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Research regarding the plasma hydrophobization of textile materials for medical articles
Lilioara SURDU1, Ioan CIOARA2, Carmen GHITULEASA1, Nicula GHEORGHE1, Laurentiu DINCA1, Adriana SUBTIRICA1, Marilena NICULESCU1, Razvan RADULESCU1, Cosmin MEDOR3
The National R&D Institute for Textiles and Leather Bucharest (INCDTP) 16, Lucretiu Patrascanu str., 030508 Bucharest, Romania e-mail: email@example.com, webpage: http://www.certex.ro 2 “Gheorghe Asachi” Technical University Iasi 29, Dimitrie Mangeron blvd., 700050, Iasi, Romania e-mail: firstname.lastname@example.org, webpage: http://www.tuiasi.ro 3 University of Medicine and Farmacy "Carol Davila" Bucharest http://www.umf.ro Abstract: The protection robes used by the medical staff within the surgery operating units should meet a number of requirements, such as: decreased absorption ability for fluids and decreased capability of water retention. Chemical treatment of the fabrics used as medical work equipment was successful in obtaining the desired properties, but there are environmental concerns related to the disposal of chemicals after treatment. Taking into account the advantages of the plasma treatment technology, an enormous interest was gained in the last years, tending to replace chemical applications in finishing and pre-treatment of textiles products. This paper outlines the results of comparative research regarding the hydrophobic properties of several textiles with special destination – medical articles – using comparatively two processes: classical chemical treatment for hydrophobization and plasma hydrophobization. Surface treatment efficiency was assessed through laboratory tests (vapor permeability and air permeability) and their appearance by electronic microscopy. The hydrophobic properties of the produced materials have been evaluated by establishing the quantity of absorbed water, absorption time and contact angle. Hydrophobic treatment of cotton fabrics with plasma gas such as hexafloropropane (C 3 H 2 F 6 ) leads to a smooth surface with increased contact angle of water. The best results for hydrophobization with plasma treatment was observed on cotton materials. The research highlighted that the plasma technology represents a new alternative for better modification of medical surfaces and textiles. Keywords: plasma, textile materials, surface morphology, functionality
1. INTRODUCTION A plasma is a (partly) ionized gas, which contains free charge carriers (electrons and ions), active radicals and excited molecules. So-called non-thermal plasmas are particularly interesting, because they operate at relatively low temperatures and do not inflict thermal damage to nearby objects. In the past two decades non-thermal plasmas have made a revolutionary appearance in solid state processing technology. Surface preparation and modification has gained in the last decennia an enormous interest and discovered new applications. It is a complete other approach to modify only the surface properties without changing the bulk properties. This delivers new materials with new possibilities, which opens perspectives to resolve production or design problems or even develop complete new applications. Production problems are mainly caused by the substitution of the base material to new materials for example polymers, which have not the correct surface behavior for further processing. Design requires of course another way of thinking because one has to take distance from the conventional mechanical and chemical modification of surfaces.  The low pressure plasma technology is such an alternative where on a dry, environmental friendly and costefficient way the surface is modified on microscopic level.  The plasma technology will be described together with the different application groups. Meaning is to give a good overview of the possibilities of plasma nowadays and to open new thoughts for the future. The plasma treatment was realized to INCDTP by CD400 Roll-to-roll, Low pressure plasma equipment. Hydrophobic treatment of textile materials for medical articles was realized with hexafloropropane (C 3 H 2 F 6 ). The advantage of this plasma compared with atmospheric-plasma equipment is that it is a well controlled and reproducible technique.
