Seminar entitled " Surface modification of woollen textiles " presented in department of Textiles and Apparel Designing, College of Community Science, UASD, Karnataka by Manpreet Kaur and Dr. Geeta Mahale.

1. Surface Modification of Woollen Textiles
SEMINAR
Manpreett Kaur and Dr. Geeta Mahale

2. Surface modification
It is an act of modifying the surface of a material by physical, chemical or
biological characteristics different from the ones originally found on the surface
of a material.
Purpose of surface modification
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• Enhancing anticorrosive properties
• Increasing the bioactivities
• Improve adhesion property
• Improve biocompatibility
• Create permanent wettability, Improve the hydrophobicity, dyability
• Soft feel

3. 09-11-2022 3
Wool Fibre
Wool fibre is obtained from follicles of sheep, goat, camel,
rabbit like vicuna, llama and alpaca as wool as wool fleece.
• Wool fibre is a protein fibre (keratin).
• It is composed of 18 amino acids in which the important
amino acids are cysteine(13.1%), glutamate (11.1%), and
serine(10.8%).
Wool fibre has three different morphological parts
• Cuticle(protective layer)
• Cortex
• Medulla(network of air occupied cells)

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4. Oxidative/ Reductive
treatment
5. Enzyme treatment
6. UV radiation
3. Chitosan treatment
2. Plasma treatment
1. Nanoparticles
7. Sol- gel technique

5. ENZYME TREATMENT
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Proteins of large molecular size
Active group reacts with
substrate to form products by
decreasing the activation energy
pH, temperature and substrate
specific

6. Objective
• To find out the effect of protease enzyme on the physical and colourfastness properties
of the woollen fabric
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Pooja et al. (2014)
Quality improvement of Wool Fabric using Protease Enzyme
1

7. Methodology
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Raw
Materials
Pretreatment
of woolen
fabrics
Enzyme
Treatment
Scouring
• Liquid soap (Ezee)
: 0.5 % (o.w.f)
• M:L : 1:50
• Temperature : 40ºC
• Time duration : 30
min
• Alkaline protease : 1,
2, 3, 4 and 5 % (o.w.f)
• M:L : 1:20
• Temperature : 40ºC
• Time : 60 minutes
• pH : 8.5
• Coarse woollen
(woven) fabric
• Alkaline Protease
Enzyme
Testing For
Physical
Properties
• Absorbency
• Fabric tensile test
• Weight loss
• Pilling resistance
• Fabric drape
• Hand of fabric
• SEM

8. Dyeing of
Wool Fabric
Acid dye : 10% (o.w.f.)
Glauber’s salt : 15% (o.w.f.)
Sulphuric acid : 4% (o.w.f.)
M:L : 1:30
Time : 45 minutes
Temperature : 60º C
Colourfastness
Testing of Dyed
Samples
SI. NO TEST EQUIPMENT TEST NUMBER
1 Colourfastness to
light
Sunlight Exposure
Rack
AATCC-RR 92, 2013
2 Colourfastness to
washing
Launderometer IS:3361-2003(test-2)
3 Colourfastness to
rubbing
Crock meter AATCC-RA 38, 2005
4 Colourfastness to
perspiration
Perspirometer AATCC-RA 52, 2006
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9. S.No TEST TEST STANDARD
1 Absorbency AATCC:79-2010
2 Fabric tensile test IS:1969(Part 2):2010/ISO 13934-2:1999
3 Weight loss ASTM d 2720-94 (2012)
4 Pilling resistance IS:10971(Part 1):2011/ISO/2945-2:2000
5 Fabric drape ASTM D-737-04 (2012)
6 Hand of fabric AATCC: EP 5
7 SEM(scanning electron microscope) ZEISS EVO 50 instrument
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Table 1 Testing For physical properties

10. SI No. Types of
treatments
Conc. Of
Protease
enzyme
Hand of fabric Weight
loss
(%)
Absorbency(
time taken
in seconds)
Fabric tensile
strength
Fabric
drape
Pilling(ra
ting)
Softness Smoothness Warp Weft
1 Control - 2 2 - 60 42 40 0.85 5(no
pilling)
2 Scoured - 2 3 0.52 45 40 36 0.75 5
3 Protease
treated
1 3 3 1.47 42 34 35 0.67 5
2 3 4 2.73 38 32 37 0.65 4-5
3 4 4 4.10 35 33 36 0.64 4
4 5 5 5.36 33 32 32 0.48 4
5 5 4 6.31 31 31 32 0.61 3
Table 2. Effect of various concentrations of Proteases enzyme treatment on physical properties of
woollen fabric
Results and Discussion
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11. Fig. 1 Scanning Electron Microscope (SEM) Test
Mag=2.00KX Mag=5.00KX
Control fibres
Scoured fibres
1g/l protease enzyme treated fibres
2g/l protease enzyme treated fibres
3g/l protease enzyme treated fibres
4g/l protease enzyme treated fibres
5g/l protease enzyme treated fibres
11

