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Stearic acid (SA) imagwiritsidwa ntchito ngati zinthu zosinthira gawo (PCM) m'zida zosungira mphamvu. Mu kafukufukuyu, njira ya sol-gel idagwiritsidwa ntchito poyika microcapsulate ya SiO2 shell surfactant. Kuchuluka kosiyanasiyana kwa SA (5, 10, 15, 20, 30, ndi 50 g) kudayikidwa mu 10 mL ya tetraethyl orthosilicate (TEOS). Zinthu zosinthira gawo lopangidwa ndi microencapsulated (MEPCM) zidadziwika ndi Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ndi scanning electron microscopy (SEM). Zotsatira za zizindikiro zidawonetsa kuti SA idayikidwa bwino ndi SiO2. Thermogravimetric analysis (TGA) idawonetsa kuti MEPCM ili ndi kukhazikika kwa kutentha kuposa CA. Pogwiritsa ntchito differential scanning calorimetry (DSC), zidapezeka kuti enthalpy value ya MEPCM sinasinthe ngakhale patatha nthawi 30 zotenthetsera-kuzizira. Pakati pa zitsanzo zonse za microencapsulated, 50 g ya SA yokhala ndi MEPCM inali ndi kutentha kwakukulu kobisika kwa kusungunuka ndi kulimba, komwe kunali 182.53 J/g ndi 160.12 J/g, motsatana. Mtengo wokwanira wa phukusi unawerengedwa pogwiritsa ntchito deta ya kutentha ndipo mphamvu yapamwamba kwambiri ya chitsanzo chomwecho inali 86.68%.
Pafupifupi 58% ya mphamvu zomwe zimagwiritsidwa ntchito mumakampani omanga zimagwiritsidwa ntchito kutentha ndi kuziziritsa nyumba1. Chifukwa chake, chinthu chofunikira kwambiri ndikupanga njira zamagetsi zogwira mtima zomwe zimaganizira kuipitsidwa kwa chilengedwe2. Ukadaulo wotentha wobisika pogwiritsa ntchito zida zosintha magawo (PCM) ukhoza kusunga mphamvu zambiri pakusintha kwa kutentha kochepa3,4,5,6 ndipo ungagwiritsidwe ntchito kwambiri m'magawo monga kusamutsa kutentha, kusunga mphamvu ya dzuwa, ndege ndi mpweya wabwino7,8,9. PCM imayamwa mphamvu yotentha kuchokera kunja kwa nyumba masana ndikutulutsa mphamvu usiku10. Chifukwa chake, zida zosintha magawo zimalimbikitsidwa ngati zida zosungira mphamvu yotentha. Kuphatikiza apo, pali mitundu yosiyanasiyana ya ma PCM monga solid-solid, solid-liquid, liquid-gas ndi solid-gas11. Pakati pawo, zida zodziwika kwambiri komanso zomwe zimagwiritsidwa ntchito pafupipafupi ndi zida zosintha magawo zolimba ndi solid-liquid phase ndi solid-liquid phase. Komabe, kugwiritsa ntchito kwawo kumakhala kovuta kwambiri chifukwa cha kusintha kwakukulu kwa volumetric kwa zida zosintha magawo amadzimadzi ndi solid-gas phase.
PCM imagwiritsa ntchito zinthu zosiyanasiyana chifukwa cha makhalidwe ake: zomwe zimasungunuka kutentha komwe kuli pansi pa 15°C zitha kugwiritsidwa ntchito mu makina oziziritsira mpweya kuti zisunge kutentha kozizira, ndipo zomwe zimasungunuka kutentha komwe kuli pamwamba pa 90°C zitha kugwiritsidwa ntchito mu makina otenthetsera kuti zipewe moto12. Kutengera ndi momwe zimagwiritsidwira ntchito komanso momwe zimasungunukira, zinthu zosiyanasiyana zosintha magawo zapangidwa kuchokera ku mankhwala osiyanasiyana achilengedwe ndi osapangidwa 13,14,15. Parafini ndiye chinthu chosinthira magawo chomwe chimagwiritsidwa ntchito kwambiri chomwe chili ndi kutentha kobisika kwambiri, chosawononga, chotetezeka komanso chomwe chimasungunuka kwambiri16,17,18,19,20,21.
Komabe, chifukwa cha kutentha kochepa kwa zinthu zosinthira gawo, ziyenera kuyikidwa mu chipolopolo (gawo lakunja) kuti zisatayike pa zinthu zoyambira panthawi yosintha gawo22. Kuphatikiza apo, zolakwika pakugwira ntchito kapena kupanikizika kwakunja kumatha kuwononga gawo lakunja (cladding), ndipo zinthu zosinthira gawo losungunuka zimatha kuchitapo kanthu ndi zinthu zomangira, zomwe zimapangitsa kuti zitsulo zomangika ziwonongeke, motero kuchepetsa ntchito ya nyumbayo23. Chifukwa chake, ndikofunikira kupanga zinthu zosinthira gawo lozunguliridwa ndi zinthu zokwanira za chipolopolo, zomwe zingathetse mavuto omwe ali pamwambapa24.
Kuyika zinthu m'magawo ang'onoang'ono (microencapsulation) pazinthu zosinthira magawo kumatha kuonjezera kutentha ndikuchepetsa kusinthika kwa chilengedwe, komanso kuwongolera kusintha kwa voliyumu. Njira zosiyanasiyana zapangidwa kuti zigwiritsidwe ntchito poyika zinthu m'magawo ang'onoang'ono (PCM encapsulation), zomwe ndi interfacial polymerization25,26,27,28, in situ polymerization29,30,31,32, coacervation33,34,35 ndi sol-gel processes36,37,38,39. Formaldehyde resin ingagwiritsidwe ntchito poyika zinthu m'magawo ang'onoang'ono (microencapsulation40,41,42,43). Ma resin a Melamine-formaldehyde ndi urea-formaldehyde amagwiritsidwa ntchito ngati zinthu za chipolopolo, zomwe nthawi zambiri zimatulutsa formaldehyde yoopsa panthawi yogwira ntchito. Chifukwa chake, zinthuzi siziloledwa kugwiritsidwa ntchito poyika zinthu m'magawo. Komabe, zinthu zosinthira magawo zomwe zimakhala zachilengedwe kuti zisungidwe mphamvu yotentha zitha kupangidwa pogwiritsa ntchito ma nanocapsules osakanizidwa kutengera mafuta acids ndi lignin 44.
