MESAPPLIED materiats ‘SXINTERFACES {© Ge This ACS Appl Mote neces XHBK 99K, K-20 won acsamiorg Thermal, Waterproof, Breathable, and Antibacterial Cloth with a Nanoporous Structure Qingxian Liu," Jun Huang,’ Jianming Zhang,’ Ying Hong,’ Yongbiao Wan,’ Qi Wang,’ Mingli Gong,’ Zhigang Wu,'"® and Chuan Fei Guo*'® "Department of Materials Science & Engineering, Southern University of Science & Technology, Shenzhen, Guangdong 1805S, China 'State Key Laboratory of Digital Manufacturing Equipment and Technology, Huazhong University of Science and Technology, Wohan 430074, China © Supporting information ABSTRACT: Wearable thermal management materials have attracted increasing attention because of the potential in energy conservation and the possibilty to mest the need of smart clothes. An ideal cloth for cold areas has to be lightweight, warm, waterproof but breathable, and antibacterial. Hezen, we presenta multifunctional cloth starting from a cotton fabric for which one side is modified to be supethydophobie by introducing sia nanopartile/poiydimethylioxane (PDMS) layer, wile the other fide is coated with a nanoporous cellulose acetate layer fllowed by depositing a thin silver film. The porosity allows the fabric to be breathable, and the slver lm plays three important roles as a. perfect ingfared reflector, a flexible heater, and an antibacterial layer. Such a multifunctional fabric might be potentially usefil in outdoor coats and other facilities KEYWORDS: porous structure, superhydrophobis, silver network, thermal control, breathability INTRODUCTION Clothing is a basic necessity of lie! Providing warmth for the human body is one of the main requirements, especially in temperate and frigid zones of the globe.” Cotton,” wool! feather,’ and chemical fbers®” have been widely used to make warm clothes, Traditional clothes provide warmth by tapping the air around the human body to decrease heat transfer via convection and conduction. However, the high emissivity (0.75-08) of common clothes provides little radiative insulation effect.” A commonly used way for further heat insulation is to increase the thickness of the clothes or wear more ayers of clothes which on the other hand make the user uncomfortable, Besides, waterproofhess i also an important aspect for such clothes. Cotton and other traditional clothes exhibit poor waterproofness, which would decrease the heat insulation performance of clothes when exposed to rain, fog. oF snow" Tt is wellknown that metals are a class of good infrared (IR) reflectors. For example, aluminized Mylar blankets perform well in blocking the radiative loss, such that they can be used as sun shields for cas. However, for clothing purpose, other performances such as light weight, high waterproofness, and high breathability should also be considered, which are not achievable by simply using metal foils oF metal membranes. Presently, a concept of “personal thermal management” is proposed as an optimal energy-saving method directly focusing ‘on maintaining the warmth in the human bedy.""""* A superior | ACS Publications thermal management material should be wearable ike common dlothes.""" An effective approach for fabricating. thermal management materials is adding conductive nanomaterialt on or inside textile Sibers, Typically, conducting nanomaterials with 4 low emissivity that form a network could effectively reflct IR. back to the body to reduce the heat loss. Such nanomaterial networks only have litle or a small adverse fect on the breathability of the fabrics because ofthe percolation network. In general, the nanoscale conductors used for thermal management inchue eazbon nanotubes (CNTs),"” graphite rnanoplatelets” graphene,”*” and metallic nanoparticle,” among, which silver nanowires are a superb choiee because of| the high IR reflection efficiency and the igh electrical conductivity of silver that allows it to be potentially used as a heater. However, silver nanowites ate expensive, typically at a price of ~$400 per gram, about 3 orders of magpitude higher than bulk silver while the IR reflection eficiency of a ver nanowire network i stil far lower than that of metal fils or flms. In addition, silver nanowires may also. present the dinadvantages of poor adhesion to the textile. Ta thie study, we ered a normal cotton textile asthe substrate to fabricate « moliinctional cloth by constructing a hydro phobic coating on one side and 2 nanoporous structure Received: October 28, 2017, Accepted: December 21,2017 Pablishes December 21, 2017,ACS Applied Materials & Interfaces a vero a sicaNPs Coton ne Figure 1. Preparation of the multifunctional doth. (1) Schematic ofthe preparation proces (S) Low-magication SEM image of psce of normal cotton clot) SEM image of eotton yar. () SEM image ofthe sia NP/PDMS treated ib c) Detaled morphology of ee sea NP/PDMS layer (4) SEM inages of the sure morphology of ellos acetate a diferent magnons, (h1) SEM images ofthe metal ver etwork