12. S I.
No
Type of
treatments
Conc. of
protease
enzyme(g/l)
Colourfa
stness
to light
Colourfastness to
washing
Colourfastn
ess to
crocking/
rubbing
Colourfastness to perspiration with acid dye
Colour
change
Colour
Staining
Dry Wet Staining(wool) Change in color
Acid Alkali
ne
Acid Alkaline
1 Control - 6 3/4 3/4 4 3/4 2/3 2 4/5 4/5
2 Scoured - 7 3 3 4/5 3/4 2/3 2 4/5 4
3
Protease
enzyme
treated
1 5 3 3/4 4 3/4 2 2 4 4
2 6 3 3/4 4 3/4 2 2/3 4/5 4/5
3 8 3 3/4 4 3/4 2/3 2/3 4/5 4/5
4 8 3/4 4 4/5 4 3 3 5 4/5
5 8 3/4 4 4/5 4 3 3 5 4/5
Table 3. Effect of Acid dye on colourfastness properties of woollen fabric
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13. • Improved physical properties including hand, drapability,
absorbency, dye ability and colour fastness properties
• Tensile strength decreased slightly
• 4 g/l enzyme concentration showed best results
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Conclusion

14. Objective:
• To find out the optimum condition to achieve the best colour after dyeing
the wool fabrics
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Pour and He
(2019)
Surface Functionalization of Wool via Microbial-Transglutaminase as
Bio-Mordant to improve dyeability with Madder in the presence of Alum
2

15. Methodology
Materials: Woolen fabric(10*10cm), plain
weave structure(195g/m2)
• Alum or Aluminum sulfate (mordant)
• Microbial transglutaminase(alizarin)
• Standard washing soap and standard
synthetic detergent
• Acetic acid
Dye
Extraction
Madder root
Natural dye powder was dissolved in water
along with continuous stirring at 1000C for 1 h
The solution was maintained at room
temperature for 24 h
Filtered, Diluted
• Woollen fabric was immersed in
5%, 10%, and 20% owf of the
alum solution
• MLR: 40:1
• pH= 4
• Temp.= 400c for 1h
• Washing and drying
• Madder (50% owf) and
acetic acid (5% v/v) at a
liquor ratio of 50:1 (water
bath shaker machine)
• 400 C to 800 C in an over 20
min period and was further
continued for 60 min
• m-TGase: 5%, 10%, and 20%
w/w
• MLR: 40:1
• pH : 9–10 at 370c
• The enzymes were inactivated
in a solution with pH 5, while
it was adjusted using acetic
acid for 5 min at 800c
• Washing with water to
prevent the hydrolyzation
Mordanting
Pretreatment of
wool
Dyeing
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16. Testing
• SEM
• Contact angle and wettability
• Colorimetric Analysis
• Colour Variation
• Colour fastness properties of dyed
woollen samples
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Fig 3. SEM images of treated wool with (a) 10% alum-5% m-TGase, (b) 20% m-TGase, and (c) 10%
alum-20% m-TGase; using more m-TGase caused surface damages on wool fiber.
Results and Discussion

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Fig 4. Water droplets on untreated wool; treated wool with 5% m-TGase; treated wool with 10% alum and
5% m-TGase

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Fig.5 (a) Colour strength and (b) Colour difference (DE) of untreated and treated wool

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Table 5. Variation of colour fastness under different treatments

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Fig.6 Colour of dyed wool (treated and untreated)

22. Conclusion:
• presence of interaction between alum, m-TGase, and wool fibers
• optimum condition: 10% owf alum and 5% owf m-TGase
Fig 7. Schematic illustration for the proposed mechanism of treated wool with alum and m-TGase
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23. 09-11-2022 23
PLASMA Surface modification