Zhang et al 45 et al adapanga lauric acid kuchokera ku tetraethyl orthosilicate ndipo adatsimikiza kuti pamene chiŵerengero cha voliyumu cha methyltriethoxysilane ndi tetraethyl orthosilicate chikuwonjezeka, kutentha kobisika kumachepa ndipo hydrophobicity pamwamba imawonjezeka. Lauric acid ikhoza kukhala chinthu chofunikira komanso chothandiza kwambiri cha ulusi wa kapok46. Kuphatikiza apo, Latibari et al. 47 adapanga ma PCM okhala ndi stearic acid pogwiritsa ntchito TiO2 ngati chipolopolo. Zhu et al. adakonza n-octadecane ndi silicone nanocapsules ngati ma PCM omwe angakhale 48. Kuchokera ku ndemanga ya mabuku, n'zovuta kumvetsetsa mlingo wovomerezeka wopanga zinthu zogwira mtima komanso zokhazikika zosinthika gawo.
Chifukwa chake, malinga ndi zomwe olembawo akudziwa, kuchuluka kwa zinthu zosintha magawo zomwe zimagwiritsidwa ntchito popangira microencapsulation ndi gawo lofunikira kwambiri popanga zinthu zosinthika magawo zomwe zimakhala zogwira mtima komanso zokhazikika. Kugwiritsa ntchito zinthu zosiyanasiyana zosintha magawo kudzatithandiza kufotokoza bwino makhalidwe osiyanasiyana ndi kukhazikika kwa zinthu zosintha magawo zomwe zimakhala zozungulira. Stearic acid (mafuta acid) ndi chinthu choteteza chilengedwe, chofunikira pazachipatala komanso chotsika mtengo chomwe chingagwiritsidwe ntchito kusunga mphamvu yotentha chifukwa chimakhala ndi mphamvu yayikulu ya enthalpy (~200 J/g) ndipo chimatha kupirira kutentha mpaka 72 °C. Kuphatikiza apo, SiO2 siiyaka moto, imapereka mphamvu yayikulu yamakina, kutentha kwa kutentha komanso kukana bwino mankhwala kuzinthu zapakati, ndipo imagwira ntchito ngati chinthu cholimba kwambiri pomanga. Simenti ikasakanizidwa ndi madzi, ma PCM osakhazikika bwino amatha kusweka chifukwa cha kuwonongeka kwa makina komanso kutentha kwambiri (kutentha kwa madzi) komwe kumachitika m'nyumba zazikulu za konkriti. Chifukwa chake, kugwiritsa ntchito microencapsulated CA yokhala ndi chipolopolo cha SiO2 kungathe kuthetsa vutoli. Chifukwa chake, cholinga cha kafukufukuyu chinali kufufuza momwe ma PCM opangidwa ndi njira ya sol-gel amagwirira ntchito pomanga. Mu ntchitoyi, tinaphunzira mwadongosolo kuchuluka kosiyanasiyana kwa SA (monga zinthu zoyambira) kwa 5, 10, 15, 20, 30 ndi 50 g zomwe zili mu zipolopolo za SiO2. Kuchuluka kokhazikika kwa tetraethylorthosilicate (TEOS) mu voliyumu ya 10 ml kunagwiritsidwa ntchito ngati njira yoyambira yopangira chipolopolo cha SiO2.
Reactive grade stearic acid (SA, C18H36O2, melting point: 72°C) monga chinthu chachikulu chinagulidwa ku Daejung Chemical & Metals Co., Ltd., Gyeonggi-do, South Korea. Tetraethylorthosilicate (TEOS, C8H20O4Si) ngati yankho loyambira idagulidwa ku Acros Organics, Geel, Belgium. Kuphatikiza apo, absolute ethanol (EA, C2H5OH) ndi sodium lauryl sulfate (SLS, C12H25NaO4S) zidagulidwa ku Daejung Chemical & Metals Co., Ltd, Gyeonggi-do, South Korea, ndipo zidagwiritsidwa ntchito ngati zosungunulira ndi zosungunulira, motsatana. Madzi osungunuka amagwiritsidwanso ntchito ngati zosungunulira.
Kuchuluka kosiyanasiyana kwa SA kunasakanizidwa ndi magawo osiyanasiyana a sodium lauryl sulfate (SLS) mu 100 mL ya madzi osungunuka pogwiritsa ntchito magnetic stirrer pa 800 rpm ndi 75 °C kwa ola limodzi (Table 1). Ma emulsion a SA anagawidwa m'magulu awiri: (1) 5, 10 ndi 15 g ya SA inasakanizidwa ndi 0.10 g ya SLS mu 100 ml ya madzi osungunuka (SATEOS1, SATEOS2 ndi SATEOS3), (2) 20, 30 ndi 50 g ya SA inasakanizidwa ndi 0.15, 0.20 ndi 0.25 g ya SLS inasakanizidwa ndi 100 ml ya madzi osungunuka (SATEOS4, SATEOS5 ndi SATEOS6). 0.10 g ya SLS inagwiritsidwa ntchito ndi 5, 10 ndi 15 g ya SA kuti apange ma emulsions ofanana. Pambuyo pake, anaganiza zowonjezera kuchuluka kwa SLS ya SATEOS4, SATEOS5 ndi SATEOS6. Gome 1 likuwonetsa ma ratio a CA ndi SLS omwe amagwiritsidwa ntchito kupeza mayankho okhazikika a emulsion.
