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I-Stearic acid (SA) isetyenziswa njengesixhobo sokutshintsha isigaba (PCM) kwizixhobo zokugcina amandla. Kolu phononongo, indlela ye-sol-gel isetyenzisiwe ukufaka i-surfactant yegobolondo le-SiO2 kwi-microcapsulate. Izixa ezahlukeneyo ze-SA (5, 10, 15, 20, 30, kunye ne-50 g) zifakwe kwi-10 mL ye-tetraethyl orthosilicate (TEOS). Izinto zokutshintsha isigaba ze-microencapsulated ezihlanganisiweyo (MEPCM) zibonakaliswe yi-Fourier transform infrared spectroscopy (FT-IR), i-X-ray diffraction (XRD), i-X-ray photoelectron spectroscopy (XPS), kunye ne-scanning electron microscopy (SEM). Iziphumo zokuchazwa zibonise ukuba i-SA ifakwe ngempumelelo yi-SiO2. Uhlalutyo lwe-Thermogravimetric (TGA) lubonise ukuba i-MEPCM inozinzo olungcono lobushushu kune-CA. Ukusebenzisa i-calorimetry ye-differential scanning (DSC), kwafunyaniswa ukuba ixabiso le-enthalpy le-MEPCM alitshintshanga nasemva kwemijikelo engama-30 yokupholisa ubushushu. Kuzo zonke iisampuli ezifakwe kwi-microcapsulated, i-50 g ye-SA equlethe i-MEPCM yayinobushushu obuphezulu obufihlakeleyo bokunyibilika nokuqina, obuyi-182.53 J/g kunye ne-160.12 J/g, ngokwahlukeneyo. Ixabiso lokusebenza kakuhle kwephakheji libalwe kusetyenziswa idatha yobushushu kwaye ukusebenza kakuhle okuphezulu kufunyenwe kwisampuli efanayo eyayiyi-86.68%.
Malunga ne-58% yamandla asetyenziswa kushishino lokwakha asetyenziselwa ukufudumeza nokupholisa izakhiwo1. Ke ngoko, eyona nto ifunekayo kukudala iinkqubo zamandla ezisebenzayo eziqwalasela ungcoliseko lokusingqongileyo2. Itekhnoloji yobushushu obufihlakeleyo esebenzisa izixhobo zokutshintsha isigaba (i-PCM) inokugcina amandla aphezulu kubushushu obuphantsi3,4,5,6 kwaye ingasetyenziswa kakhulu kwiindawo ezifana nokudluliselwa kobushushu, ukugcinwa kwamandla elanga, i-aerospace kunye ne-air conditioning7,8,9. I-PCM ifunxa amandla obushushu avela ngaphandle kwesakhiwo emini kwaye ikhuphe amandla ebusuku10. Ke ngoko, izixhobo zokutshintsha isigaba ziyacetyiswa njengezixhobo zokugcina amandla obushushu. Ukongeza, kukho iintlobo ezahlukeneyo ze-PCM ezifana ne-solid-solid, i-solid-liquid, i-liquid-gas kunye ne-solid-gas11. Phakathi kwazo, izixhobo zokutshintsha isigaba ezidumileyo nezisetyenziswa rhoqo zizixhobo zokutshintsha isigaba eziqinileyo kunye nezixhobo zokutshintsha isigaba eziqinileyo. Nangona kunjalo, ukusetyenziswa kwazo kunzima kakhulu ngenxa yotshintsho olukhulu lwevolumu yezinto zokutshintsha isigaba ezimanzi kunye ne-solid-gas.
I-PCM ineendlela ezahlukeneyo zokusetyenziswa ngenxa yeempawu zayo: ezo zinyibilikayo kumaqondo obushushu angaphantsi kwe-15°C zingasetyenziswa kwiinkqubo zomoya opholileyo ukugcina amaqondo obushushu abandayo, kwaye ezo zinyibilikayo kumaqondo obushushu angaphezulu kwe-90°C zingasetyenziswa kwiinkqubo zokufudumeza ukuthintela imililo12. Ngokuxhomekeke kuhlobo lokusetyenziswa kunye noluhlu lwamanqaku okunyibilika, izixhobo ezahlukeneyo zotshintsho lwesigaba zenziwe kwiikhemikhali ezahlukeneyo ze-organic kunye ne-inorganic13,14,15. Iparafini yeyona nto isetyenziswa kakhulu kutshintsho lwesigaba enobushushu obufihlakeleyo, engaboliyo, ukhuseleko kunye noluhlu olubanzi lwamanqaku okunyibilika16,17,18,19,20,21.