24. Functionalization of Wool Fabric with Phase-Change Materials
Microcapsules after Plasma Surface Modification
Objective
• To examined the influence of dielectric barrier discharge (DBD) plasma treatment
on the adhesion of phase-change material (PCM) microcapsules on wool fabric
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Oliveira et al. (2012)
3

25. Materials
Microcapsules
PCMs
Wool fabric (100 %
wool plain weave
fabric with 194g/cm2)
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Methodology
PRETRHERMO C -25(
melamine microcapsule
agent )

26. Dielectric barrier discharge
Plasma treatment
Contact angle and Surface free energy
Microcapsule Size Distribution
Impregnation of the PCM microcapsules
SEM, XPS, DSC, Washing test
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Laboratorty prototype,
LISBOA
Data physics instrument
using OCA20 Software
Malvern mastersizer for
particle size analysis
Padding process,
PCM microcapsules= 160g/l,
binder= 50g/l, MgCl2=5g/l, pH=
5 Temp.= 1400C
Dielectric barrier discharge
Malvern Mastersizer

27. Speed (m/min) N P (W) Dosage (W min/m2)
4.0 1 500 250
4.0 2 500 500
4.0 3 500 750
4.0 4 500 1000
4.0 5 500 1250
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Table 6 Plasma Dosages Applied
Plasma Dosage= NP/vl
Where:
N= number of passages
P= power
V= Velocity
l= width of treatment
Liquid  (mJ/m2)
Distilled
water
72.8
PEG 2000 43.5
Glycerol 63.4
= Total surface energy
PEG 2000= Polyethyleneglycol
Table 7 Surface Energy of the Tested Liquids
Results and Discussion

28. 09-11-2022 28
Fig.8 Static Contact angles of the Wool Fabric
Fig. 9 Dynamic contact angles of the wool
fabric with different plasma dosages

29. Table 8 Contact Angle (Standard Deviation), Surface Energy
Sample Water (○) PEG (○) Glycerol (○)  (mJ/m2) D (mJ/m2) P (mJ/m2)
Untreated 160.8 (0.5) 132.6 (5.9) 151.8 (4.5) 4.4 4.4 0.0
250 W min/m2 130.7 (14.0) 60.9 (4.0) 151.2 (5.5) 10.5 10.0 0.5
500 W min/m2 95.5 (7.8) 54.7 (5.7) 141.8 (9.9) 15.4 9.0 6.3
750 W min/m2 81.2 (9.9) 51.3 (3.1) 133.4 (7.2) 21.4 5.5 15.8
1000 W min/m2 38.7 (7.6) 47.1 (5.2) 130.5 (5.7) 30.5 5.0 25.5
1250 W min/m2 20.5 (9.0) 45.5 (4.9) 129.3 (4.5) 53.4 0.5 53.0
= Contact angle
= Total surface energy
D= Dispersive component of surface
energy
P= Polar component of surface energy
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30. 09-11-2022 30
Fig. 10 SEM micrographs obtained with secondary electrons of the (a) untreated and (b)
DBD plasma-treated wool fabric with a dosage of 1250 W min/m2

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Fig. 11 Photoemission spectra of the wool fibres before and after DBD plasma treatment (1250
W min/m2): (a) C1s and (b) O

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Fig. 12 Deconvoluted XPS C1S and O1S core level spectra of (a,c) untreated wool fibers and (b,d)
plasma-treated (1250 W min/m2) wool fibers

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Fig. 13 PCM microcapsule size distribution and SEM micrograph

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Fig. 14 SEM micrographs obtained with secondary electrons (SE) of the untreated and
plasma-treated (1250 W min/m2) wool fabric with PCM micro- capsules before and after
washing fastness test

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Fig.15 DSC thermograms of the untreated and plasma-treated wool fabric with PCM
microcapsules before and after the washing test

36. Conclusion
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• The plasma treatment caused a decrease in the static and dynamic
contact angles
• Increase in the surface energy of the wool substrate
• increased the amount of oxygen on the surface of the substrate,
created more polar groups, and improved the
hydrophilicity/wettability of the wool fiber (DBD treatment)

37. Study of Surface Modification of Wool Fabrics Using Low Temperature
Plasma
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Shahidi et al. (2013)
4
Objective:
• To change the fabric surface both physically and chemically by using LTP treatment