Ikani 10 ml TEOS, 10 ml ethanol (EA) ndi 20 ml madzi osungunuka mu beaker ya 100 ml. Kuti muphunzire momwe ma ratio osiyanasiyana a SA ndi SiO2 amagwirira ntchito, coefficient ya synthesis ya zitsanzo zonse idalembedwa. Chosakanizacho chinasakanizidwa ndi magnetic stirrer pa 400 rpm ndi 60°C kwa ola limodzi. Kenako yankho la precursor linawonjezedwa pang'onopang'ono ku emulsion yokonzedwa ya SA, linasakanizidwa mwamphamvu pa 800 rpm ndi 75 °C kwa maola awiri, ndikusefedwa kuti mupeze ufa woyera. Ufa woyera unatsukidwa ndi madzi osungunuka kuti uchotse SA yotsala ndikuumitsidwa mu uvuni wa vacuum pa 45°C kwa maola 24. Zotsatira zake, SC yosungunuka yokhala ndi chipolopolo cha SiO2 idapezeka. Njira yonse yopangira ndi kukonzekera kwa microencapsulated SA ikuwonetsedwa pa Chithunzi 1.
Ma microcapsule a SA okhala ndi chipolopolo cha SiO2 adakonzedwa pogwiritsa ntchito njira ya sol-gel, ndipo njira yawo yolumikizira ikuwonetsedwa mu Chithunzi 2. Gawo loyamba limaphatikizapo kukonzekera emulsion ya SA mu yankho lamadzi ndi SLS ngati surfactant. Pankhaniyi, kumapeto kwa hydrophobic kwa molekyulu ya SA kumalumikizana ndi SLS, ndipo kumapeto kwa hydrophilic kumalumikizana ndi mamolekyu amadzi, ndikupanga emulsion yokhazikika. Chifukwa chake, magawo a hydrophobic a SLS amatetezedwa ndikuphimba pamwamba pa dontho la SA. Kumbali ina, hydrolysis ya mayankho a TEOS imachitika pang'onopang'ono ndi mamolekyu amadzi, zomwe zimapangitsa kuti TEOS yolumikizidwa ndi hydrolyzed ipangidwe pamaso pa ethanol (Chithunzi 2a) 49,50,51. TEOS yolumikizidwa ndi hydrolyzed imachitika ndi condensation reaction, pomwe n-hydrolyzed TEOS imapanga magulu a silica (Chithunzi 2b). Magulu a silica adazunguliridwa ndi SA52 pamaso pa SLS (Chithunzi 2c), yomwe imatchedwa microencapsulation process.
Chithunzi chojambula cha microencapsulation ya CA yokhala ndi chipolopolo cha SiO2 (a) hydrolysis ya TEOS (b) condensation ya hydrolyzate ndi (c) encapsulation ya CA yokhala ndi chipolopolo cha SiO2.
Kusanthula kwa mankhwala a bulk SA ndi microencapsulated SA kunachitika pogwiritsa ntchito Fourier transform infrared spectrometer (FT-IR, Perkin Elmer UATR Two, USA) ndipo ma spectra adalembedwa pakati pa 500 mpaka 4000 cm-1.
Choyezera kuwala cha X-ray (XRD, D/MAX-2500, Rigaku, Japan) chinagwiritsidwa ntchito pofufuza magawo a bulk SA ndi zinthu za microcapsule. Kusanthula kwa kapangidwe ka X-ray kunachitika pa 2θ = 5°–95° ndi liwiro la kusanthula la 4°/min, pogwiritsa ntchito kuwala kwa Cu-Kα (λ = 1.541 Å), momwe ntchito imagwirira ntchito ya 25 kV ndi 100 mA, mu mawonekedwe osanthula mosalekeza. Zithunzi za X-ray zinapangidwa pa 2θ = 5–50°, popeza palibe chiwopsezo chomwe chinawonedwa pambuyo pa 50° m'zitsanzo zonse.
Kujambula zithunzi za X-ray photoelectron spectroscopy (XPS, Scienta Omicron R3000, USA) kunachitika pogwiritsa ntchito Al Kα (1486.6 eV) ngati gwero la X-ray kuti timvetse momwe mankhwala alili mu bulk SA komanso zinthu zomwe zili mu encapsulation. Ma XPS spectra omwe adasonkhanitsidwa adakonzedwa kufika pa C 1s peak pogwiritsa ntchito exotic carbon (mphamvu yomangira 284.6 eV). Pambuyo pokonza maziko pogwiritsa ntchito njira ya Shirley, ma high-resolution peaks a chinthu chilichonse adachotsedwa ndikuyikidwa ku ntchito za Gaussian/Lorentzian pogwiritsa ntchito pulogalamu ya CASA XPS.
Kapangidwe ka bulk SC ndi microencapsulated SC kanawunikidwa pogwiritsa ntchito scanning electron microscopy (SEM, MIRA3, TESCAN, Brno, Czech Republic) yokhala ndi energy-dispersive X-ray spectroscopy (EDS) pa 15 kV. SEM isanajambulidwe, zitsanzozo zinapakidwa platinamu (Pt) kuti zipewe kuwononga mphamvu.
Kapangidwe ka kutentha (malo osungunuka/kulimba ndi kutentha kobisika) ndi kudalirika (kusinthasintha kwa kutentha) zinatsimikiziridwa ndi differential scanning calorimetry (DSC, TA Instrument, Discovery DSC, Newcastle, USA) pa kutentha/kuzizira kwa 10 °C/min pa 40 °C. ndi 90 °C ndi nayitrogeni yopukutidwa mosalekeza. Kusanthula kuchepetsa thupi kunachitika pogwiritsa ntchito TGA analyzer (TA Instrument, Discovery TGA, New Castle, USA) mu kuyenda kosalekeza kwa nayitrogeni kuyambira pa kutentha kwa 40–600 °C, ndi kutentha kwa 10 °C/min.
