uniform coating layer by controlling its parameters, such as spray pressure, distance of spray and spray solution. Polyvinyl alcohol (PVA) and resin were added as glue to increase the adhesion of the cellulose and wool. The properties of the coated fabric were analysed, which provides an essential platform for the further modification of cellulose particles to achieve specific functions on the fabric.

2. Materials and Methods

2.1. Materials

Microcrystalline cellulose (product number 435236, particle size 51 μm, bulk density = 0.6 g/mL (25 °C)), Polyvinyl alcohol (PVA), Mw 89,000–98,000, 99+% hydrolysed, were purchased from Sigma-Aldrich, Castle Hill, NSW, Australia. Acetone, 98% sulfuric acid and sodium hydroxide (Pellet, AR grade) were purchased from Chem-Supply, Gillman, SA, Australia. EpoFix resin and hardener were purchased from Struers, Ballerup, Demark. Wool fabrics were obtained from Commonwealth Scientific and Industrial Research Organisation (CSIRO), Melbourne, VIC, Australia, featuring a 126 g/m2, with 18 ends/cm and 20 picks/cm, made from wool fibres with an average diameter of 19 µm.

2.2. Preparation of CNCs, PVA Solution and Spray Solution

To compare the influence of the size of cellulose on the sprayed coating, MCC and CNCs were used as the reinforcing materials in the spray solution. CNCs were fabricated following a standard fabrication method from Dong et al. [23]. A total of 4.4 g of MCC was added into a 62.5 mL 64 wt% sulfuric acid solution and kept in a round bottle flask at 45 °C for 1 h. The reaction was stopped by adding 10-fold water. The final solution was centrifuged for 15 min at 7000× g at room temperature and washed with DI water several times. The solution was further neutralised by adding NaOH solution until the pH reached 7.
To understand the impact of different concentrations on spray coating, the amount of PVA was kept constant for each solution. A total of 6.6 g PVA was dissolved in water with different concentrations (1%, 3%, 5%, 10%, 15% and 20%) of either MCC or CNCs by adding different weight amounts of water at the temperature of 90 °C for at least 8 h. The spray solution was a mixture of 4.4 g microcrystalline cellulose (or cellulose nanocrystals), 6.6 g PVA solution (different water amount), 38.4 g acetone and 0.6 g resin. The sample component information is shown in Table 1.

2.3. Spray Solution on Wool Fabric

A blue-coloured woven wool fabric was first cut into a square of 10 cm × 10 cm. Dark-coloured fabric was chosen for a strong contrast between the fabric and the spray solution (white). The gravity feed spray gun with a nozzle size of 1.4 mm was purchased from Supercheap Auto, Waurn Ponds, Australia. The air compressor (Dynamic Power HB-AS186 1/6HP, 20–23 L/min) provided the compressed air to the spray gun. The distance from the nozzle to the fabric was optimised at 60 cm. Each fabric was sprayed with a controlled weight of the spray solution, as shown in Figure 1, and the detailed information is listed in Table 1. For the MCC, we compared two different concentrations of 5% and 10%, while for CNCs, the same spray solution was used but with a difference in the spray amount.

2.4. Characterisations

The fabric thickness was tested by Absolute Digimatic Indicator (Mitutoyo mode ID-C1012; Kawasaki, Japan) with the pressure of 0.5 kPa, each sample having 5 repeats.
The morphology of the fabrics was captured using FEI Quanta 3D FEG FIB-SEM (FEI Company, Hillsboro, OR, USA), while the fabric surfaces were coated with Pt before imaging.
The pore size of the fabrics was tested by using a Quantachrome porometer instrument (3GZH; Quantachrome Instruments, Boynton Beach, FL, USA). The fabrics were first made wet by a Porofil liquid. Nitrogen gas (pressurised) was used to force the wetting Porofil liquid through the analysed fabrics.
The ultraviolet protection factor (UPF) was tested by using a YG902 UPF spectrophotometer based on the EN 13758-2 standard [24]. The samples were stored in ambient conditions at a temperature of 20 °C under regular white, fluorescent light for 2 years and retested to understand the coating durability.
The air permeability of fabric was tested by using a Textile Air Permeability Tester according to the ASTM D737 [25]. Briefly, the test area was 38 cm2 and the test pressure was 125 Pa. Each sample was tested 5 times at different places on the fabric samples.
The water permeability of the fabric was tested by a Labthink Water Vapor Transmission Rate Tester (Labthink, Jinan, China) at 20 °C and 65% humidity as per ASTM E96 [26].