4 Warp and weft Yarn 2 100% cotoon Nm 70/1 yarn 14.4 40. bandages and bonds were produced and analyzed (characteristics are presented in Table 2).2 596 V4 made from Yarn 4 100% PES 166.2 (70.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia. bandages and bonds). 100% PA. were manufactured woven textiles materials for medical articles. 1 2 3 4 5 6 Characteristics Length density Tensile strength Breaking elongation Twist direction Twist Destination t/m Cv % Tex (Nm) Cv % N Cv % % Cv % With the yarns shown in table 1.8 September 2012 Surface treatment process for hydrophobic treatment Surface preparation and modification has gained in the last years an enormous interest and discovered new applications.8 7. with characteristics required by the beneficiaries. 6 . Characteristics 1 2 3 4 5 6 Fibre composition Fabric width Mass Density U B Structure Breaking force U B cm g/m2 fire/ 10cm - 100 % cotton 115 73 80 80 Linen cloth 199 195 N .7 3. 2.4 3.2 5.7 15.0 7.2 (108. It is a complete other approach to modify only the surface. 100% PES.4 13.2 3.3 2. The present paper presents the modification of surface properties of textile materials by hexafloropropane plasma treatment (a) in comparison with hydrophobization / oleophobization product treatment (b).5 (33. The physical and mechanical characteristics of the yarns for the manufacturing of the textile medical articles are presented in Table 1.69) 1.5 6 twistless Warp and weft Yarn 4 Polyester 9. Table 2: Characteristics of raw fabrics V1 made from Yarn 1 V2 made from Yarn 2 100 % cotton 114 98 80 125 Linen cloth 197 242 V3 made from Yarn 3 100% PA 138. Fabrics used for this study were made of 100% cotton. Table 1: Physical and mechanical characteristics of yarns used for the production of medical textile articles Yarn 1 100% cotton Nm 34/1 29.9 8.5 Warp and weft Yarn3 100% PA HT 940/140 187 (168) 1.4 45.9) 1.6 2.8 6.4) 4.83 140 760 360 Linen cloth 1204 1084 No.4 Warp and weft No.2 Z 866 2.3 1.3 420 200 100 Linen cloth 547.0 Z 1470 3. Four types of fabrics used for dressings.4 Z 659. EXPERIMENTAL PART The production of fabrics used for medical applications (dressings.7 13.
they are made suitable for manufacturing of hygienic and sanitary applications. breaking force (N). The barrier type fabrics were produced accordingly to the technical specifications. presented in table 2 were bleached and finished accordingly to technical specification for medical textile articles.by finishing the fabrics made of single spun yarns. the requirements specific to hospitals – surgery departments were considered. vapor permeability and air permeability was considered relevant.8 September 2012 Breaking elongation U B 7 % 7.resistance to hydrostatic pressure of minimum 200 mm water column. 1 2 3 4 5 6 7 8 9 10 Characteristics Width ( cm) Mass (g/ mp) Density (yarns/10cm) U Density (yarns/10cm) B Breaking force U (N) Breaking force B ( N) Breaking elongation U (%) Breaking elongation B (%) Thickness (mm) Air permeability to a depression of 200mm water column (l/m2/sec) Raw fabric 168 140 744 342 1135 1077 46 40 0.6 62.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia. .the use of lubricant deposition device permits the manufacture of single-yarn products on weaving machines. The fabrics were finished and after their analysis we could conclude that: . The operations performed had the following purposes: . . 2 . .resistance to repeated washing of minimum 100 cycles. For a general characterization of surface modifications the investigation of higroscopicity. The quantity of water absorbed (W H2O ) was determined by artificial rain method.persistency of hydrophobic effect to repeated washings in harsh conditions as well as in sterilization. absorption time and contact angle.values obtained for the mass (g/m²). elongation (%) do recommend the use of these fabrics for the production of dressings and bands with varying degrees of compressibility. treated during warping with lubricants.hydrophobic character.31 8.low weight. The characteristics of raw and finished barrier-type fabrics obtained are presented in Table 3.6 The four types of fabrics. Raw fabrics obtained were processed in the finishing department in order to ensure the specific conditions imposed.4 275 Finished fabric 163 142 774 356 1244 1071 44 35 0. Table 3: Physical and mechanical characteristics of raw and finished barrier type fabrics No. m1 (1) . The production of barrier-type fabrics To achieve this objective.5 39.3 216 The hydrophobic character of obtained materials after classical treatments was evaluated by determining the quantity of water absorbed.65 7. . .2 61 46.air permeability of 100-200 l/m /sec. in conformity with the following relation: W H 2O where: m2 m1 100 (%). 6 . to a depression of 200 mm water column. . The characteristics of the fabrics are the following: .obtaining a whiteness degree in accordance with the users’ requirements.3 8.