Chithunzi 3 chikuwonetsa ma spectra a FTIR a bulk SC komanso ma microencapsulated SC (SATEOS1, SATEOS2, SATEOS3, SATEOS4, SATEOS5 ndi SATEOS6). Ma high absorbation pa 2910 cm-1 ndi 2850 cm-1 m'zitsanzo zonse (SA komanso ma microencapsulated SA) amachitiridwa ndi ma symmetrical stretching vibrations a magulu a –CH3 ndi –CH2, motsatana10,50. Ma high pa 1705 cm-1 amachitiridwa ndi vibrational stretching ya C=O bond. Ma high pa 1470 cm-1 ndi 1295 cm-1 amachitiridwa ndi in-plane bending vibrate ya gulu la –OH functional, pomwe ma high pa 940 cm-1 ndi 719 cm-1 amachitiridwa ndi in-plane vibrate ndi yield. -plane deformation vibrate, motsatana - gulu la OH. Ma peak a kuyamwa kwa SA pa 2910, 2850, 1705, 1470, 1295, 940 ndi 719 cm-1 adawonedwanso mu SA yonse yokhala ndi microcapsulated. Kuphatikiza apo, peak yatsopano yomwe idapezeka pa 1103 cm-1 yofanana ndi kugwedezeka kwa kufalikira kwa gulu la Si-O-Si idawonedwa mu microcapsule ya SA. Zotsatira za FT-IR zikugwirizana ndi Yuan et al. 50 Adakonza bwino SA yokhala ndi microcapsulated mu chiŵerengero cha ammonia/ethanol ndipo adapeza kuti palibe kuyanjana kwa mankhwala komwe kunachitika pakati pa SA ndi SiO2. Zotsatira za kafukufuku wa FT-IR wapano zikuwonetsa kuti chipolopolo cha SiO2 chidasunga bwino SA (core) kudzera mu njira yolumikizirana ndi polymerization ya TEOS yosungunuka. Pa kuchuluka kwa SA kotsika, mphamvu yayikulu ya gulu la Si-O-Si ndi yayikulu (Chithunzi 3b-d). Pamene kuchuluka kwa SA kukuwonjezeka kufika pa 15 g, mphamvu ya nsonga ndi kufalikira kwa gulu la Si-O-Si kumachepa pang'onopang'ono, kusonyeza kupangika kwa wosanjikiza woonda wa SiO2 pamwamba pa SA.
Ma spectra a FTIR a (a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 ndi (g) SATEOS6.
Mapangidwe a XRD a bulk SA ndi microencapsulated SA akuwonetsedwa mu Chithunzi 4. Nsonga za XRD zili pa 2θ = 6.50° (300), 10.94° (500), 15.46° (700), 20.26° \((\overline {5}malinga ndi JCPDS No. 0381923, 02)\), 21.42° mu zitsanzo zonse (311), 24.04° (602) ndi 39.98° (913) zimaperekedwa ku SA. Kusokonekera ndi kusakanikirana ndi bulk CA chifukwa cha zinthu zosatsimikizika monga surfactant (SLS), zinthu zina zotsalira ndi microencapsulation ya SiO250. Pambuyo pozungulira, mphamvu ya ma main peaks (300), (500), (311), ndi (602) imachepa pang'onopang'ono poyerekeza ndi bulk CA, kusonyeza kuchepa kwa crystallinity ya chitsanzocho.
Mapangidwe a XRD a (a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 ndi (g) SATEOS6.
Mphamvu ya SATEOS1 imachepa kwambiri poyerekeza ndi zitsanzo zina. Palibe nsonga zina zomwe zidawonedwa m'zitsanzo zonse zazing'ono (Chithunzi 4b–g), zomwe zimatsimikizira kuti kuyamwa kwa SiO252 m'malo mwa kuyanjana kwa mankhwala kumachitika pamwamba pa SA. Kuphatikiza apo, zidaganiziridwanso kuti kuyika kwa SA pang'ono sikunapangitse kuti pakhale mawonekedwe atsopano. SiO2 imakhalabe yoyera pamwamba pa SA popanda kuchitapo kanthu kwa mankhwala, ndipo pamene kuchuluka kwa SA kukuchepa, nsonga zomwe zilipo zimawonekera bwino (SATEOS1). Zotsatirazi zikusonyeza kuti SiO2 imaphimba kwambiri pamwamba pa SA. Nsonga pa (700) imasowa kwathunthu, ndipo nsonga pa \((\overline{5}02)\) imakhala hump mu SATEOS 1 (Chithunzi 4b), yomwe imagwirizanitsidwa ndi kuchepa kwa kristalo ndi kuwonjezeka kwa amorphism. SiO2 ndi yopanda mawonekedwe, kotero nsonga zomwe zimawonedwa kuyambira 2θ = 19° mpaka 25° zimakhala ndi hump ndi kufalikira53 (Chithunzi 4b–g), zomwe zimatsimikizira kukhalapo kwa SiO252 yopanda mawonekedwe. Mphamvu yotsika ya diffraction peak ya microencapsulated SA imachitika chifukwa cha nucleation effect ya khoma lamkati la silica ndi khalidwe loletsa crystallization49. Amakhulupirira kuti ndi kuchuluka kwa SA kochepa, chipolopolo chokhuthala cha silica chimapangidwa chifukwa cha kukhalapo kwa TEOS yambiri, yomwe imamatiridwa kwambiri pamwamba pa SA. Komabe, pamene kuchuluka kwa SA kukuwonjezeka, malo a pamwamba pa madontho a SA mu emulsion solution akuwonjezeka ndipo TEOS yambiri imafunika kuti encapsulation ikhale yoyenera. Chifukwa chake, ndi kuchuluka kwa SA, SiO2 peak mu FT-IR imachepetsedwa (Chithunzi 3), ndipo mphamvu ya diffraction peak pafupi ndi 2θ = 19–25° mu XRF (Chithunzi 4) imachepa ndipo kukula kumachepanso. Sikuwoneka. Komabe, monga momwe zikuonekera pa Chithunzi 4, kuchuluka kwa SA kukangowonjezeka kuchoka pa 5 g (SATEOS1) kufika pa 50 g (SATEOS6), nsonga zimakhala pafupi kwambiri ndi bulk SA, ndipo nsonga pa (700) imawonekera ndi mphamvu zonse za nsonga zomwe zadziwika. Zotsatirazi zikugwirizana ndi zotsatira za FT-IR, komwe mphamvu ya nsonga ya SiO2 SATEOS6 imachepa pa 1103 cm-1 (Chithunzi 3g).