on the close aecate porous patter with diferent magaiatons Sele bars 200 jm panel bl 10pm in anes ce SO pm in panel 2 ym panel gy I yon in panels hj and the inset in panel followed by depositing a metalic film on the other side. The outer layer exhibits a water contact angle of 161° and a sliding angle of less than 5°, which effectively prevent the entry of water from the outside. The porous layer is a cellulose acetate thin film with dense nanopores that are beneficial to the high Deeathabilty and the improvement of the surface flatness of the whole textile, and the metallic silver network deposited on the porous layer can effectively reflect IR from the human body and. also be used as heater to provide additional Joule heat beyond the passive insulation by loading a small voltage. In this way, the multifunctional cloth can not only maintain the original nature of the cotton textile with high breathability but also ‘possess significant properties including waterproofness, anti fouling property, IR reflection, Joule heat generation, and antibacterial activities, Such @ fabric might find wide applications in clothing, outdoor sports, and so forth PREPARATION OF THE MULTIFUNCTIONAL ‘CLOTH ‘The preparation of the multifmetional cloth i shown as a schematic in Figure Ja, A common cotton textile is used as the substrate for the following procedure, Fics, we modify the surface of the normal cotton textile by introducing a silica rnanopattcle (NP)/polydimethyisioxane (PDMS) coating to make the surface superhydrophobic, After that, a cellulose acetate/acetone/IL. solution is coated on the other side of the cotton textile and immersed into 2 water bath leading to the formation ofa porous cellulose acetate film. A silver film is then deposited on the porous structures by using thermal evaporation, forming a aver network following the shape of the porous cellalose acetate flm (Figure S1). igure Ibje shoves the scanning electron microscopy (SEM) mages of the morphology of the cotton texile material. The rateral is basicaly a loosely woven textile structure which consists of cotton yam of 200 jm diameter with an interyarn space of 200 jm, 'The surfce ofeach fber is generally smooth. Aller introducing the silica NP/PDMS lays, small sea NPs ate distebuted on the surlace of the cotton fibers, as shown in Figure Ide. Here, PDMS plays as an adhesive wrapped around the silica NPs on the cotton fibers, and the hydrophobic silica NPs generate a dusbatze surface roughness to improve the hydrophobicity of the cloth, The detailed preparation procedure of the superhydrophabic layer is shown in Figure 52. On the other side ofthe textile, the porous cellulose acetate film Iooks smooth when inspected using SEM at a low magnification (Figuce 19. However; the high magnification SEM image indicates thatthe film consists of dense pores with an average diameter of ~$00 nm and a wall thickness of ~70 fam (Figure 1g), as a result of phase separation. It is worth noting thatthe pores are penetrated throughout the cellulose acetate membranes, and the pore interconnectivity ie exhibited in the crose-rectional image shown in the inset of Figure Ig Immersion precipitation has been employed for the fabrication of the polymeric porous film:"—* The precipitant i usually riscible with the solvent but itamiscible with the polymer During the phase separation, the solid polymersich phase forms the walls and the liquid polymerlean phase forms the pores.” Herein, the cellulose acstate/acetone/IL solution is coated on the cotton textile and immersed into a water bath toACS Applied Materials & Interfaces * ime (h) g ‘Water contact angle’) Figure 2. Wetsbilty ofthe coton tele before and ater coating sen NPs. (a) Water deop (2 i.) on the untested cotton tet, showing 2 contact angle close to 0°. (b) Unteated normal cotton cath i pllated when immersed in diay water. (c) Untreated cotton texte is completely instated with dns water drop. (8) Water deop (2 HL) om te otto textile wth sien NP, shoving a contact angle of ~161" anda ding angle less than 5°. (e) Alter hydrophobic treatment the cotton fibre becomes anfouling to dity water (0 Ditty water drops on the treated fabri, showing a remarkable antifouling propery. (g) Change of water contact ange with vlrasonie cleaning duration. (b) SEM image ofthe coating surface aller 66 b of ultasoncation. Sale bats are Tera in panels ef and 5 am tn panel Womat cotton clotn b c ES eet ‘transmittance (%) 2 ene —— eel cel as ; es fal 2 gs 3a eel on tt as el ac ry 5 = BF ad os. | | * 5 % a8) ewereser Fee a Figure 3. (a) Transmittance of the normal cloth, Ag nanowire cloth, Ag lm, and the multfenctional cloth observed using an Fourier transform infrared mizoscope.