Nangona kunjalo, ngenxa yokuqhuba okuphantsi kobushushu bezinto zokutshintsha isigaba, kufuneka zifakwe kwiqokobhe (umaleko wangaphandle) ukuthintela ukuvuza kwezinto ezisisiseko ngexesha lenkqubo yokutshintsha isigaba22. Ukongeza, iimpazamo zokusebenza okanye uxinzelelo lwangaphandle zingonakalisa umaleko wangaphandle (i-cladding), kwaye izinto zokutshintsha isigaba ezinyibilikisiweyo zinokusabela kwizinto zokwakha, zibangele ukugqwala kweebha zentsimbi ezifakwe ngaphakathi, ngaloo ndlela zinciphisa ukusebenza kwesakhiwo23. Ke ngoko, kubalulekile ukudibanisa izinto zokutshintsha isigaba ezifakwe ngaphakathi ngezinto ezaneleyo zeqokobhe, ezinokusombulula ezi ngxaki zingasentla24.
Ukufakwa kwezinto ezincinci zokutshintsha isigaba kunokunyusa ngempumelelo ukudluliselwa kobushushu kwaye kunciphise ukusabela kwendalo, kunye nokulawula utshintsho lwevolumu. Iindlela ezahlukeneyo ziye zaphuhliswa zokufakwa kwezinto kwi-PCM, ezizezi: i-interfacial polymerization25,26,27,28, i-in situ polymerization29,30,31,32, i-coacervation33,34,35 kunye neenkqubo ze-sol-gel36,37,38,39. I-Formaldehyde resin ingasetyenziselwa i-microencapsulation40,41,42,43. Ii-Melamine-formaldehyde kunye ne-urea-formaldehyde resins zisetyenziswa njengezinto zegobolondo, ezihlala zikhupha i-formaldehyde enobuthi ngexesha lokusebenza. Ke ngoko, ezi zinto azivumelekanga ukusetyenziswa kwiinkqubo zokupakisha. Nangona kunjalo, izinto zokutshintsha isigaba ezinobuhlobo nokusingqongileyo zokugcina amandla obushushu anokulinganiswa zinokwenziwa kusetyenziswa ii-nanocapsules ezixutyiweyo ezisekelwe kwi-fatty acids kunye ne-lignin44.
UZhang nabanye 45 badibanise i-lauric acid kwi-tetraethyl orthosilicate baza bagqiba kwelokuba njengoko umlinganiselo wevolumu ye-methyltriethoxysilane ukuya kwi-tetraethyl orthosilicate uyanda, ubushushu obufihlakeleyo buyancipha kwaye i-hydrophobicity yomphezulu iyanda. I-Lauric acid inokuba yinto enokwenzeka nesebenzayo kwi-kapok fibers46. Ukongeza, uLatibari nabanye 47 badibanise ii-PCM ezisekwe kwi-stearic acid besebenzisa i-TiO2 njengezinto zegobolondo. UZhu nabanye balungiselele i-n-octadecane kunye ne-silicone nanocapsules njengee-PCM ezinokwenzeka 48. Ukusuka kuphononongo lweencwadi, kunzima ukuqonda idosi ecetyiswayo yokwenza izinto ezisebenzayo nezizinzileyo zokutshintsha isigaba se-microencapsulated.