Mkhalidwe wa mankhwala a zinthu zomwe zili mu SA, SATEOS1 ndi SATEOS6 zawonetsedwa mu Zithunzi 1 ndi 2. Zithunzi 5, 6, 7 ndi 8 ndi Table 2. Kusanthula kwa muyeso wa bulk SA, SATEOS1 ndi SATEOS6 kwawonetsedwa mu Chithunzi 5 ndipo kusanthula kwapamwamba kwa C 1s, O 1s ndi Si 2p kwawonetsedwa mu Zithunzi 5, 6, 7 ndi 8 ndi Table 2. 6, 7 ndi 8 motsatana. Mphamvu zomangira zomwe zimapezeka ndi XPS zafotokozedwa mwachidule mu Table 2. Monga momwe zikuonekera mu Chithunzi 5, Si 2s ndi Si 2p peaks zoonekeratu zidawonedwa mu SATEOS1 ndi SATEOS6, komwe microencapsulation ya chipolopolo cha SiO2 idachitika. Ofufuza am'mbuyomu adanenanso za Si 2s peak yofanana pa 155.1 eV54. Kupezeka kwa ma Si peaks mu SATEOS1 (Chithunzi 5b) ndi SATEOS6 (Chithunzi 5c) kumatsimikizira deta ya FT-IR (Chithunzi 3) ndi XRD (Chithunzi 4).
Monga momwe zasonyezedwera mu Chithunzi 6 a, ma C 1 a bulk SA ali ndi ma peak atatu osiyana a CC, caliphatic, ndi O=C=O pa mphamvu yomangira, omwe ndi 284.5 eV, 285.2 eV, ndi 289.5 eV, motsatana. Ma peak a C–C, caliphatic ndi O=C=O adawonedwanso mu SATEOS1 (Chithunzi 6b) ndi SATEOS6 (Chithunzi 6c) ndipo afotokozedwa mwachidule mu Table 2. Kuphatikiza pa izi, peak ya C 1s ikugwirizananso ndi peak yowonjezera ya Si-C pa 283 .1 eV (SATEOS1) ndi 283.5 eV (SATEOS6). Mphamvu zathu zomangira zomwe zawonedwa za C–C, caliphatic, O=C=O ndi Si–C zimagwirizana bwino ndi magwero ena55,56.
Ma spectra a XPS a O 1 SA, SATEOS1 ndi SATEOS6 akuwonetsedwa mu Zithunzi 7a–c, motsatana. Nsonga ya O 1s ya bulk SA yachotsedwa ndipo ili ndi peaks ziwiri, zomwe ndi C=O/C–O (531.9 eV) ndi C–O–H (533.0 eV), pomwe O 1 ya SATEOS1 ndi SATEOS6 ndi yofanana. Pali peaks zitatu zokha: C=O/C–O, C–O–H ndi Si–OH55,57,58. Mphamvu yomangira ya O 1s mu SATEOS1 ndi SATEOS6 imasintha pang'ono poyerekeza ndi bulk SA, zomwe zimagwirizana ndi kusintha kwa chidutswa cha mankhwala chifukwa cha kukhalapo kwa SiO2 ndi Si-OH mu chipolopolo.
Ma spectra a Si 2p XPS a SATEOS1 ndi SATEOS6 akuwonetsedwa mu Chithunzi 8a ndi b, motsatana. Mu bulk CA, Si 2p sinawonekere chifukwa cha kusowa kwa SiO2. Si 2p peak ikufanana ndi 105.4 eV ya SATEOS1 ndi 105.0 eV ya SATEOS6, yofanana ndi Si-O-Si, pomwe SATEOS1 peak ndi 103.5 eV ndipo SATEOS6 peak ndi 103.3 eV, yofanana ndi Si-OH55. Kuyika kwa Si-O-Si ndi Si-OH peak mu SATEOS1 ndi SATEOS6 kwawonetsa bwino microencapsulation ya SiO2 pamwamba pa SA core.
Kapangidwe ka zinthu zomwe zili ndi ma microcapsules n'kofunika kwambiri, komwe kumakhudza kusungunuka, kukhazikika, kusinthika kwa mankhwala, kuyenda bwino komanso mphamvu59. Chifukwa chake, SEM idagwiritsidwa ntchito pofotokoza mawonekedwe a bulk SA (100×) ndi microcapsuled SA (500×), monga momwe zasonyezedwera pa Chithunzi 9. Monga momwe zikuonekera pa Chithunzi 9a, chipika cha SA chili ndi mawonekedwe ozungulira. Kukula kwa tinthu tating'onoting'ono kumaposa ma microns 500. Komabe, njira yochepetsera ma microcapsule ikapitirira, mawonekedwe ake amasintha kwambiri, monga momwe zasonyezedwera pa Zithunzi 9 b–g.
Zithunzi za SEM za (a) SA (×100), (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 ndi (g) SATEOS6 pa ×500.
Mu chitsanzo cha SATEOS1, tinthu tating'onoting'ono ta SA tomwe tili ndi SiO2 tomwe tili ndi malo ozungulira timawonedwa (Chithunzi 9b), zomwe zitha kukhala chifukwa cha hydrolysis ndi condensation polymerization ya TEOS pamwamba pa SA, zomwe zimathandizira kufalikira mwachangu kwa mamolekyulu a ethanol. Zotsatira zake, tinthu ta SiO2 timayikidwa ndipo agglomeration imawonedwa52,60. Chipolopolo cha SiO2 ichi chimapereka mphamvu yamakina ku tinthu ta CA tomwe tili ndi microcapsulated komanso chimaletsa kutuluka kwa CA yosungunuka kutentha kwambiri10. Zotsatirazi zikusonyeza kuti ma microcapsules a SA okhala ndi SiO2 angagwiritsidwe ntchito ngati zinthu zosungira mphamvu61. Monga momwe tikuonera kuchokera pa Chithunzi 9b, chitsanzo cha SATEOS1 chili ndi kugawa kwa tinthu tofanana ndi gawo la SiO2 lokhuthala lomwe limaphimba SA. Kukula kwa tinthu ta microcapsulated SA (SATEOS1) ndi pafupifupi 10–20 μm (Chithunzi 9b), komwe ndi kochepa kwambiri poyerekeza ndi bulk SA chifukwa cha kuchuluka kwa SA kochepa. Kukhuthala kwa microcapsule layer kumachitika chifukwa cha hydrolysis ndi condensation polymerization ya precursor solution. Agglomeration imachitika pa mlingo wochepa wa SA, mwachitsanzo mpaka 15 g (Chithunzi 9b-d), koma mlingo ukangowonjezeka, palibe agglomeration yomwe imawoneka, koma tinthu tating'onoting'ono tomwe timafotokozedwa bwino timawonedwa (Chithunzi 9e-g) 62.