3. Results

3.1. The Properties of Spray-Coated Fabric

The thickness of the fabric is listed in Table 2. The thickness could indicate the change due to the solid amount added from the spray solution. For both sprayed samples with the MCC, the thickness was higher than other sprayed fabrics, i.e., control and nanocellulose-coated fabrics. CNC-sprayed samples showed a predictably lower thickness due to their minor sizes compared to microparticles. In fact, CNCs and resin showed similar contributions to the fabric thickness. The 5% CNC/PVA thickness showed a positive correlation between the weight of the spray solution and the sprayed fabric’s thickness. Since the thickness of the fabric is important for both the air and water permeability measurements, they were further used in those calculations.

3.2. The Morphology of the Sprayed Fabric

The digital images of the sprayed fabric are shown in Figure 2. As the spray solution was white, the fabric’s white dots were recognised as the dried sprayed particles. It can be observed that the white dots were distributed uniformly on the fabric surface (5-MCP and 10-MCP). Both resin and PVA were not observable due to their transparency. For the different ratios of CNC/PVA samples, it was expected that the white dots would increase with the spray amount (from 1 g to 10 g). However, the CP10-sprayed fabric showed fewer white dots than the CP5-sprayed fabric. This indicates the possibility of reaching the limit of spraying, as the additional CNCs leached out. It could also be evident from the thickness of the coating layer (Table 2), which was not doubled by a two-times amount of spray solution. This appearance was also similar to the CNC control sample (CC), which comprised a similar combination except for the inclusion of resin and PVA, which darken the appearance of CP10. The sprayed solution also changed the handle property, as CP5 was found more flexible and softer than CP10. This phenomenon was not observed in MCC-integrated samples. MCC had a large particle size, and, after combining with PVA and resin, the particle could not go through the fabric’s inner structure.
The SEM images of the fabric are shown in Figure 3. The WF sample showed the woven structure of wool fabric, while some resin particles were visible with the wool fibres in RC. The sprayed particles were visible in 5-MCP and 10-MCP with the micro-sized cellulose. The MCC could form the core, and the resin and PVA were wrapped outside the MCC, resulting in a large particle as the MCC could establish strong interfacial interaction with PVA through hydrogen bonding [27]. It was also confirmed that the MCC particle was attached to the fabric surface rather than occupied inside it. From the CC sample, CNCs and resin were visible on the wool fibre surface, and these particles were much smaller than those of the MCC (5-MCP and 10-MCP). With the smaller size, the cellulose nanocrystals could stick to the fabric more like a film, as perceived in the SEM images of CNC-coated fabrics, particularly CP5 and CP10. Some pores were found in both samples. The wider size of pores was found in CP10 compared with CP5, indicating the possibility of greater penetrability. These pores could influence the air and water vapour permeability of the sprayed fabric, which are discussed in the following sections.