(b) Thermal image of a normal cloth on a hand. (e) Thermal image of a multunctignl cloth on a hand. (d) Heat taster measurement bythe temperature increase when placing the cloth at diferent fabrication stages on an open-air hot pate of 33°C. (e) Temperature change v ime ater applying diferent yltages toa cin X 2 em sample ofthe mullifnctional cloth, (2) Change ofthe sheet restance asa fonction of number of bende ata bending racivs of $ mm. form the porous film (Figure $3). Note that this porous layer surface of the textile. The SEM images (Figure 1h) show that also fills up the gaps that are between the cotton yar, and this the silver film follows well the morphology of the porous allows the subsequent porous silver film to cover the entire cellulose acetate but with a pore size slightly smaller than theACS Applied Materials & Interfaces Moisture permeation (mg/cm?) Time (h) Figure 4 (a) Mac increas of desiccante sealed with diferent fbrice. Inst isthe corresponding photograph ofthe botles sealed bythe following clothe: (1) normal cotton cloth, (2) sea NPs/eotton, (3) ses NPs/cotton/celose acetate, and (4) sea NPs/cotton/eellloseacetate/sllver (b-e) Antibiotic test of (b) normal coton cloth, (c) silica NPs/cottn, (d) sce NPs/eatton/celulose acetate, and (c) silica NPs/cotton/cellulose aclate/sver (malufuneional oth withthe slvr fm facing down). Sele basin panels b~e ae ll OS em oiginal pore size (~S00 nm) of the exlllose acetate pattern The coresponding specimens at each stage are shown i Figure SA I WATERPROOFNESS The cotton fabric coated with silica NPs exhibits super. hydrophobicity. As shown in Figure 2a, when a drop of water fills onto the untreated cotton fabric, the water wets the fabric immediately with water contact angle approaching 0° because of complete infltration. By contrast, after coating with a silica NP/PDMS layes, the water contact angle of the textile dramatically increases to 161°, while the sling angle is less than $° (Figure 2d), indicating an extraordinary waterproofness (shown in Figure S5). In. addition, the treated super- hydrophobic textile also exhibits antifouling function in dirty water as indicated in the case with red chalk powders dissolved in water. As shown in Figure 2b. the original cotton cloth is dyed red by immersing into dirty water within a short time, whereas the superhydrophobie cotton fabric shows a remarkable antifouling ability in dirty water (Figure 269. Furthermore, the washing durability was evaluated by ultra sonication in a mixed solution of water and ethanol. The change of the water contact angle is less than 9° after 66 b of ultrasonication, indicating that the cloth might be durable to washing (Figure 2g). The SEM observation reveals that the coating surface still etains its rough morphology ater 66 b of tltrasonication (Figure 2h). This simple and low-cost coating shows a remarkable superhydrophobic property that is potentially useful for waterproof and self-cleaning protective tents THERMAL CONTROL, ELECTRICAL PROPERTY, ‘AND DURABILITY “The pore diameter ofthe conductive metalhi siver network is far smaller than the wavelength of the blackbody radiation of| the human body which is centered at 9 jm, indicating thatthe cloth can effectively reflect human body radiation, The transmittance spectra of the normal cloth, Ag nanowire cloth (Figure S6), Ag film, and multifunctional eloth are compared in Figure 3a The average transmittance in the range of 25-16 um for the multifunctional cloth is close to ~0%, which is significantly lower than that ofthe Ag nanowire cloth (20.6%) and normal cotton cloth (72.3%) and almost completely ‘overlaps with that of the continuous silver films. The low IR transmittance clearly indicates that the multifunctional cloth is 2 perfect IR reflector and, therefore, suitable to trap the thermal radiation around the human body. Figure 3b illustrates the ‘thermal images of a human hand with a normal cloth and with a ‘multifunctional cloth attached on, respectively, Both specimens are in thermal equilibrium on the palm before imaging at a ppalm temperature of 333 °C and an atmosphere temperature 9 25.0 °C. For the normal cotton cloth, the textile emits IR in a temperature range of 31.732.7 °C as detected by using an IR camera. By contrast, the IR camera shows thatthe temperature of the multifunctional cloth on palm is lower, in the range of 304-31.1 °C, indicating a decrease of 13-16 °C compared with that of the normal cotton cloth. Although the multifune tional cloth is tested under the same temperature as the normal cotton cloth, the low emissivity of the silver network induces lower thermal radiation making the multifunetional cloth cooler in the thermal images, ‘The results prove that the multifune tional cloth is an effective IR reilector that can effectively decrease the heat loss fzom the human body. We have further compared the heat transfer property of the normal cloth and the multifunctional cloth by putting them on an open-air hot plate and testing the surface temperature. In principle, the larger the difference in temperature between the hot plate top, and the upper surface of the sample, the better the thermal insulation is. The hot plate is set to 