Kuphatikiza apo, pamene kuchuluka kwa SLS surfactant kuli kokhazikika, kuchuluka kwa SA (SATEOS1, SATEOS2 ndi SATEOS3) kumakhudzanso magwiridwe antchito, mawonekedwe ndi kukula kwa tinthu. Chifukwa chake, SATEOS1 idapezeka kuti ikuwonetsa kukula kochepa kwa tinthu, kufalikira kofanana komanso pamwamba pokhuthala (Chithunzi 9b), zomwe zidachitika chifukwa cha chibadwa cha SA chokonda madzi chomwe chimalimbikitsa nucleation yachiwiri pansi pa surfactant yokhazikika63. Amakhulupirira kuti powonjezera kuchuluka kwa SA kuchokera pa 5 mpaka 15 g (SATEOS1, SATEOS2 ndi SATEOS3) ndikugwiritsa ntchito kuchuluka kosasinthasintha kwa surfactant, mwachitsanzo 0.10 g SLS (Table 1), gawo la tinthu chilichonse cha molekyulu ya surfactant lidzachepa, motero kuchepetsa kukula kwa tinthu ndi kukula kwa tinthu. Kufalikira kwa SATEOS2 (Chithunzi 9c) ndi SATEOS3 (Chithunzi 9d) kumasiyana ndi kufalikira kwa SATEOS 1 (Chithunzi 9b).
Poyerekeza ndi SATEOS1 (Chithunzi 9b), SATEOS2 inasonyeza mawonekedwe okhuthala a microencapsulated SA ndipo kukula kwa tinthu tating'onoting'ono kunawonjezeka (Chithunzi 9c). Izi zimachitika chifukwa cha agglomeration 49, zomwe zimachepetsa kuchuluka kwa coagulation (Chithunzi 2b). Pamene kuchuluka kwa SC kukuwonjezeka ndi kuwonjezeka kwa SLS, ma microcapsules amaonekera bwino, monga momwe zasonyezedwera mu Chithunzi. momwe kusonkhana kumachitikira. Kuphatikiza apo, Zithunzi 9e-g zikuwonetsa kuti tinthu tonse timakhala tozungulira bwino komanso kukula kwake. Zadziwika kuti pakakhala kuchuluka kwa SA, kuchuluka koyenera kwa silica oligomers kumatha kupezeka, zomwe zimapangitsa kuti condensation ndi encapsulation yoyenera zipangidwe motero kupangika kwa microcapsules yodziwika bwino49. Kuchokera ku zotsatira za SEM, n'zoonekeratu kuti SATEOS6 idapanga microcapsules yofanana poyerekeza ndi kuchuluka kochepa kwa SA.
Zotsatira za energy dispersive X-ray spectroscopy (EDS) ya bulk SA ndi microcapsule SA zaperekedwa mu Table 3. Monga momwe taonera pa tebulo ili, kuchuluka kwa Si kumachepa pang'onopang'ono kuchokera ku SATEOS1 (12.34%) kufika ku SATEOS6 (2.68%). Kuwonjezeka kwa SA. Chifukwa chake, tinganene kuti kuwonjezeka kwa kuchuluka kwa SA kumabweretsa kuchepa kwa kuyika kwa SiO2 pamwamba pa SA. Palibe miyezo yofanana ya zomwe zili mu C ndi O mu Table 3 chifukwa cha kusanthula kwa EDS51 kwa semi-quantitative. Kuchuluka kwa Si mu microencapsulated SA kunagwirizana ndi zotsatira za FT-IR, XRD ndi XPS.
Kachitidwe ka kusungunuka ndi kuuma kwa bulk SA komanso microencapsulated SA yokhala ndi chipolopolo cha SiO2 kakuwonetsedwa mu Zithunzi 1 ndi 2. Kawonetsedwe mu Zithunzi 10 ndi 11 motsatana, ndipo deta ya kutentha ikuwonetsedwa mu Table 4. Kutentha kwa kusungunuka ndi kuuma kwa microencapsulated SA kunapezeka kuti ndi kosiyana. Pamene kuchuluka kwa SA kukuwonjezeka, kutentha kwa kusungunuka ndi kuuma kumawonjezeka ndikuyandikira mtengo wa bulk SA. Pambuyo pa microencapsulation ya SA, khoma la silika limawonjezera kutentha kwa crystallization, ndipo khoma lake limagwira ntchito ngati maziko olimbikitsa kusiyana. Chifukwa chake, pamene kuchuluka kwa SA kukuwonjezeka, kutentha kwa kusungunuka (Chithunzi 10) ndi kuuma (Chithunzi 11) kumawonjezekanso pang'onopang'ono49,51,64. Pakati pa zitsanzo zonse za microencapsulated SA, SATEOS6 inawonetsa kutentha kwakukulu kwa kusungunuka ndi kuuma, kutsatiridwa ndi SATEOS5, SATEOS4, SATEOS3, SATEOS2, ndi SATEOS1.