3.3. FTIR Spectrum of the Spared Fabric

The FTIR characterisation was used to understand how the spray solution changed the fabric structure, and the spectra are shown in Figure 4. The spectrum in the broad peak around 3280 cm−1 is assigned to the H-bonded O-H group stretching vibrations [28] rich in cellulose, resin, PVA and wool. The sample containing CNCs has a side peak around 3338 cm−1, which is related to O-H hydrogen bonding [29]. All the samples have a peak at 3069 cm−1, which could be from the O-H group from the wool structure [30]. A difference in the spectrum of CNC/PVA samples was observed; the peak at 2964 cm−1 was gradually transferred to 2942 cm−1, especially with the increase of the CNC/PVA amount. The peak at 2967 cm−1 represents the C-H stretching vibrations in C-H3, and the peak at 2942 cm−1 represents the C-H stretching vibrations in C-H2. This could be the stretching vibration from the wool fabric, as it also has this peak, and, with the additional coating amount, this feature has been covered by the coating layer feature. All samples containing PVA showed a peak at 1739 cm−1, which is related to the –C=O bonding from the PVA [31]. Interestingly, there is another peak at 1714 cm−1, observed from CP5, indicating the forming of ester bonds [32]. The peak around 1232-1242 cm−1 represents the asymmetric C–O–C stretching, which is found in all the samples [33]. The peak at 1060 cm−1, observed from CP10, represents the asymmetric bending vibration of the C–O–C ether bond from the pyranose rings in polysaccharide [34] which is from the cellulose structure. This peak is also found in CP5, CP10 and CC. By coating with more spray solution, the feature of the coating is found similar to the cellulose coating.

3.4. Pore Size of the Sprayed Fabric

To understand the coating’s influence on the permeability, the pore size of different fabrics was tested. It can be perceived from Figure 5 that the inclusion of MCC does not have much effect on the pore size, with the addition rate of 5%. However, with the increase of MCC to 10%, the pore size increased. As shown on the morphology part of the fabric, MCC formed thin white dots on the surface of the wool fabric, which increased the thickness of the fabric. The large gap between these white dots contributed to the large pore size. With a lower amount of CNCs, the layer was thin, which had not much influence on the pore size (28 µm). But when the amount was higher, it formed a thicker layer, which increased the thickness of the fabric (826 µm), leading to the increase of the pore size of the coated fabric. However, both resin and CNC coating could reduce the pore size of fabric. From the CP1 and CP5 samples, we found the pore size was reduced as expected. The cellulose nanocrystals could fill the gap in the fabric, which led to the reduction of pore size. Nevertheless, for the CP10 fabric, the pore size was increased. This could be due to the coating amount reaching the limit and being unable to maintain the coating structure with white dots. It is also related to the testing method, as we added liquid and measured the accessibility of these liquids. More CNC coating would increase the hydrophilicity of the fabric, and the liquid would be easier to access. The reduced pore size by CNCs, particularly in the CP5 fabric (28 µm), could provide functional benefits. For example, if such fabric was used as a mask, it could filter out larger pollen grains, such as cherry pollen (35 um) and pine pollen (45–85 um), thereby decreasing the likelihood of hay fever symptoms caused by these allergens.

3.5. UV-Shielding Properties of the Spray-Coated Fabric

The UV-shielding ability of the spray-coated fabric is shown in Figure 6a. The Ultraviolet Protection Factor (UPF) measures the amount of UV radiation, including UVB and UVA rays, that a fabric allows to penetrate human skin. The raw wool fabric showed a good UV-shielding ability, and adding the extra coating could influence its UV-shielding capability. The UPF number of wool fabrics is found to be 171, which shows ‘excellent’ UV-shielding protection according to EN 13758-2 (a UPF number over 40 is considered ‘excellent’). Though the additional coating influenced the UPF number, all the fabrics achieved the ‘excellent’ grades. The UPF of fabric is also related to the pore size of the fabric. With larger pore size, the UPF number is lower, which refers to the lower UV-shielding ability, as larger pore size comprises more tunnels that can let UV light pass through. To investigate the durability or aging of the coating, the UPF values of the samples were also tested after 2 years. No significant difference was observed between the UPF values over the 2 years, indicating the coating layers were quite stable under the general condition. Figure 6b shows the transmission rate of UV light in the UVA and UVB ranges. The transmission of RC, CC, CP1 and CP5 in the UVA and UVB ranges is similar to the wool fabric. The transmission of CP10 is higher due to the larger pore size of the fabric. Both fabrics containing MCC have higher transmission rates, which is consistent with the UPF result.