38. Wool fabrics (20 denier)
LTP Treatment
Characterization tests
The DC magnetron sputtering reactor was used to treat the
wool fabrics, and non polymerizing reactive gases, such as O2,
N2 and Ar
Sheet of wool fabric was placed on the anode or cathode
Before the process started air and old gases had to be
pumped out by the vaccum pump
Plasma gas was introduced into the reaction chamber
SEM, FTIR
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Methodology
The pressure remained at 0.02 Torr for the entire glow-discharge
period

39. Sample Description
No1 Sample was placed on the cathode Ar gas
was used for 7 min
No2 Sample was placed on the cathode O2 gas
was used for 7 min
No3 Sample was placed on the Anode O2 gas
was used for 7 min
No4 Sample was placed on the Anode N2 gas
was used for 7 min
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Fig. 17 SEM images of treated and untreated samples
Table 9. Description of samples
Results and Discussion

40. Fig. 18 FTIR spectra of samples
Fig. 19 Reflection spectroscopy of untreated
and treated samples
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41. Sample Absorption time
Untreated 20 min
No1 5 sec
No2 1 sec
No3 2 sec
No4 3 sec
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Table 10: Absorption time of treated and untreated samples
Conclusion
• Increased wettability and dyability
• Surface of wool samples were changed physically and chemically

42. Chitosan treatment
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Non toxic and biodegradable
Composed of hydroxyl and amine
groups, ether linkages

43. Objective
• To analyze polymer loading%, k/s value, dye uptake% and wash
fastness property of the dyed wool fabric
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Rana et al. (2017)
Surface Modification of Wool Fabric with Chitosan and Gamma
Radiation
5

44. 09-11-2022 44
Materials:
Single jersey
fabric
Chemicals:
Sodium carbonate: Scouring agent
Hydrogen peroxide: bleaching agent
Chitosan: cationizing agent
Acid Red dye: Maintain the pH
Soda ash: assessing colour fastness of
fabric

45. Methodology
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Sampling: Wool Samples ,Two different sizes
6*6 cm and 10*10cm
Scouring and Bleaching of Wool: Detergent (Felson NOF) :2 g/L, Na2CO3 :5 g/L, H2O2:6 g/L,
Stabilizer(Sodium silicate):1.5 g/L, Sequestering agent:1 g/L, Temp.:600C, Time:80min
Treatment of wool with Gamma Radiation: Irradiation with Cobalt-60 gamma radiation
Dose rate :5, 10, 20, and 50KGy/h individually
Dyeing process of treated and untreated wool: 1% Acid Red New, temp.:1000C, time: 30min,
MLR: 1:10, H2SO41 g/L, pH:3-4, washing at Temp.:800C, for 10 min with 1 g/L soaping agent
Treatment of wool with chitosan: Conc.0.1%, 0.3%, 0.5%, 0.7%, and 1%, temp.600C,
time.30min, exhausted method ,in IR Dyer

46. Determination of polymer loading: Polymer loading% = (W2-W1)/ W1×100%, Where W1=dry
weight of untreated sample, W2=dry weight of sample after treatment
FT-IR Analysis
Determination of color strength: Color strength(k/s) = (1-R)2/2R
Determination of Dye uptake%: UV visible spectrophotometer
Dye uptake% = (A0-A1)/A0×100%, Where A0= Maximum
absorbency before dying, A1= maximum absorbency after dyeing
Determination of color fastness to wash: Method ISO 105 C04
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47. Result and Discussion
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Fig. 20 Fourier Transform Infrared Spectrometer Analysis of Wool
The infrared spectrum of untreated wool The infrared spectrum of 0.1% chitosan treated wool
The infrared spectrum of 10kGy gamma treated wool The infrared spectrum of 0.1%chitosanand 10kGy gamma treated wool