38 °C to simulate the Ihuman skin temperature, From Figure 3d, the multifunctional cloth has a 93% and a 26% increase in temperature difference compared with the normal cotton cloth and the silica NP/ cotten/cellulose acetate cloth, respectively, indicating that the thermal insulation is a collective elect of the silver network and the porous doth, ‘he silver network has a sheet resistance of 2.84 0/sq, and ssuch a highly conducting layer ean also be used at a heater ‘Figure Se shows time-dependent temperatures of a 2 cm X 2 ‘em sample at applied voltages of 05, 12, and LS V. The low sheet resistance of the multinctional cloth enables the generation of Joule heating at a low voltage. At a room, temperature of 25 °C, an applied voltage of only 0.5 V can induce a temperature up to 34.1 °C, higher than the average skin temperature of 33 °C. Note that the voltage we tested is safe for the buman body. To identity the durability of the silver network under repeated deformations, we have measured theACS Applied Materials & Interfaces ‘Table 1. Comparison of the Properties of the Normal Cotton Cloth, Ag Nanowire Cloth, and Multifunctional Cloth” sample CA (deg) IR raamtaes (8) AT (°C) rommal catton dosh ~0 ms 1s 202 Agranowie doth 0 ans 1207 rmultfinciona doth 161-22 0 ap £02 ‘moisture permeation (mg/(cm'h)} temperature at 0.S V (°C) antibacterial 102 2s s oo sea rm oon a re “CA, water contact angle on the outside ofthe cloth; AT's the diferencia temperature between the hot plate top (38 °C) and the upper surice of the cloth sheet resistance under realtime cyclic bending at a bending radius of 5 mm for 1000 cycles (Figure 3f), and the sheet resistance shows only a 18.4% increase. Such a small change in sheet resistance typically does not have a perceptible effect on, heating. The wear rate of the cloth is also shown in Figure S7. Although the wear rate inereases with the increasing number of abrasion cycles, iis still in an acceptable range, indicating that the cloth is durable under mechanical wear I BREATHABILITY AND ANTIBACTERIAL PROPERTY ‘The multifunctional cloth has a silica NP/PDMS coating on cone side and a porous cellulose acetate film covered by a silver fm on the other side. Especially, the porous cellulose acetate fm ills up the gaps between the cotton yarn, and itis therefore necessary to investigate the effect of the added layers on breathability. The breathability of both the multifunctional cloth and the normal cotton cloth is characterized by the mass increase of the desiceant in a bottle sealed by the respective cloth. Water vapor permeates through the cloth and gets absorbed by the desiccant, leading to a weight gain over time, ‘The multifunctional cloth can still maintain its good breath- ability, with a weight gain rate reduction of only ~4% compared, with the normal cotton cloth (Figute 4a), All samples were tested in the same time duration and under the same environment to avoid possible deviation in ambient temper ature and humidity. The result indicates that the mine tional cloth exhibits high breathability and ensures comfortable ‘wearing feeling with the aid of porous nature, Besides, the ‘multifunctional cloth also exhibits the antibacterial property, probably becaute nanoscale silver is an effective antibacterial material. As shown in Figure be, an empty gap around the multifunctional cloth reveals its ability to suppress the growth, ‘of bacteria, winereas nether the normal cloth nor those without the deposition of silver show this antibiotic effec. The multifunctional cloth can restrain the reproduction of bacteria, and lengthen the lifespan of the personal thermal management doth. Ml ROLE OF THE NANOPOROUS CELLULOSE ACETATE FILM ‘The porous clilose acetate film plays several important roles Frist, the hydeophii and high-porosity materials maintain the good hygroscopicity and breathabity ofthe fabric. The well interconnected nanopores with hydrophilicity penetrate Ahvoughout the whole fm, allowing water vapor to dfs fom one side tothe other (Figure $8), which is fundamental for heat balance and comfort. The resistance to difsion in perforated fs has been studied,” given as bond? ~ prints + @ ‘where tis the thickness ofthe film, dis the average diameter of the pores, isthe percentage area ofthe pores and Ry is the x, resistance ofthe ‘il in centimeters of stil at: From eq 1, the water vapor transmission through the surface increases as the ppore size decreases on a constant porosity and thickness. ‘Therefore, the interconnected nanopores contribute positively to the breathability of the cloth. This might be the reason that although the large gaps (between the fiber yarn, ~200 um) are filled up with the nanoporous fm, the breathability of the teatile has a litle change. A cloth that is both waterproof and breathable provides the wearer with a high level of comfort in many situations Second, the porous film fills up the sub-milmeter holes between the cotton yam and thus