97 0.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia. i H.81 .0046 Permeability to vapours air.h m3/m2. t – relative humidity time = 100 %. The capacity of materials to allow the passage of vapours was evaluated by calculating the vapour permeability index (μ).94 17.10 Contact angle. by means of a device especially designed for this purpose .8 September 2012 m 1 – initial mass of the sample. 5. degrees 127 136 143 148 154 Hygroscopicity H. t – time for maintaining the sample under diffusion conditions.min 16.43 0.0067 0.228 0. Contact angle was determined directly by measuring the angle formed by a drop of distilled water deposited on the fabric surface. Vapor absorption capacity is determined by the following relation: H abs Mu Mc 100 (%). Hydrophobization Effect of plasma treatment on polyester fabrics Variant V 1b V 2b V 3b V 4b V 5b Quantity of water absorbed. g/m2. h.h % 0. Higroscopicity index (i H ) is thus calculated: iH Mu Mc .208 0.24 17. g.76 28. g/m2. water and sample). 6. S – sample surface subjected to vapor diffusion conditions. 6 .300 0. The characteristics of the plasma treated fabrics are shown in table 4.59 18.h S t (3) where: S – sample surface.38 1. in a standard atmosphere environment (RH = 65%) and wet environment (RH = 100 %)  were used. Table 4.0050 0. g/m2. g. To evaluate higroscopicity samples with the dimensions of 50 x 50 mm that were kept successively for 24 hours.78 26. in conformity with the established methodology : M . m2. g. m2.54 27.93 24. Mf – final mass of the testing set. g. g/m2.03 23. Another indicator considered relevant for characterizing the treated materials is the air permeability (P a ). Surface morphology of non-treated and treated samples was studied by SEM (scanning electron microscope). g. Hydrophilicity was evaluated by determining the absorption time of a drop of distilled water deposited on the fabric surface. M c – average mass of samples conditioned at relative humidity RH = 65 %.0059 0.h S t M M 0 M f . g (4) (5) where: M 0 – initial mass of the testing set (Herfeld glass. Low pressure plasma equipment. m 2 – sample mass after test.46 0. g.264 0. Hydrophobic treatment of textile materials for medical articles was performed with hexafloropropane (C 3 H 2 F 6 ).0052 0. The plasma treatment was realized to INCDTP by CD400 Roll-to-roll. Mc (2) where: M u – average mass of samples conditioned at relative humidity RH = 100 %. The surface images by SEM microscopy are presented in Figure 1-6.235 0.46 17. Air permeability: The air permeability of the fabrics was measured on a FX 3300 Air Permeability Tester at a test pressure of 100 Pa and a test area of 20 cm2 according to EN ISO 9237. as plasma gas. % 2. h.