48. Softness
Table 11. Polymer loading % of different chitosan
concentration treated wool specimens
Fabric
typec
Chitosan
conc.
W1 W2 (W1)-(W2)+
W1×100%
Average
polymer
loading%
1 0.10% 5.001 5.063 1.32% 1.21%
11.303 11.438 1.19%
2 0.30% 4.198 4.255 1.35% 1.38%
11.809 11.976 1.41%
3 0.50% 3.787 3.802 0.39% 0.32%
12.317 12.348 0.25%
4 0.70% 4.734 4.738 0.11% 0.14%
11.611 11.631 0.17%
5 1.00% 3.877 3.899 0.55% 0.48%
12.268 12.319 0.41%
Fig.21 Polymer loading % of different
chitosan concentration treated wool
specimens
W1 =Average wt. before treatment W2= Average wt. after treatment
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49. Code Test fabric type
U Untreated
A 0.10% Chitosan treated
B 0.30% Chitosan treated
C 0.50% Chitosan treated
D 0.70% Chitosan treated
E 1% Chitosan treated
R1 5kGy Gamma radiation treated
R2 10kGy Gamma radiation treated
R3 20kGy Gamma radiation treated
R4 50kGy Gamma radiation treated
A R1 0.10% Chitosan+ 5kGy Gamma radiation treated
A R2 0.10% Chitosan+10kGyGamma radiation treated
A R3 0.10% Chitosan+ 20kGyGamma radiation treated
A R4 0.10% chitosan+ 50kGyGamma radiation treated
Table 12. Designation of specimens
Fabric type L* C* h* k/s value
U 40.117 50.828 2.661 12.8
A 38.447 50.227 2.412 14.0
B 38.257 50.829 2.626 14.4
C 39.900 51.004 1.892 12.8
D 40.087 51.535 2.501 12.8
E 38.455 50.889 3.424 14.2
R1 38.414 50.163 2.993 14.1
R2 37.729 50.236 3.007 15.0
R3 39.283 49.863 2.923 13.1
R4 39.619 48.809 2.204 12.5
A R1 37.988 49.770 2.378 14.3
A R2 39.139 50.372 2.126 13.7
A R3 39.129 49.888 0.124 13.1
A R4 38.287 47.516 2.197 13.0
Table 13. Variation of k/s value of treated and untreated wool specimens
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50. 09-11-2022 50
70
75
80
85
90
95
U A B C D E R1 R2 R3 R4 AR1 AR2 AR3 AR4
Dye uptake(%)
Fig. 22 Dye uptake % treated and untreated wool specimens

51. 09-11-2022 52
Table 14: Colour fastness to wash of treated and untreated sample

52. Conclusion
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• The higher the polymer loading % is, the higher the k/s value will be
• The k/s value of gamma treated specimens increased up to 10kGy then it decreased with
the increase of irradiation rate
• dye exhaustion of untreated specimen was highest, the fixation was the lowest

53. Environmentally friendly surface treatment of wool fiber with Plasma and Chitosan
for Improved Coloration with Cochineal and Safflower Natural Dyes
Objective
To know the effect of surface modification of wool fibre with oxygen plasma and chitosan
(PC) on the color strength of the samples dyed with cochineal and safflower natural dyes
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Haji et. al (2020)
6

54. Materials and Methods
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Preparation of stock
solution of natural
dyes
Plasma treatment
Chitosan treatment
Dyeing
Testing:
• Colour strength Measurement
• Colour fastness Evaluation
• Levelness measurement
• Dye Uptake measurement
• Dye Fixation measurement
• Evaluation of wettability
• Tensile Strength measurement
• SEM, FTIR

55. Results and Discussion
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Fig 26. Effect of pH on the colour strength of samples dyed
with cochineal (90 ºC, 60 min)
Fig 27. Effect of pH on the colour strength of
samples dyed with safflower (90 ºC, 60 min)

56. 09-11-2022 57
ig.28 Effect of dyeing temperature on the colour strength of
amples dyed with safflower (pH=3.6, 60 min)
Fig 31. Effect of dyeing time on the colour strength of
samples dyed with safflower (90 ºC, pH=3.6)
Fig 29. Effect of dyeing temperature on the colour strength
of samples dyed with cochineal (pH=3.6, 60 min).
Fig 32. Effect of dyeing time on the colour strength of samples
dyed with cochineal (90 ºC, pH=3.6).

57. 09-11-2022 58
Figure 33. SEM images of raw (a), plasma-treated (b), and chitosan-treated (c) samples

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Fig 34. Water wicking of raw, plasma-treated, and
chitosan treated samples
Fig 35. Proposed mechanism for attachment of chitosan to
plasma-treated wool fibers

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Table 14. Physical properties of raw, plasma-treated and chitosan coated woolen yarns
Table 15. Fastness properties and RUI values of wool samples dyed with cochineal and safflower
(pH=3.6, 60 min, 90 ºC)

60. Table 16. Dye uptake and dye fixation values of wool samples dyed with cochineal and safflower
(pH=3.6, 60 min, 90 ºC)
09-11-2022 61

61. Conclusion
• Increase in dyeability of wool fiber with cochineal and safflower
• Dye uptake, dye fixation, levelness, fastness, wicking, and tensile
properties of wool samples were improved
• Simple and environmentally friendly method
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62. 09-11-2022 63
Modificationby
Nanoparticles

