Nano-Coating on Different Patterned and Unpatterned Light-Weight and Delicate Curtain and Lacy Fabrics; Multifunctional Features and Comparing ICP-OES and UV-vis Spectroscopy to Determine Washing Fastness

  

    
Sample code 
    
Fabric type 
    
Fabric texture 
    
Warp yarn 
    
Weft yarn 
    
Pattern yarn 
  
  

    
FL 
    
Fine lacy 
    
warp knitted 
    
multi-filament 
    
- 
  
  

    
CL 
    
Coarse lacy 
    
warp knitted 
    
multi-filament 
    
- 
  
  

    
SC 
    
Striped curtain 
    
woven 
    
mono-filament 
    
mono-filament 
    
intermingled 
  
  

    
TC 
    
Tiled curtain 
    
woven 
    
multi-filament 
    
mono-filament 
    
multi-filament 
  
  

    
LC 
    
Limbed curtain 
    
woven 
    
mono-filament 
    
mono-filament 
    
multi-filament 
  

Table 1: Raw samples structures.

Treating materials: Water-based nano-sized colloidal TiO₂ Aerodisp W 740X (40% TiO₂ P25 nano titanium dioxide in water and polysiloxane CT 208 E emulsion) were kindly provided by Evonik Degussa Corporation and Wacker Finish, respectively. Evaluating the particle size by zeta-sizer has confirmed the size of about 85.95 nm for TiO₂ nanoparticles [5].

Samples preparation: The cut samples were exposed to a prewash preparation to remove any impurities such as dust particles from their surfaces. A washing bath was prepared with 1g/L of a anionic detergent with a liquor-to-goods ratio (L:G) of 80:1 at 50°C. The samples were immersed in the bath for 20 minutes and rinsed completely. To ensure removing the excess detergent, the samples were rinsed twice more with distilled water at 50°C for 5 minutes.

Fabric treatment: The nano-sized colloidal TiO₂ and the polysiloxane emulsion were diluted using distilled water at an ambient temperature (25°C) to achieve a specific concentration. All the prewashed samples were immersed in the prepared bath (TiO₂) for 20 seconds and squeezed by a pad, down to a 100% wet pick-up. The padded samples were dried at 100°C in an oven for about 3 minutes.

A subsequent treatment bath was prepared with distilled water and a specific concentration of resin. All the pre-treated samples were treated in the same condition again but within a shorter immersion time (i.e. 3-5 seconds). An associated control sample treated with only XPs was also prepared. To facilitate reporting the results, all the samples were introduced by proper codes. The samples treated with both TiO₂ and XPs were subject to an after-wash process in the same conditions as mentioned for the pre-wash.

Test Methods

Water droplet absorption time

Water drops (10 microliter) were dropped from a distance of about 10 mm of the fabric surface, and its absorption time was recorded at a controlled temperature and relative humidity (20°C and 30%).

Water droplet contact angle

After releasing water drops on the sample surface, the droplet statue was examined by mean of a self-developed goniometer apparatus equipped with a high-resolution camera and a suitable lens [33] and the corresponding contact angles were measured manually by using MB-Ruler software.

Stain repellency

Stain repellency was evaluated according to the modified method AATCC 22 [32]. Stain drops of methylene blue (0.005%) were released on the samples at an angle of 45° with respect to the horizon. At the end, trace of stains on the samples was scanned and reported.

To quantify the results, another study was designed [34] and done. Accordingly, every sample was immersed into a methylene blue (0.005%) container lying on a vibrating plate (shaker) for 10 seconds at the rate of 60 rpm. The characteristics of color (L, a, b) were extracted by an X-rite Spectrophotometer. The color difference between before and after staining was calculated for each sample by the following well-known equation:

ΔE = [(L₂ – L₁)² + (a₂ – a₁)² + (b₂ – b₁)²] ^0.5

Washing fastness

Determination of titanium quantity, released in each wash, was considered as the most accurate measure of washing stability [32]. Washing test was done 20 times for every sample according to standard the AATCC 61(2A)-1996. Each sample was immerged in a washing solution (5 g/l of detergent with L: R=1:80) and shaken at 40°C for 40 minutes. Washing effluents of 1-5th and 6-20th with proper dilution factors were studied separately by ICP-OES (Perkin Elmer Plasma 400 Sequential ICP-OES Spectrometer) and a transmission spectrophotometer (UV mini-1240) in the ultraviolet region near visible (UV-vis.) through transition spectroscopy at λ_max= 318 nm. The released TiO₂ was calculated considering the dilution factors and calibration series. For FL samples, titanium quantity released in each wash was also determined by inductively coupled plasma spectrometry test ICP-OES, and the results compared to the data resulted UV-vis spectrometry.