SATEOS1 ikuwonetsa malo otsika kwambiri osungunuka (68.97 °C) ndi kutentha kolimba (60.60 °C), zomwe zimachitika chifukwa cha kukula kochepa kwa tinthu ta SA komwe kuyenda kwa tinthu ta SA mkati mwa ma microcapsules kumakhala kochepa kwambiri ndipo chipolopolo cha SiO2 chimapanga wosanjikiza wokhuthala motero Core Material imaletsa kutambasuka ndi kuyenda49. Lingaliro ili likugwirizana ndi zotsatira za SEM, pomwe SATEOS1 idawonetsa kukula kochepa kwa tinthu tating'onoting'ono (Chithunzi 9b), zomwe zimachitika chifukwa chakuti mamolekyu a SA ali mkati mwa gawo laling'ono kwambiri la ma microcapsules. Kusiyana kwa kutentha kwa kusungunuka ndi kulimba kwa main main main, komanso ma microcapsules onse a SA okhala ndi zipolopolo za SiO2, kuli pakati pa 6.10–8.37 °C. Zotsatirazi zikusonyeza kuti microencapsulated SA ingagwiritsidwe ntchito ngati chinthu chosungira mphamvu chifukwa cha kutentha kwabwino kwa chipolopolo cha SiO2 65.
Monga momwe taonera pa Table 4, SATEOS6 ili ndi enthalpy yapamwamba kwambiri pakati pa ma SC onse okhala ndi ma microcapsulated (Chithunzi 9g) chifukwa cha encapsulation yoyenera yomwe SEM yawona. Kuchuluka kwa SA packing kungathe kuwerengedwa pogwiritsa ntchito equation (1). (1) Poyerekeza deta ya kutentha kobisika ya microcapsulated SA49.
Mtengo wa R ukuyimira digiri ya encapsulation (%) ya SC yolumikizidwa ndi microcapsulated, ΔHMEPCM, m ikuyimira kutentha kobisika kwa kuphatikiza kwa SC yolumikizidwa ndi microcapsulated, ndipo ΔHPCM, m ikuyimira kutentha kobisika kwa kuphatikiza kwa SC. Kuphatikiza apo, kugwira ntchito bwino kwa ma paketi (%) kumawerengedwa ngati gawo lina lofunikira laukadaulo, monga momwe zasonyezedwera mu Equation (1). (2)49.
Mtengo wa E ukuyimira mphamvu ya encapsulation (%) ya microencapsulated CA, ΔHMEPCM,s ikuyimira kutentha kobisika kwa kuchiritsa kwa microencapsulated CA, ndipo ΔHPCM,s ikuyimira kutentha kobisika kwa kuchiritsa kwa CA.
Monga momwe zasonyezedwera mu Table 4, kuchuluka kwa kulongedza ndi kugwira ntchito kwa SATEOS1 ndi 71.89% ndi 67.68%, motsatana, ndipo kuchuluka kwa kulongedza ndi kugwira ntchito kwa SATEOS6 ndi 90.86% ndi 86.68%, motsatana (Table 4). Chitsanzo cha SATEOS6 chikuwonetsa kuchuluka kwa kulongedza ndi kugwira ntchito bwino kwambiri pakati pa ma SA onse okhala ndi ma microcapsulated, zomwe zikusonyeza kuti kutentha kwake kuli kwakukulu. Chifukwa chake, kusintha kuchoka pa cholimba kupita ku madzi kumafuna mphamvu zambiri. Kuphatikiza apo, kusiyana kwa kutentha kwa kusungunuka ndi kulimba kwa ma microcapsule onse a SA ndi bulk SA panthawi yozizira kukuwonetsa kuti chipolopolo cha silica chimakhala chokhazikika pamalo panthawi yopanga microcapsule. Chifukwa chake, zotsatira zake zikuwonetsa kuti pamene kuchuluka kwa SC kukuwonjezeka, kuchuluka kwa kulongedza ndi kugwira ntchito bwino kumawonjezeka pang'onopang'ono (Table 4).
Ma curve a TGA a bulk SA ndi microcapsule SA okhala ndi chipolopolo cha SiO2 (SATEOS1, SATEOS3 ndi SATEOS6) akuwonetsedwa mu Chithunzi 12. Makhalidwe okhazikika a kutentha a bulk SA (SATEOS1, SATEOS3 ndi SATEOS6) adayerekezeredwa ndi zitsanzo za microencapsulated. N'zoonekeratu kuchokera ku TGA curve kuti kuchepa kwa kulemera kwa bulk SA komanso microencapsulated SA kukuwonetsa kuchepa kosalala komanso pang'ono kwambiri kuchokera pa 40°C mpaka 190°C. Pa kutentha kumeneku, bulk SC simawola kutentha, pomwe microencapsulated SC imatulutsa madzi obzalidwa ngakhale itauma pa 45 °C kwa maola 24. Izi zidapangitsa kuti kulemera kuchepe pang'ono,49 koma kupitirira kutentha kumeneku, zinthuzo zinayamba kuwonongeka. Pa kuchuluka kwa SA kotsika (monga SATEOS1), kuchuluka kwa madzi obzalidwa kumakhala kwakukulu ndipo motero kutayika kwa unyinji mpaka 190 °C kumakhala kwakukulu (chithunzi cha Chithunzi 12). Kutentha kukangokwera pamwamba pa 190 °C, chitsanzocho chimayamba kutaya kulemera chifukwa cha njira zowola. Bulk SA imayamba kuwola pa 190°C ndipo 4% yokha imatsala pa 260°C, pomwe SATEOS1, SATEOS3 ndi SATEOS6 zimasunga 50%, 20% ndi 12% kutentha kumeneku, motsatana. Pambuyo pa 300 °C, kutaya kwakukulu kwa bulk SA kunali pafupifupi 97.60%, pomwe kutaya kwakukulu kwa SATEOS1, SATEOS3, ndi SATEOS6 kunali pafupifupi 54.20%, 82.40%, ndi 90.30%, motsatana. Ndi kuwonjezeka kwa kuchuluka kwa SA, kuchuluka kwa SiO2 kumachepa (Table 3), ndipo kupendekeka kwa chipolopolo kumawonedwa mu SEM (Chithunzi 9). Motero, kuchepa kwa kulemera kwa microencapsulated SA ndikochepa poyerekeza ndi bulk SA, zomwe zimafotokozedwa ndi makhalidwe abwino a chipolopolo cha SiO2, chomwe chimalimbikitsa kupangidwa kwa carbonaceous silicate-carbonaceous layer pamwamba pa SA, motero kumalekanitsa pakati pa SA ndikuchepetsa kutulutsidwa kwa zinthu zosinthika zomwe zimachokera10. Char layer iyi imapanga chotchinga chakuthupi panthawi ya kutentha, zomwe zimalepheretsa kusintha kwa mamolekyulu oyaka moto kupita ku gasi phase66,67. Kuphatikiza pa izi, titha kuwonanso zotsatira zazikulu zochepetsa kulemera: SATEOS1 ikuwonetsa mitengo yotsika poyerekeza ndi SATEOS3, SATEOS6 ndi SA. Izi zili choncho chifukwa kuchuluka kwa SA mu SATEOS1 ndi kochepa kuposa mu SATEOS3 ndi SATEOS6, komwe chipolopolo cha SiO2 chimapanga layer wandiweyani. Mosiyana ndi izi, kuchepa konse kwa kulemera kwa bulk SA kumafika pa 99.50% pa 415 °C. Komabe, SATEOS1, SATEOS3, ndi SATEOS6 zinawonetsa kuchepa kwa thupi ndi 62.50%, 85.50%, ndi 93.76%, motsatana, pa 415 °C. Zotsatirazi zikusonyeza kuti kuwonjezera kwa TEOS kumathandizira kuwonongeka kwa SA mwa kupanga gawo la SiO2 pamwamba pa SA. Zigawozi zimatha kupanga chotchinga chakuthupi, motero kusintha kwa kutentha kwa CA yolumikizidwa ndi microcapsulated kungawonekere.