63. Objective:
To analyze the performance of silver nanoparticles with different surface charge using
three different methods
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Barani et al. (2013)
Surface roughness and wettability of wool fabrics loaded with silver
nanoparticles
7

64. Materials and methods
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Materials :
• Reagent and wool fabric:
• Silver nitrate, Sodium
borohydride, lecithin
Area
weight
(g/m2)
Warp density
(Count/cm)
Weft density
(Count/cm)
Type of
weave
Yarn
fineness
(dtex)
Fibre mean
diameter*
(mm)
125 21 18 Plain
1/1
300/300 19 ± 3
Table 17. Characteristics of the wool fabric
Fig 36 Two- and three-dimensional images of an untreated wool fabric: (a) untreated wool fabric (scan area
of 4mm4mm); (b) type of weave; (c) 3D image of untreated wool fabric (scan area of 4mm4mm).
Methods
Silver nanoparticles loading methods
• Exhaustion
• Pad dry cure
• In situ synthesis

65. Silver nanoparticles loading methods
Exhaustion
Scoured wool fibric
sample immersed in an
aqueous solution
containing silver
nanoparticles (liquor ratio
of 40:1) , temp- 40 0C
In 25 min temp increased
up to 900C
Pad- dry cure method
• Scoured wool fabrics
immersed into solution of
silver nanoparticles with
different lecithin
concentration foe 15 min.
• Fabrics were squeezed by
padder machine.
• Padded sample dried at 800C
for 20 min.
In-situ synthesis
• Silver nanoparticles
synthesised in wool fibre
structure
• The scoured wool fabric
samples immersed in
silver nitrate solution with
various lecithin ratios at
room temperature for 1h
Sample code [Lecithin]/ [Ag] Ag (ppm) Surface charge (mV)
K 0 400 -26.3
K 0.2 400 -48.8
K 1 400 -49.1
K 2 400 -63.1
Table 2. Preparation of colloidal silver nanoparticles with their surface charge

66. Sample Sa (µm) Sq (µm) St (µm) Srl Svo
(µm3/µm2)
Untreated 17.7 21.3 122.6 1.1 0.135
EhK0
32.2 28.4 163.5 1.072 0.591
EhK0.2
20.4 24.8 152.3 1.125 0.414
EhK1
23.3 28.2 156.8 1.154 0.506
EhK2
23.5 28.3 154.0 1.126 0.371
ISK0
32.9 40.3 246.6 1.142 1.075
ISK0.2
35.2 42.9 272.7 1.152 0.793
ISK1
32.7 40.0 264.3 1.142 0.923
ISK2
34.2 41.7 268.0 1.148 0.943
PDCK0
22.0 26.6 147.2 1.106 0.279
PDCK0.2
32.1 27.9 153.9 1.132 0.272
PDCK1
23.3 28.1 152.9 1.128 0.411
PDCK2
24.1 29.0 168.8 1.189 0.366
Table 19. Surface roughness and porosity characteristics of wool fabrics loaded with silver nanoparticles
Results and Discussion
09-11-2022 67
Sa=surface
roughness
Sq=root mean
square surface
roughness
St=maximum
height between
the highest and
lowest point
Srl= hybrid
parameter
Svo =free
volume
available on
the textile
surface

67. Softness Smoothness Warp Weft
Absorbency
Fig 36 . Images of wool fabric loaded with silver nanoparticles without lecithin
using different methods: (a) untreated; (b) EhK0; (c) ISK0; and (d) PDCK0.
Fig 37. Heights histogram of wool samples treated with silver
nanoparticles using different loading methods.
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Results and Discussion

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Fig 38. Schematic representation of a cross-section of the wool fabric loaded
Untreated wool fabric
Pad dry cure method
In situ synthesis

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Fig 39 . Roughness characteristics of the wool
fibres loaded with silver nanoparticles using
different methods.
Fig 40. Effects of various modification methods
and lecithin concentrations on (a) contact angle
and (b) spreading rate.