Abrasion resistance test

This test was conducted according to the standard ASTM-D4966/ D4970 using Shirley Martindale Abrasion Tester. The number of rub cycles until the first break point was considered as the standard end point.

Sunlight resistance test

The abrasion resistance of the samples exposed to the sunlight was considered as the criterion of sunlight resistance [29] and was compared with the primary sample. For this purpose, the samples were exposed to the sunlight of Yazd city, Iran, for 100 and 160 hours in summer during several days and at certain times of the day (from 10 a.m. to 4 p.m. in July, 2013). Then, abrasion resistance of each irradiated sample was determined according to the standard ASTM- 4966/D4970.

Crease recovery angle

Crease recovery angle was determined by a Shirley Crease Recovery Tester according to the standard AATCC Method 66.

Surface friction

This test was done based on the standard test method BS3424 using a Shirley instrument. The results were reported as the static angle of surface drag (Ds) according to the standard test method.

Air permeability

The air permeability is one of the important features of delicate fabrics, especially lacy fabrics. To investigate the effect of nanotreatment on air permeability, a test was performed according to the standard BS-5636 on four folded samples under 1mm H₂O column pressure.

Bending length

This test was done according to the standard ASTM-D1388 using a Shirley Stiffness Tester.

Scanning electron microscopy

Scanning Electron Microscope (SEM) micrographs were obtained using a Vega 3, Tescan scanning electron microscope with different magnifications.

Results and Discussion

Hydrophilicity-hydrophobicity

The Samples, treated with an optimal percentage of titanium dioxide (obtained in prior studies), were treated with different concentrations of XPs resin, and then the absorption time was considered as a hydrophobicity index. Overall, evaluation of the hydrophobicity of the samples treated via this method can be considered as a criterion for determining whether or not to form a thorough layer of resin on the surface [32]. Hence, an appropriate concentration of resin to form an optimal resin layer covering the surface should be determined. Therefore, hydrophobicity has an optimal point [32]. Actually, maximum hydrophobicity is obtained when a film of resin is formed on the surface. Incomplete coverage reduces hydrophobicity with respect to the optimal status. Similarly, the excess resin, due to rearrangement of hydrophilic groups, can also increase hydrophilicity. The appropriate resin concentration also depends on other treatments as well as the fabric structure. The study revealed that a 1% concentration of resin is the optimal amount to form a thorough layer on the surface (Table 2). In fact, the optimum concentration of resin was achieved at maximum hydrophobicity (Table 2). Considering achieving maximum droplet absorption time at the concentration of 1% in all the cases, this concentration was chosen as the selected concentration of resin to treat all the delicate fabrics.

Table 2: Water droplet absorption Time (s) of control and XPs+TiO₂ treated samples with 1wt% and 1.5 wt% of resin. Data has been reported in “Average (SD)” form.

  

    
Sample
    
Control
    
Treatment
    
Resin    1%
    
Resin    1.5%
  
  

    
CL 
    
180 (11)
    
XPs+TiO2 
    
5484 (150)* 
    
4080 (34)
  
  

    
W(XPs+TiO2) 
    
26040 (2508) 
    
3936 (20)
  
  

    
FL 
    
456 (66)
    
XPs+TiO2 
    
3840 (252) 
    
4200 (44)
  
  

    
W(XPs+TiO2) 
    
21720 (1368) 
    
4020 (52)
  
  

    
SC 
    
8500 (59)
    
XPs+TiO2 
    
9480 (66) 
    
3900 (0)
  
  