g/m2.7180 Permeability to vapours air. Hydrophobization Effect of plasma treatment on cotton fabrics Variant V 1b V 2b V 3b V 4b V 5b V 6b M Quantity of water absorbed % 31.15 13. This can be explained by a decrease of pores’ dimension due to the setting of the hydrophobization product. The water and oil repellent character of the plasma treated materials is illustrated both in the very high absorption time (15000s) and in the spherical shape of the water and oil drops on their surface.84 0. The lowest values are registered for polyamide fabrics that present a higher density structure.85 0.208 0.min 15. .05 5.4531 8. the strongest modification of water repellence is registered for polyester.0463 2. g/m2.09 0.41 0.5582 9.19 0.26 Contact angle.24 50.99 48.83 16. For the synthetic fibre materials.0445 2.0046 0.99 0.55 14.98 0.54 0.99 17. A comparative analysis of the three fibres shows that the best results are obtained on cotton fabrics.96 0.11 11.60 2.0534 3. g/m2.12 2.67 It can be noticed that the amount of water absorbed by the textile materials (polyester.59 49. It is worth noting that the most intense effect in absolute value is obtained for cotton. When concentration reaches the maximum value. g/m2.03 15.fluoride compound form hexafluorpropene.02 20.29 17.52 51.39 14.72 30.0484 2. The values of the vaporization coefficients increase with the decrease of hygroscopicity and this shows that the treatment leads to fibre structure modification – they become water repellent.56 23. For higher concentration the contact angle is not significantly modified.96 16. hygroscopicity and the hygroscopicity index decreases with its increase in the treatment baths.36 16. The hydrophobic effect is reflected also by the value of the contact angle of the distilled water drop deposited on the fabric surface.42 Tabelul 5. We notice that for the three textile materials the values of the contact angles are very large compared to the untreated material due to the increase of the concentration of the fluoride product in plasma.25 48. the quantity of water absorbed is ten times lower than for the untreated sample.23 48. The quantity of water retained by the material is comparable to the values specific to untreated polyester and polyamide.360 0.0081 18.22 17.3 155 10 0.39 73.h m3/m2.01 13.50 Tabel 8.02 0.h % 3.h m3/m2.50 6.4192 12. Permeability to air decreases with the increase of the concentration of the treatment product.52 16.4346 7.h % 10. polyamide and cotton) decreases with the increase of the treatment product concentration.63 8. 6 .4887 8.82 13. degrees 124 132 138 144 150 150 70 Hygroscopicity H.13 7.0595 3.66 3.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia. i H.05 16. degrees 128 139 146 152 158 159 0 Hygroscopicity H. We should mention that the results obtained are in perfect agreement with those registered following the hexafluorpropene plasma treatment for the three materials studied.21 0.62 15.83 17. polyester and polyamide.0446 4.09 Contact angle.52 0. Hydrophobization Effect of plasma treatment on polyamide fabrics Variant V 1b V 2b V 3b V 4b V 5b V 6b M Quantity of water absorbed % 9. the capacity to retain water vapours decreases and vapours can easily cross the textile structure.min 16.0630 Permeability to vapours air. i H.4186 7.57 0.15 50.40 16.86 17. In relative value.84 14. This can be explained by the increase of the quantity of hexafluorpropene reacting with the fibre: the increase of induced water repellence is determined by the chain F 3 C-(CF 2 ) x .15 16.82 0.08 17.51 6. the decrease of retained moisture is over 110 lower.82 12.8 September 2012 V 6b M 0.
polyamide and polyester woven samples were evidenced by the SEM image analysis and are shows in figure 1-6. SEM images of untreated PA samples Figure 4.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia. Figure 1.8 September 2012 The changes in the surface properties of the cotton. SEM images of plasma-treated cotton samples Figure 3. 6 . SEM images of plasma-treated PA samples . SEM images of untreated cotton samples Figure 2.
6 .8 September 2012 Figure 5. Plasma activation treatments modify the surface characteristics of the cotton. For accomplishing the aim of this study. SEM images of plasma-treated PES samples 3. that can only be attributed to the applied fluoride product. The action of cold plasma is evidenced in the polymer destruction with the formation of small molecule and even volatile products. it was used low pressure plasma equipment from the INCDTP laboratory. Hexafloropropane (C 3 H 2 F 6 ) as plasma gas was applied on all surface of the fabrics with destination medical articles . . 4. Besides the treatments for water and oil repellence.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia.the water quantity absorbed by the plasma treated material (shown in table 8). The SEM analysis on the materials treated with hexafloropropane shows the presence of roughness on the fibre surface. the plasma treatments ensure the repellence of many other liquids including inks and alcohols. polyester and polyamide treated by hydrophobization classical treatments compared to plasma treatments have been analyzed within this paper. polyamide and polyester fibres. SEM images of untreated PES samples Figure 6. The plasma treatment and grafting of the textile materials with water repellent monomers can be an alternative to classical treatments that are more expensive and have a negative impact on the environment. 6. by formation of visible roughness. The surface modifications of the textile materials were analyzed by SEM microscopy and the images are shown in figures 1-6. This could be easily observed by SEM on the fibre surface. The analysis of experimental data for all textile materials treated with hexafloropropane indicates higher values for the absorption time and for the contact angle when compared to the untreated samples. Hexafloropropane (C 3 H 2 F 6 ) provides good properties for repellance of water and oil and other liquids compared to classical hydrophobization treatments. CONCLUSIONS The properties of the weavings accomplished from cotton. shown in figure 2. The most prominent changes in terms of absolute value are obtained for the cotton material .