Zotsatira za kudalirika kwa kutentha kwa bulk SA ndi chitsanzo chabwino kwambiri cha microencapsulated (monga SATEOS 6) pambuyo pa ma cycle 30 otentha ndi kuzizira a DSC51,52 akuwonetsedwa mu Chithunzi 13. Zitha kuwoneka kuti bulk SA (Chithunzi 13a) sikuwonetsa kusiyana kulikonse pa kutentha kosungunuka. kulimba ndi enthalpy, pomwe SATEOS6 (Chithunzi 13b) sikuwonetsa kusiyana kulikonse pa kutentha ndi enthalpy ngakhale pambuyo pa ma cycle 30 otentha. ndi njira yozizira. Bulk SA inawonetsa malo osungunuka a 72.10 °C, kutentha kolimba kwa 64.69 °C, ndipo kutentha kwa fusion ndi kulimba pambuyo pa ma cycle oyamba kunali 201.0 J/g ndi 194.10 J/g, motsatana. Pambuyo pa kuzungulira kwa 30, kutentha kwa zinthuzi kunatsika kufika pa 71.24 °C, kutentha kwa kulimba kunatsika kufika pa 63.53 °C, ndipo kuchuluka kwa enthalpy kunatsika ndi 10%. Kusintha kwa kutentha kwa kusungunuka ndi kulimba, komanso kuchepa kwa kuchuluka kwa enthalpy, kukuwonetsa kuti bulk CA ndi yosadalirika pa ntchito zosagwiritsa ntchito microencapsulation. Komabe, pambuyo poti microencapsulation yoyenera yachitika (SATEOS6), kutentha kwa kusungunuka ndi kulimba ndi kuchuluka kwa enthalpy sikusintha (Chithunzi 13b). Ikayikidwa microencapsulated ndi zipolopolo za SiO2, SA ingagwiritsidwe ntchito ngati zinthu zosinthira gawo pakugwiritsa ntchito kutentha, makamaka pomanga, chifukwa cha kutentha kwake koyenera kwa kusungunuka ndi kulimba komanso enthalpy yokhazikika.
Ma curve a DSC omwe apezeka pa zitsanzo za SA (a) ndi SATEOS6 (b) pa nthawi yoyamba ndi ya 30 yotenthetsera ndi kuzizira.
Mu kafukufukuyu, kafukufuku wokonzedwa bwino wa microencapsulation unachitika pogwiritsa ntchito SA ngati chinthu chachikulu ndi SiO2 ngati chinthu cha chipolopolo. TEOS imagwiritsidwa ntchito ngati choyambira kupanga gawo lothandizira la SiO2 ndi gawo loteteza pamwamba pa SA. Pambuyo popanga bwino microencapsulated SA, zotsatira za FT-IR, XRD, XPS, SEM ndi EDS zinawonetsa kupezeka kwa SiO2. Kusanthula kwa SEM kukuwonetsa kuti chitsanzo cha SATEOS6 chikuwonetsa tinthu tating'onoting'ono tozungulira tozunguliridwa ndi zipolopolo za SiO2 pamwamba pa SA. Komabe, MEPCM yokhala ndi kuchuluka kochepa kwa SA ikuwonetsa kusonkhana, komwe kumachepetsa magwiridwe antchito a PCM. Kusanthula kwa XPS kunawonetsa kupezeka kwa Si-O-Si ndi Si-OH mu zitsanzo za microcapsule, zomwe zidawonetsa kuyamwa kwa SiO2 pamwamba pa SA. Malinga ndi kusanthula kwa magwiridwe antchito a kutentha, SATEOS6 ikuwonetsa kuthekera kosungira kutentha kodalirika kwambiri, ndi kutentha kosungunuka ndi kulimba kwa 70.37°C ndi 64.27°C, motsatana, ndi kutentha kobisika kwa kusungunuka ndi kulimba kwa 182.53 J/g ndi 160.12 J/g. G. motsatana. Mphamvu yayikulu yolongedza ya SATEOS6 ndi 86.68%. Kusanthula kwa TGA ndi DSC thermal cycle kwatsimikizira kuti SATEOS6 ikadali ndi kukhazikika kwa kutentha komanso kudalirika ngakhale patatha njira 30 zotenthetsera ndi kuziziritsa.
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