    
W(XPs+TiO2) 
    
5280 (288) 
    
4140 (66)
  
  

    
TC 
    
660 (48)
    
XPs+TiO2 
    
5460 (114) 
    
3660 (0)
  
  

    
W(XPs+TiO2) 
    
4920 (384) 
    
3480 (0)
  
  

    
LC 
    
480 (42)
    
XPs+TiO2 
    
5220 (288) 
    
4020 (24)
  
  

    
W(XPs+TiO2) 
    
4200 (606) 
    
3660 (30)
  

Table 2: Water droplet absorption Time (s) of control and XPs+TiO2 treated
samples with 1wt% and 1.5 wt% of resin. Data has been reported in “Average
(SD)” form.

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Water droplet contact angle

Since the samples without resin had a rapid absorption (about 20s for untreated control sample and about 5s for only TiO₂ treated samples) water drops had a contact angle less than 90 degree and were not stable on the surface. Thus, the contact angle of the samples treated with resin was evaluated. Super hydrophobicity was obtained by reaching the contact angle up to over 130 degrees in the FL and SC samples and up to 150 degree in the CL sample. It has been realized that lowering the surface tension cannot increase contact angle more than 120º [35]. However, a hydrophobic nano-roughness can enhance the contact angle significantly [36]. In this paper, hydrophobicity can be accomplished by using the optimal concentration of resin on the created nano-roughness. (Figure 1-a) shows the drops and their evaluated contact angle.

Figure 1: Hydrophobisity of Sample; a) The water droplet status on “TiO₂+XPs” samples; Average Contact Angle (ACA) has been reported for each sample, b) Effect of slipping of methylene blue drop; left samples are control and right samples are treated samples.

    

    

    Figure 1:  Hydrophobisity of Sample; a) The water droplet status on “TiO2+XPs” samples; Average Contact Angle (ACA) has been reported for each sample, b)
Effect of slipping of methylene blue drop; left samples are control and right samples are treated samples.
    
    

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Stain repellency

As shown in (Figure 1-b), in the control sample, stain drops were thoroughly absorbed during moving on the surface. However, in the samples treated with resin, the drops rapidly slipped without any trace. Investigation of the stain repellency of the samples was also pursued by another method. The samples were turned into a dye solution, and then color changes were studied. Figure 2-a shows the color difference between after and before staining for each sample.

Figure 2: a) calculated color difference (ΔE) after staining as compared to same samples before staining, b) comparing the results of two effluent analysis techniques to determine released TiO₂ in washing effluents, c) sunlight resistance of samples (end points in abrasion resistance test).

    

    

    Figure 2:  a) calculated color difference (ΔE) after staining as compared to same samples before staining, b) comparing the results of two effluent analysis
techniques to determine released TiO2 in washing effluents, c) sunlight resistance of samples (end points in abrasion resistance test).
    
    

Close

TiO₂ samples, which had super-hydrophilic features, absorbed methylene blue more than control samples did, while sample which have XPs treatment varied less and resisted staining. According to (Figure 2-a), the color differences between the after and before staining for XPs-treated samples were very low. Therefore, the positive performance of XPs is confirmed. Figure 2-a shows ΔE values, the color difference between before and after staining calculated for each sample by the formula mentioned in the test method section.

Scanning electron microscopy

Scanning Electron Microscopy (SEM) was used to observe the particle dispersion on the treated samples. As (Figure 3), SEM observations of different magnifications, showed the nanoparticles had good dispersibility. It was also confirmed that an even coating had formed on the fiber surfaces.

Figure 3: SEM micrographs of nanofunctionalized fabrics with different magnifications. 1^st row a-d) TC, 2^nd row e-f) FL and g-h) CL.

    

    

    Figure 3:  SEM micrographs of nanofunctionalized fabrics with different magnifications.
1st row a-d) TC, 2nd row e-f) FL and g-h) CL.
    