Jia. F. Faculty of Natural Science and Engineering..15. I. Hou W.15. Co-author(s): Dr. A.151  Schindler.fr . A.85-90. The textile Institute and Woodhead Publishing Limited. Cambridge England.. 340. Mureşan. Mureşan.tuiasi.certex. Xu. Eng. e-mail: certex@ns. Woodhead Publishing Limited.: “Physical and Absorptive Changes in Plasma Treated Viscose Fibres“. Iasi. L.42.tuiasi.J..1016-1029..Postal code: 030508. p.: “Introduction to Complex Plasmas”. Gherardi..Postal code: 030508. Lucretiu Patrascanu 16. Ursache.ro. Bucharest. “Surface and Coatings Technology”. R.00. Wei.: “Plasma technologies for textiles”. W. webpage: http://www. 340. ISBN 90-386-2737-8/2005  Caraiman. Slovenia. 74-86 Corresponding author: Drd. Fax: (00402)1-340. 6 . U. 2000. F. Romania phone: 0040213404928 fax: 0040213405515 e-mail: certex@ns. .a: Revista Română de Textile – Pielărie. Eng. 1. 2007  Kieft.55. Bucharest. 5. Postal code :030508..49. Ioan CIOARA Department for TEXTILE. Romania Tel: (00402)1-340. 700050. 2007  Loghin C. s.8 September 2012 4.surdu@yahoo. Sommer. 6/ 2011  Shishoo.ro. Lucretiu Patrascanu 16. Adriana SUBTIRICA Department for Material Research and Investigation.D.ro.: “Tratamente de suprafaţă aplicate materialelor textile şi implicaţii asupra comportării în mediu umed”.ro. eng. Razvan RADULESCU. e-mail: certex@ns..certex.49.certex. University of Ljubljana. 2002  Alexander. Eng. Industria textila nr. F. P. “Plasmas and Polymers”. Romania Tel: (00402)1-340. Prof.  Bonitz. p.14th Romanian Textiles and Leather Conference – CORTEP 2012 Sinaia.certex. “Chemical finishing of textiles”. Lucretiu Patrascanu 16. Fax: (00402)1-340. “Gheorghe Asachi” Technical University Iasi.00.49. B. Bucharest. Carmen GHITULEASA General Director The Research-Development National Institute for Textile and Leather Address: Str.Postal code: 030508. 29.42... Dimitrie Mangeron blvd. Hauser. nr.00.. Cambridge: University Press “Plasma physics and engineering Plasma chemistry Low temperature plasma physics”/ (2008).28. Romania e-mail: icioara@tex..: “Plasma needle: exploring biomedical applications of non-thermal plasmas” Technische Universiteit Eindhoven. The Research-Development National Institute for Textile and Leather Address: Str. M.ro Eng.. Romania Tel: (00402)1-340. N.ro. 340. dr. Lilioara SURDU Department for Material Research and Investigation. lilioara. M. X. 2004.15. INCDTP Str.D.28.. Ljubljana. p. Department for Material Research and Investigation. M.55. Lucretiu Patrascanu No 16. R. Fax: (00402)1-340. e-mail: certex@ns. REFERENCES  Vrabič.42. The Research-Development National Institute for Textile and Leather Address: Str. Bucharest. E. H. Cambridge England / 2007  Wang S. Department of Textiles.28.55. Liu. 2010  Massines. The Research-Development National Institute for Textile and Leather. 10..
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