Ngoko ke, ngokolwazi lwababhali, ubungakanani bezinto zokutshintsha isigaba ezisetyenziselwa i-microencapsulation luphawu olubalulekileyo lokuveliswa kwezinto zokutshintsha isigaba ezisebenza kakuhle nezizinzileyo. Ukusebenzisa ubungakanani obahlukeneyo bezinto zokutshintsha isigaba kuya kusenza sikwazi ukucacisa iipropati ezahlukeneyo kunye nokuzinza kwezinto zokutshintsha isigaba ezifakwe i-microencapsulated. I-Stearic acid (i-fatty acid) yinto enobuhlobo nokusingqongileyo, ebalulekileyo kwezonyango kwaye inoqoqosho enokusetyenziswa ukugcina amandla obushushu kuba inexabiso eliphezulu le-enthalpy (~200 J/g) kwaye inokumelana namaqondo obushushu ukuya kuthi ga kwi-72 °C. Ukongeza, i-SiO2 ayitshi, inika amandla aphezulu oomatshini, ukuqhuba kobushushu kunye nokumelana okungcono kweekhemikhali kwizinto eziphambili, kwaye isebenza njengezinto ezibangela i-pozzolanic ekwakheni. Xa isamente ixutywe namanzi, ii-PCM ezingafakwanga kakuhle zinokuqhekeka ngenxa yokuguguleka koomatshini kunye namaqondo obushushu aphezulu (ubushushu bokufuma) aveliswa kwizakhiwo ezinkulu zekhonkrithi. Ke ngoko, ukusetyenziswa kwe-CA efakwe i-microencapsulated eneqokobhe le-SiO2 kunokusombulula le ngxaki. Ngoko ke, injongo yolu phononongo yayikukuphanda ukusebenza kakuhle kwee-PCM ezenziwe ngenkqubo ye-sol-gel kwizicelo zokwakha. Kulo msebenzi, sifunde ngokucwangcisiweyo ubungakanani obahlukeneyo be-SA (njengezinto ezisisiseko) ze-5, 10, 15, 20, 30 kunye ne-50 g ezifakwe kwiigobolondo ze-SiO2. Isixa esimiselweyo se-tetraethylorthosilicate (TEOS) kumthamo we-10 ml sisetyenziswe njengesisombululo sokuqala sokwenziwa kwegobolondo le-SiO2.
I-stearic acid ye-reactive grade (SA, C18H36O2, indawo yokunyibilika: 72°C) njengezinto eziphambili ithengwe kwiDaejung Chemical & Metals Co., Ltd., Gyeonggi-do, eMzantsi Korea. I-Tetraethylorthosilicate (TEOS, C8H20O4Si) njengesisombululo sangaphambili ithengwe kwiAcros Organics, Geel, eBelgium. Ukongeza, i-absolute ethanol (EA, C2H5OH) kunye ne-sodium lauryl sulfate (SLS, C12H25NaO4S) zithengwe kwiDaejung Chemical & Metals Co., Ltd, Gyeonggi-do, eMzantsi Korea, kwaye zisetyenziswe njenge-solvents kunye ne-surfactants, ngokwahlukeneyo. Amanzi anyibilikisiweyo akwasetyenziswa njenge-solvent.
Izixa ezahlukeneyo ze-SA zixutywe ngemilinganiselo eyahlukeneyo ye-sodium lauryl sulfate (SLS) kwi-100 mL yamanzi acociweyo kusetyenziswa i-magnetic stirrer kwi-800 rpm kunye ne-75 °C iyure e-1 (Itheyibhile 1). Ii-emulsions ze-SA zahlulwe zangamaqela amabini: (1) I-5, 10 kunye ne-15 g ye-SA zixutywe ne-0.10 g ye-SLS kwi-100 ml yamanzi acociweyo (SATEOS1, SATEOS2 kunye ne-SATEOS3), (2) I-20, 30 kunye ne-50 g ye-SA zixutywe ne-0.15, 0.20 kunye ne-0.25 g ye-SLS zixutywe ne-100 ml yamanzi acociweyo (SATEOS4, SATEOS5 kunye ne-SATEOS6). I-0.10 g ye-SLS isetyenzisiwe kunye ne-5, 10 kunye ne-15 g ye-SA ukwenza ii-emulsions ezifanelekileyo. Emva koko, kwacetyiswa ukuba kwandiswe inani le-SLS kwi-SATEOS4, SATEOS5 kunye ne-SATEOS6. Itheyibhile 1 ibonisa umlinganiselo we-CA kunye ne-SLS ezisetyenziselwa ukufumana izisombululo ze-emulsion ezizinzileyo.