3.6. Air Permeability of the Spray-Coated Fabric

The air permeability of the spray-coated fabric is shown in Figure 7a. An air permeability of 5–25 cm3/cm2/s is considered ideal for Outdoor Gear [35,36]. An air permeability from 1 to 20 cm3/cm2/s could be used for medical textiles and the air permeability from 5 to 20 cm3/cm2/s is ideal for home textiles [36]. The air permeability of the tested fabrics was in these ranges, which indicates the widespread application of these fabrics. It also confirmed that these fabrics were breathable and comfortable. The data in Figure 7a show the total air permeabilities of the spray-coated fabric while the thickness of the spray-coated fabric is different. The air permeability value of spray-coated fabric that is normalised by film thickness is shown in Figure 7b. There is no significant difference in the air permeability between 5-MCP, RC, CC, 10-MCP, CP1 and WF. However, CP5 and CP10 show significant differences from other samples. This result could relate to the spray-coated fabric structure. The lowest amount of air permeability, that of CP5, may result from its –C=O bonding, found at 1714 cm−1 (FTIR data). This boding could generate a more condensed structure, which would lead to the reduction of air permeability. After reaching the threshold, the added spray solution of CP10 is higher than CP5. The structure of CP10 is different from CP5, which could relate to the air permeability. With part of the CNC leaching out, most of it was PVA, which could lead to higher air permeability. This could also be confirmed by the FTIR result, as the peak at 1714 cm−1 was only found in CP5. Moreover, as observed from the digital and SEM images, the structures of CP5 and CP10 are different. The higher air permeability could be beneficial to the comfortability of the fabric.

3.7. Water Vapour Permeability of the Spray-Coated Fabric

The water vapour transmission ability of spray-coated fabric is shown in Figure 8a. The water vapour transmission ability is related to the moisture, which relates to the breathability of the fabric. There is not much difference in the water vapour transmission in the samples, as this figure does not consider the fabric thickness in the calculation. The water vapour permeability shown in Figure 8b considers the thickness of the fabric. As shown in Figure 8b, the water vapour permeability of CP10 was much higher than CP5 and CP1. This could be related to the hydrophilic nature of PVA and CNC solutions. Both samples containing MCC show a higher water vapour permeability than most of the samples. This could be due to the better interaction of cellulose with water. This also explains why the water vapour permeability of 10-MCP is higher than 5-MCP, as it contains a higher MCC amount. With the same 5% amount, the water permeability of CP10 is higher than that of 5-MCP. This could be due to the smaller size and larger surface area of CNCs compared to MCC. Thus, there could be more chances of interaction with water, resulting in a higher water vapour permeability.

4. Conclusions

In summary, this study investigated the influence of micro- and nanocellulose coatings on the properties of wool fabric through the solution blow spinning technique. The UV-shielding ability, air permeability and water vapour permeability were tested to understand the barrier properties of the fabric. The coating of the fabric did not influence the UV-shielding ability of wool fabric, and all the fabrics showed excellent UV-shielding ability. For the pore size of the fabric, CP5 (5% CNC/PVA 5 g) reached the lowest air permeability compared with CP1 (5% CNC/PVA 1 g) and CP10 (5% CNC/PVA 10 g). Though 10 g of 5% CNC/PVA was added for the CP10 sample, the pore size was not reduced, which could be due to the change in coating structure of the fabric. The lowest pore size, seen in CP5, could be beneficial for filtering larger pollen grains with comfortability, as shown by the water vapour permeability and air permeability of the fabric. Another application of coated fabric could be a printing option for fabric, as both MCC and CNCs could appear white colour in certain concentrations and spray amounts. Overall, this research contributes valuable knowledge to the field of textile engineering by demonstrating the effectiveness of micro- and nanocellulose coatings in enhancing wool fabric properties.

Author Contributions

Conceptualization, M.N. and Y.Z.; methodology, Y.Z.; formal analysis, Y.Z.; writing—original draft preparation, Y.Z.; writing—review and editing, Y.Z., A.N.M.A.H. and M.N.; visualisation, Y.Z. and A.N.M.A.H.; supervision, M.N. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Acknowledgments

The authors acknowledge the support from Deakin Advanced Characterisation Facility and Australian Research Council ITRH (IH210100023).