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Fig 41. Correlation between water contact angle and wool fibre roughness Ra (a) and
arithmetic mean surface roughness Sa and wool fibre roughness Ra (b)
*= exhaustion method
Pad dry cure
In situ method

71. 09-11-2022 72
Conclusion
• Silver nanoparticle on wool surface using exhaustion method creates a surface
which is more hydrophobic
• Highest value for roughness, porosity, smoothness by in situ method

72. Modificationby Sol- gel technique
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73. Objective
• To know the self- leaning and hydrophilic property of wool fabrics
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Pakdel et al. 2013
Self-cleaning and superhydrophilic wool by TiO2/SiO2 nanocomposite
8

74. Equipments
• SEM
• X ray Diffractor
• Water contact angle meter
Methodology
Materials
• Wool fabric(substrate)
• Tetraethylorthosilicate(TEOS)and
Titanium tetraisopropoxide (TTIP
97%) (Precursor of SiO2 and TiO2)
• HCl and glacial acetic acid (sol
preparation)
Preparation of Sols
Scouring
TiO2 and SiO2
Treatment
Self cleaning test on
fabrics
Solid extraction
Pad dry cure process
Stained with 20l of 12g/l coffee
solution and exposed to UV radiation
Evaluated based on color removal
After adding sodium carbonate
solution into solution SiO2 and
TiO2 sols
Nanoparticles formed a
precipitate at the bottom of the
beaker
Precipitate separated
through centrifugation
Drying at 700c
for 12h
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75. TTIP+ Acetic acid+ Distilled Water+ HCl for 2h at 600c
Titania sols
Silica sols
Hydrolysis and condensation of TEOS in water+
HCl(pH= 3)
Stirred for 2h and kept
overnight at 16h
TiO2 and SiO2
Nanocomposites
TiO2 + SiO2 Sols on Ti/Si molar percentage ratio (70:30,
50:50,30:70) for 1h
Preparation of Sols
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76. 09-11-2022 77
Fig. 42 XRD patterns of extracted powders
Results and Discussion
25.31

77. 09-11-2022 78
Fig. 43. Coffee stain removal of wool samples: (a)
pristine wool; fabric treated with (b) TiO2, (c)
TiO2/SiO2 70:30, (d) TiO2/SiO2 50:50, (e) TiO2/SiO2
30:70, and (f) SiO2
Fig. 44. Water droplets on wool samples: (a) pristine wool; wool treated
with (b) TiO2, (c) TiO2/SiO2 70:30, (d) TiO2/SiO2 50:50 or 30:70
Fig. 45 Water contact angle on wool samples: (a) pristine wool; fabrics treated
with (b) TiO2, (c) TiO2/SiO2 70:30, (d) TiO2/SiO2 50:50, and (e) TiO2/SiO2
30:70.

78. 09-11-2022 79
Fig. 48 SEM images of wool samples: (a) pristine wool; fibres coated with (b) TiO2,
(c) TiO2/SiO2 50:50, and (d) TiO2/SiO2 30:70.
a
c
b
d

79. • Increasing the concentration of silica, the TiO2/SiO2 nanocomposite showed more capability
in decomposing the stains
• After applying TiO2/SiO2 50:50 and 30:70 onto a wool fabric, a superhydrophilic surface was
obtained even in the absence of UV irradiation
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Conclusion

80. UltrasoundTechnology
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81. Functional Antibacterial Finishing of Woolen Fabrics Using
Ultrasound Technology
Objective
• To enhance the functional antibacterial property of woollen fabrics
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Abdelghaffar et al. 2018
9

82. Preparation of Wool/PEG
• Coating with PEG by exhaustion
merthod using conventional and
ultrasound technique
• Concentration of PEG: 0-20g/l
• CaCl2: 0-3g/l, pH: 4.5 at 600C for
60min, MLR: 50:1
Dyeing modification wool fabric
MLR: 50:1, Temp: 600C, 2%(owf) acid
dye, pH: 4.5 time : 60min
Materials: Wool fabrics
• Polyethylene glycol(PEG)
• SiO2 nanoparticle
• Acid Red 1
• Calcium chloride, citric acid and
sodium hypophosphite
Bacterial strains: Escherichia coli
(ATCC 25922), Staphylococcus aureus
(ATCC 33591)
Scouring of Wool : 20 min in ultrasound
bath, 5g/l non ionic detergent at 400C
Ultrasound Equipment: CREST
Ultrasonic, TRU-SWEEPTM ultrasonic
benchtop cleaner bath
Methodology
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Preparation of Wool/SiO2NPs and
Wool/PEG/SiO2NPs
• Crosslinking agent: 50g/l citric
acid, 15g/l sodium hypophosphite,
1g/l SiO2NPs for 15 min.
• Immersed at 700C for 60 min
• Drying at 800C for 5 min and cured
at 1500C for 3min
Characterization: SEM, FTIR, XRD
Testing: Mechanical properties, Fastness
testing, Antibacterial test