increases the effective area of the IR reflector with a factor of ~33% (the area faction of the ‘gaps in the original cotton fiber), In addition, the metal film deposits not only on the walls between the nanopores but also fils inside the nanopores, thus offering an ideal IR reflection ‘effect close to that of a smooth metal film and better than that of silver nanowires. This i the reason that our cloth exhibits fll IR reflectance “Third, the porous structure acts as a template for silver deposition, and the corresponding silver network offers a better durability than loosely assembled one-dimensional silver nanowires. Typically, silver nanowite suspension is quite expensive, whereas depositing s metal film is relatively cheaper. ‘The metal network can be formed not only by using vacuum deposition but also by chemical plating and other methods. The deposited metal type can be diverse: other cheaper metals such as coppes, nickel, and aluminum could also be deposited (Figure 59), i MULTIFUNCTION OF THE CLOTH Some iteratue has reported smart clothes that meet diferent ‘requirements, such as waterproof elothes,”° energy harvesting clothes,"'~"*' antibacterial clothes,"~"” and energy _manage- ment clothes." However, these clothes typically have only a Single finction. In comparison, the multnetioal doth we developed has a series of properties including waterprooinss, ‘breathability antibacterial activity, and personal thermal control (as given im Tbe 1), Such 2 cloth with malttnesons wil allow for diese applications tnder harsh conditions. In ‘dition, although the superhydcophobie feature makes it Gifcl to wash st the cloth oat on water, the antifoling and Sntbacterl properties allowr our cloth to be washees We have alo tried dy cleaning, andthe electrical resistance of the cloth exhibits only a slight increase afer several eyes of dry leaning tests (Figure S10). CONCLUSIONS In conclusion, we have fabricated a multifunctional cloth with a superhydrophobic silica NP/PDMS layer on one side and a metalic silver network templated by a porous film on the other surface. ‘The multifunctional cloth not only maintains the original nature of cotton textile with a high breathability and flexibility but also possesses other desired properties includingACS Applied Materials & Interfaces ‘waterproofness, antibacterial activity, IR reflection, and the ability to generate Joule heat. The porous cellulose acetate film plays important roles: it increases the IR reflection efficiency and maintains the high breathability. This multifunctional doth might have practical applications in wearable electronics and smart garments and offers a new design consideration for thermal control. ASSOCIATED CONTENT © Supporting Information ‘The Supporting Information is available fice of charge on the ACS Publications website at DOL: 10.1021 /acsami:7b16422, Materials required; methods of preparation of the ‘waterproof layer, cellulose acetate porous film, and Ag network layer; characterization analysis of the mliune tional cloth; cross-sectional SEM image of the mult: functional cloth; schematic procedure of the preparation, of the superhydrophobie cotton textile; SEM images of the membrane surfaces with varying cellulose acetate concentrations; images of the textiles at diferent stages; seaterproofness testing of the textile; wear rate plot for the multifunctional cloth; optical photographs showing. time-dependent water contact angles; SEM images of the ‘Ag nanowize cloth and nickel network cloth; and the change of resistance of the multifunctional cloth after several dry cleaning eyeles (PDF) AUTHOR INFORMATION Corresponding Author “Boma: guoci@eusteedacn orciD® Zhigang Wa: co00.00023719-s05% ‘Chuan Fei Guo: 000.00034513:3117 ‘Author Contributions QL. and CEG. conceived the idea and designed the experiments, QL. and JH. fabricated the multifunctional dloth and measured the water contact angle, infared spectrum, thermal imaging, breathability, bending experiment, and Joule heating. JZ. and M.G, conducted the SEM. characterization YH. and YW. drow the schematic diagram, QW. conducted the antibiotic test. QL. and CEG. analyzed the data and co: wrote the paper, All the authors disused the result of the ‘whole pape. Notes The authors declare no competing financial interes. I ACKNOWLEDGMENTS ‘The work was financially supported by the fonds of the waangdong Innovative and Entrepreneurial Research ‘eam Program” under contract no. 2016ZTOSGSS7, the National Natural Seience Foundation of China (no. U1613204), the “Science Technology and Innovation Committee of Shenzhen Municipality” (grant no. JC¥J20160613160524995), and the “Peacock Plan” (no. YOI2S6120). REFERENCES (1) Ross, R. Clothing: A Global History; Polity Press: Cambridge, 2008, (2) Mointye, D. A; Gniiths, LD. The eects of added clothing on warmth and comfort in cool conditions. Ergonomiss 1975, 18, 205~ aL (8) Vivekaalan, M. 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