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Fabrication process of coated fabric.
Figure 1. Fabrication process of coated fabric.
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Figure 2. The digital images of raw and spray-coated wool fabrics. The details of sample names are provided in Table 1.
Figure 2. The digital images of raw and spray-coated wool fabrics. The details of sample names are provided in Table 1.
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Figure 3. SEM images of raw and spray-coated wool fabrics.
Figure 3. SEM images of raw and spray-coated wool fabrics.
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Figure 4. FTIR spectra of raw and spray-coated wool fabrics.
Figure 4. FTIR spectra of raw and spray-coated wool fabrics.
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Figure 5. The pore size of raw and spray-coated wool fabrics.
Figure 5. The pore size of raw and spray-coated wool fabrics.
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Figure 6. (a) UV-shielding ability; and (b) UVA/UVB shielding of raw and spray-coated wool fabrics.
Figure 6. (a) UV-shielding ability; and (b) UVA/UVB shielding of raw and spray-coated wool fabrics.
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Figure 7. (a) Air permeability of tested fabrics; and (b) Air permeability of tested fabrics normalised by fabric thickness.
Figure 7. (a) Air permeability of tested fabrics; and (b) Air permeability of tested fabrics normalised by fabric thickness.
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Figure 8. (a) Water vapour transmission rate; and (b) Water vapour permeability of raw and spray-coated wool fabrics.
Figure 8. (a) Water vapour transmission rate; and (b) Water vapour permeability of raw and spray-coated wool fabrics.
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Table 1. Sample names and their components.
Table 1. Sample names and their components.
Sample NameDescriptionSpray Solution ComponentSpray Solution Amount (g)Spray Distance (cm)Spray Pressure (psi)
PVA (g)Water (g)Resin (g)Acetone (g)MCC (g)CNCs
(g)
WFWool fabric00000006035
RC5% Resin control0125.40.638.500106035
5-MCP5% MCC/PVA6.6125.40.638.54.40106035
10-MCP10% MCC/PVA6.662.70.638.54.40106035
CC5% CNC control0125.4038.504.4106035
CP15% CNC/PVA 1g6.6125.40.638.504.416035
CP55% CNC/PVA 5 g6.6125.40.638.504.456035
CP105% CNC/PVA 10 g6.6125.40.638.504.4106035
Table 2. The thickness of fabric samples and their coating layers.
Table 2. The thickness of fabric samples and their coating layers.
Sample NameThickness (μm)Coating Layer Thickness (μm)Pressure for Thickness Measurement (kPa)
WF510.0 ± 10.0000.5
RC574.0 ± 5.48640.5
5-MCP722.0 ± 27.752120.5
10-MCP826.7 ± 61.86316.70.5
CC584.0 ± 8.94740.5
CP1538.0 ± 4.47280.5
CP5628.0 ± 13.041180.5
CP10690.0 ± 25.501800.5
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MDPI and ACS Style

Zhang, Y.; Haque, A.N.M.A.; Naebe, M. Impact of Micro- and Nanocellulose Coating on Properties of Wool Fabric by Using Solution Blow Spinning. Fibers 2024, 12, 107. https://doi.org/10.3390/fib12120107

AMA Style

Zhang Y, Haque ANMA, Naebe M. Impact of Micro- and Nanocellulose Coating on Properties of Wool Fabric by Using Solution Blow Spinning. Fibers. 2024; 12(12):107. https://doi.org/10.3390/fib12120107

Chicago/Turabian Style

Zhang, Yi, Abu Naser Md Ahsanul Haque, and Maryam Naebe. 2024. "Impact of Micro- and Nanocellulose Coating on Properties of Wool Fabric by Using Solution Blow Spinning" Fibers 12, no. 12: 107. https://doi.org/10.3390/fib12120107

APA Style

Zhang, Y., Haque, A. N. M. A., & Naebe, M. (2024). Impact of Micro- and Nanocellulose Coating on Properties of Wool Fabric by Using Solution Blow Spinning. Fibers, 12(12), 107. https://doi.org/10.3390/fib12120107

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