83. 09-11-2022 84
Fig 47. SEM and EDX of raw wool fabric (a), Wool/PEG (b, c), Wool/SiO2 NPs (d, e) and Wool/PEG/SiO2 NPs (f, g) in ultrasound and conventional techniques
Results and Discussion
a
e
d
c
b
f g

84. 09-11-2022 85
Fabric sample Change in tensile
strength
(%)
Contact angle
(o)
Blank (Raw wool) - 114.7
Wool/SiO2 NPs (CH) 14.73 117.4
Wool/SiO2 NPs (US) 11.30 121.0
Wool/PEG/SiO2 NPs (CH) 30.45 123.9
Wool/PEG/SiO2 NPs (US) 19.40 124.1
Table 20. Mechanical properties of untreated and treated wool fabrics

85. 09-11-2022 86
Fig. 49 Contact angle measurements of raw wool fabric (a),
Wool/SiO2 NPs (b, c) and Wool/PEG/SiO2 NPs (d, e) in conventional
and ultrasound techniques
Fig. 51 Effect of the concentration of calcium chloride on the
dyability of wool fabrics
Fig. 50. Effect of addition of different concentration of PEG2000 on
the dyeability of wool fabrics
a b
c
e
d

86. Sample Fastness properties
Washing Perspiration Crocking
Alkali Acid Dry Wet Light
W C P Alt W C P Alt
W C P Alt
Blank 3 1 4 3 4 2-3 4-5 4 4 3 4-5 4 4 4 5
Wool/SiO2NP
s (CH)
3 2-3 4 3 4 2-3 4-5 4 3-4 3 4-5 4 4 3-4 6-7
Wool/SiO2NP
s (US)
2-3 2 4 2-3 4 2-3 4-5 4 3-4 2 4-5 4 3-4 2-3 6-7
Wool/PEG/Si
O2 NPs (CH)
4 3 4 3 3 2-3 4 4 3-4 3 4-5 4 4 3 6
Wool/PEG/Si
O2 NPs (US)
3 2-3 4 3 2-3 3 4 4 3-4 2-3 4-5 3-4 3-4 3 6-7
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Where, W: staining on wool, C: staining on cotton, P: staining on polyester, and Alt: alteration (change in colour).
Table 21. Fastness properties of dyed untreated and treated wool fabrics by PEG and SiO2 NPs using conventional and
ultrasound techniques

87. Sample Reduction of bacterial count (%)
Staphylococcus aureus ATCC 33591 Escherichia coli ATCC 25922
1 washing cycle 6 washing
cycle
10 washing
cycle
1 washing cycle 6 washing cycle 10 washing cycle
Blank 0 0 0 0 0 0
Wool/SiO2NPs (CH) 86.7 65.1 64.7 82.6 79.5 71.6
Wool/SiO2NPs (US) 89.2 78.2 74.5 98.6 57.2 51.4
Wool/PEG/SiO2 NPs (CH) 93.4 79.7 76.3 96.4 56.3 56.3
Wool/PEG/SiO2 NPs (US) 97 83.9 79 99.5 63.2 59
Table 22. Percent reduction of standard bacterial strains (American Type Culture Collection)
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88. Conclusion
09-11-2022 89
• Impart protective properties against microbial attack to wool fabrics
• PEG2000 coating on wool fabrics prior to the treatment with SiO2 NPs has
enhanced the antibacterial activity
• modification of wool fabrics increases the tensile strength
• ultrasound technique leads to improve the dyability of fabrics

89. REFERENCES
1. Abdelghaffar, F., Arafa, A, A. and Kamel, M, M., 2018, Functional antibacterial finishing of Woolen fabrics using Ultrasound Technology.
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3. Baran, H., Montazer, M., Calvimontes, A. and Dutschk, V., 2013, Surface roughness and wettability of wool fabrics loaded with silver
nanoparticles. Tex. Res. J., 1(2):1-9.
4. Haji, A., Ashraf, S., Nasiriboroumand, M. and Lievens, C., 2020, Environmental friendly surface treatment of wool fiber with Plasma and
Chitosan for improved coloration with Cochineal and Safflower natural dyes. Fibres and Polymers., 21(4): 743-750.
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