    

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Washing stability

As mentioned, there is no affinity between TiO₂ and fabrics. Nanoparticles are reluctant to react chemically with polymer surfaces. Therefore, they were absorbed physically and their stability was completely related to XPs resin to characterize the released TiO₂, proper diluted washing effluents were analyzed by ICP-OES. For this purpose, FL samples were chosen to examine. The final results have been reported in (Figure 2-b). The results demonstrated that XPs resin could save about 81% and 80% of nanoparticles after 5^th and 20th washing cycles, respectively, while the TiO₂ remaining on the sample without XPs was about 26% and 22% after 5th and 20th washing cycles, respectively.

Because of such features as availability and low cost, UV-vis spectroscopy was used to evaluate the washing stability of the samples. To investigate the competency of such an alternative, all the data obtained by both methods were compared (Figure 2-b). The results showed a good consistency, thus it can be concluded that UVVis spectroscopy is a good alternative to follow the ICP-OES method in this case.

Table 3 reports the amount of the released titanium dioxide in all the effluent samples with “TiO₂” and “(XPs+TiO₂)” treatment as an index for measuring nanoparticle stability. The percentage of the remaining TiO₂ on each washed sample was also calculated to investigate the stabilizing efficiency of XPs treatment.

Table 3: UV-Vis based effluent analysis and calculated fastness.

  

    
Samples 
    
Treatment Status 
    
Washing cycle 
    
Released TiO2 (ppm) 
    
Remained TiO2 on fabrics (%) 
  
  

    
FL 
    
TiO2
    
5
    
39180
    
21.64
  
  

    

    
TiO2+Ps
    
5
    
9776
    
80.45
  
  

    

    
TiO2
    
20
    
40619
    
18.76
  
  

    

    
TiO2+Ps
    
20
    
10552
    
78.90
  
  

    
TC 
    
TiO2
    
5
    
27132
    
45.74
  
  

    

    
TiO2+Ps
    
5
    
7500 
    
  85.00
  
  

    

    
TiO2
    
20
    
28268
    
43.46
  
  

    

    
TiO2+Ps
    
20
    
10700
    
78.60
  
  

    
LC 
    
TiO2
    
5
    
31544
    
36.91
  
  

    

    
TiO2+Ps
    
5
    
8544
    
82.91
  
  

    

    
TiO2
    
20
    
32452
    
35.10
  
  

    

    
TiO2+Ps
    
20
    
8803
    
82.39
  
  

    
SC 
    
TiO2
    
5
    
49150
    
1.70
  
  

    

    
TiO2+Ps
    
5
    
2426
    
95.15
  
  

    

    
TiO2
    
20
    
49714
    
0.57
  
  

    

    
TiO2+Ps
    
20
    
2499
    
95.00
  

Table 3: UV-Vis based effluent analysis and calculated fastness.

Close

Based on the results, there was a significant loss in the amount of titanium dioxide on the sample without resin after 5th wash, as compared to the sample treated with TiO₂ and resin. Calculating the titanium dioxide remaining on the SC fabrics revealed that about 95% of nanoparticles still existed on the fabric treated with resin after 20 times of home laundering. As predicted, in the samples treated only with TiO₂, nanoparticles were easily separated from the surface. Here, the role of resin, as a good holder is clear because, even in the five primary effluents of samples treated with resin and titanium dioxide (Xps+TiO₂), the concentration is extremely lower than that of the sample without the resin.

Sunlight resistance

To evaluate the protection efficiency of nanomaterial against sunlight, the samples were exposed to sunlight for 100 and 160 hours and then the abrasion resistance was tested as an index for evaluating the resistance of fabrics against structural degradation under UV. The results (Figure 2-c) showed that increasing the time of exposure to sunlight weakened the fibers of the control samples (in the case of FL and CL which were tested), and their abrasion resistance decreased, while nano-treatment could control the harmful effects of sunlight. It seems that applying this feature in upholstery, especially curtains, is significantly constructive.

Air permeability

FL and CL fabric series were examined in terms of air permeability. The results were reported in (Table 4). The statistical analysis indicated that the nano-functionalization has no significant effect on air permeability.

Table 4: Physical properties of lace fabrics (Data is reported in “Average (S.D.)” form).