Beka i-10 ml ye-TEOS, i-10 ml ye-ethanol (EA) kunye ne-20 ml yamanzi acociweyo kwi-100 ml beaker. Ukuze kufundwe ukusebenza kakuhle kwe-encapsulation yemilinganiselo eyahlukeneyo ye-SA kunye ne-SiO2 shells, i-synthesis coefficient yazo zonke iisampuli yarekhodwa. Umxube wavuselelwa nge-magnetic stirrer kwi-400 rpm kunye ne-60°C iyure e-1. Isisombululo se-precursor saza songezwa kwi-SA emulsion elungisiweyo, savuselelwa ngamandla kwi-800 rpm kunye ne-75 °C iiyure ezi-2, saza sahluzwa ukuze kufunyanwe umgubo omhlophe. Umgubo omhlophe wahlanjwa ngamanzi acociweyo ukuze kususwe i-SA eseleyo kwaye womiswe kwi-vacuum oven kwi-45°C iiyure ezingama-24. Ngenxa yoko, kwafunyanwa i-SC ecociweyo ene-shell ye-SiO2. Yonke inkqubo yokwenza kunye nokulungiselela i-microencapsulated SA iboniswe kuMfanekiso 1.
Ii-microcapsules ze-SA ezineqokobhe le-SiO2 zilungiselelwe ngendlela ye-sol-gel, kwaye indlela yazo yokufaka i-capsulation iboniswe kuMfanekiso 2. Inyathelo lokuqala libandakanya ukulungiselela i-emulsion ye-SA kwisisombululo samanzi esine-SLS njenge-surfactant. Kule meko, isiphelo se-hydrophobic se-molecule ye-SA sibopha kwi-SLS, kwaye isiphelo se-hydrophilic kwiimolekyuli zamanzi, senza i-emulsion ezinzileyo. Ngoko ke, iindawo ze-hydrophobic ze-SLS zikhuselwe kwaye zigubungela umphezulu we-droplet ye-SA. Kwelinye icala, i-hydrolysis yezisombululo ze-TEOS yenzeka kancinci yi-molecules zamanzi, nto leyo ekhokelela ekwakhiweni kwe-hydrolyzed TEOS xa kukho i-ethanol (Umzobo 2a) 49,50,51. I-Hydrolyzed TEOS ifumana impendulo ye-condensation, apho i-n-hydrolyzed TEOS yenza amaqela e-silica (Umzobo 2b). Amaqela e-silica afakwe i-SA52 xa kukho i-SLS (Umzobo 2c), ebizwa ngokuba yinkqubo ye-microencapsulation.
Umzobo weskemakhi we-microencapsulation ye-CA eneqokobhe le-SiO2 (a) i-hydrolysis ye-TEOS (b) ukujiya kwe-hydrolyzate kunye (c) ukujiya kwe-CA eneqokobhe le-SiO2.
Uhlalutyo lweekhemikhali lwe-bulk SA kunye ne-microencapsulated SA lwenziwe kusetyenziswa i-Fourier transform infrared spectrometer (FT-IR, Perkin Elmer UATR Two, USA) kwaye ii-spectra zarekhodwa kumgama ophakathi kwe-500 ukuya kwi-4000 cm-1.
I-X-ray diffractometer (XRD, D/MAX-2500, Rigaku, eJapan) yasetyenziswa ukuhlalutya izigaba ze-SA ezinkulu kunye nezinto ze-microcapsule. Ukuskena kwesakhiwo se-X-ray kwenziwe kuluhlu lwe-2θ = 5°–95° ngesantya sokuskena se-4°/min, kusetyenziswa imitha ye-Cu-Kα (λ = 1.541 Å), iimeko zokusebenza ze-25 kV kunye ne-100 mA, kwimo yokuskena eqhubekayo. Imifanekiso ye-X-ray yakhiwe kuluhlu lwe-2θ = 5–50°, kuba akukho ncochoyi ibonwe emva kwe-50° kuzo zonke iisampuli.