  

    
Physical factor
    
FL samples
    
CL samples
  
  

    
C
    
TiO2
    
W(XPs+TiO2)
    
C
    
TiO2
    
W(XPs+TiO2)
  
  

    
Air permeability  (ml.S-1/5cm-2) 
    
276 (10.6)
    
-
    
266 (9.7)
    
214 (10.1)
    
-
    
208.2 (4.45)
  
  

    
Bending length (cm) 
    
1.93 (0.4)
    
1.96 (0.15)
    
1.8 (0.2)
    
3.18 (0.4)
    
3.3 (0.32)
    
2.8 (0.6)
  
  

    
Crease recovery angle    (degree) 
    
148.2 (2.4)
    
69.6 (11)
    
162.6 (1.7)
    
141 (1.6)
    
104.6 (1.8)
    
152.2 (2.6)
  
  

    
Static angle of    surface drag (Ds) 
      
(degree) 
    
40.3 (4.5)
    
47.9 (1.8)
    
36.5 (4.9)
    
39.8 (1.35)
    
47.9 (1.8)
    
44.3 (1.77)
  

Table 4: Physical properties of lace fabrics (Data is reported in “Average (S.D.)” form).

Close

Bending length

Bending length was evaluated as a criterion of stiffness and handle for FL and CL fabric series. The results were reported in (Table 4). Although the results showed TiO₂ treatment made surfaces stiffer, XPs had an opposite effect. However, according to the statistical analysis, the differences were not significant.

Crease recovery angle

An experiment was performed to evaluate FL and CL crease recovery angle. As reported in (Table 4), TiO₂ treatment significantly decreased the crease recovery angle; however, XPs significantly improved the anti-wrinkle properties of both kinds of fabrics as compared to both control samples and TiO₂ treated samples.

Surface friction

FL and CL fabric series were also examined for surface friction properties (Table 4). According to the results, TiO₂ treatment increased friction coefficient as compared to the control samples. XPs had compensated for this effect. According to the statistical analysis, the differences between all the samples were significant in the case of CL series fabrics; however, in the case of FL series, only the differences between TiO₂ and TiO₂+XPs were significant. However, the treatments had no significant effect as compared to the control FL sample.

Conclusions

In this study, different patterned and unpatterned light-weight and delicate fabrics and lacy fabrics were treated by titanium dioxide and polysiloxane resin (XPs), and their final properties were evaluated. By applying TiO₂ and XPs treatment, significant hydrophobicity and super hydrophobicity were achieved. The results revealed that the textiles constructions significantly affected on the results. In the ideal case, absorption time of water-drop was approximately 6 hours. Stain droplets slipped on the samples without any trace; and thus, the desirable stain repellency was achieved. The maximum obtained value of contact angle was about 150 degrees, which is another sign of good hydrophobicity of the treated sample.

Based on results, XPs treatment was able to effectively prevent separation of particles from the fabric surface during washing. After calculating the percentage of titanium dioxide remaining on the fabrics, it was found that, in the case of the best fastness, about 95% of the particles still remained after 20 times of domestic laundering. The optimal stability was directly related to silicone resin. Polysiloxane resin on TiO₂ compensated for the unpleasant variation created by titanium dioxide treatment in flexural stiffness, air permeability, as well as friction, and improved wrinkle recovery. Based on the results, the nanocomposite coating served as a protective layer against the destructive effect of sunlight. Consequently, the nano-finishing can be used as a novel effective treatment to enhance practical properties and/or add some desirable functions to the different patterned and unpatterned and lacy light-weight and delicate fabrics. However, it should be noted that the level of improvement depends on textiles constructions and it may be optimized to achieve the ideal properties.

Acknowledgement

The authors would like to thank Evonik (Degussa) Corporation (Germany) and Wacker Finish Company (Germany) for their kind providing of nano-sized colloidal TiO₂ and polysiloxane emulsion, respectively.

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Citation: Dastjerdi R, Zavareh HH, Mashroteh H and Ardakani AK. Nano-Coating on Different Patterned and Unpatterned Light-Weight and Delicate Curtain and Lacy Fabrics; Multifunctional Features and Comparing ICPOES and UV-vis Spectroscopy to Determine Washing Fastness. Adv Res Text Eng. 2018; 3(1): 1020.

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