I-X-ray photoelectron spectroscopy (XPS, Scienta Omicron R3000, USA) yenziwe kusetyenziswa i-Al Kα (1486.6 eV) njengomthombo we-X-ray ukuqonda imeko yekhemikhali ye-bulk SA kunye nezinto ezikhoyo kwizinto ezifakwe kwi-encapsulation. Ii-XPS spectra eziqokelelweyo zilinganiswe kwi-C 1s peak kusetyenziswa i-exotic carbon (amandla okubopha angama-284.6 eV). Emva kokulungiswa kwemvelaphi kusetyenziswa indlela yeShirley, iincochoyi eziphezulu zento nganye zasuswa kwaye zafakwa kwimisebenzi yeGaussian/Lorentzian kusetyenziswa isoftware yeCASA XPS.
Imo ye-bulk SC kunye ne-microencapsulated SC ihlolwe kusetyenziswa i-scanning electron microscopy (SEM, MIRA3, TESCAN, Brno, Czech Republic) exhotyiswe nge-energy-dispersive X-ray spectroscopy (EDS) kwi-15 kV. Ngaphambi komfanekiso we-SEM, iisampulu zazigqunywe ngeplatinum (Pt) ukuze kuthintelwe imiphumo yokutshaja.
Iipropati zobushushu (indawo yokunyibilika/yokuqina kunye nobushushu obufihlakeleyo) kunye nokuthembeka (ukujikeleza kobushushu) zichongiwe nge-differential scanning calorimetry (DSC, TA Instrument, Discovery DSC, Newcastle, USA) kwizinga lokufudumeza/lokupholisa le-10 °C/min kwi-40 °C. kunye ne-90 °C ngokuhlanjwa kwe-nitrogen okuqhubekayo. Uhlalutyo lokunciphisa ubunzima lwenziwe kusetyenziswa i-TGA analyzer (TA Instrument, Discovery TGA, New Castle, USA) kwi-continuous flow ye-nitrogen eqala kwi-40–600 °C, kunye nezinga lokufudumeza le-10 °C/min.
Umfanekiso 3 ubonisa i-FTIR spectra ye-bulk SC kunye ne-microencapsulated SC (SATEOS1, SATEOS2, SATEOS3, SATEOS4, SATEOS5 kunye ne-SATEOS6). Iincopho zokufunxwa kwi-2910 cm-1 kunye ne-2850 cm-1 kuzo zonke iisampuli (SA kunye ne-microencapsulated SA) zibangelwa kukungcangcazela okulinganayo kwamaqela e-–CH3 kunye ne-–CH2, ngokulandelelana kwe-10,50. Incopho kwi-1705 cm-1 ihambelana nokungcangcazela kokungcangcazela kwe-C=O bond. Iincopho kwi-1470 cm-1 kunye ne-1295 cm-1 zibangelwa kukungcangcazela kokugoba kweqela elisebenzayo le-–OH, ngelixa iincopho kwi-940 cm-1 kunye ne-719 cm-1 zihambelana nokungcangcazela kwe-in-plane kunye ne-yield. -plane deformation vibration, ngokulandelelana kwe-OH group. Iincopho zokufunxa ze-SA kwi-2910, 2850, 1705, 1470, 1295, 940 kunye ne-719 cm-1 nazo zabonwa kuyo yonke i-SA ene-microcapsulated. Ukongeza, incopho esandula ukufunyanwa kwi-1103 cm-1 ehambelana nokungcangcazela kokunwebeka okungalinganiyo kwebhendi ye-Si-O-Si yabonwa kwi-microcapsule ye-SA. Iziphumo ze-FT-IR ziyahambelana noYuan et al. 50 Balungiselele ngempumelelo i-SA ene-microcapsulated kwi-ammonia/ethanol ratio kwaye bafumanisa ukuba akukho ntsebenziswano yeekhemikhali eyenzekileyo phakathi kwe-SA kunye ne-SiO2. Iziphumo zophando lwangoku lwe-FT-IR zibonisa ukuba igobolondo le-SiO2 liyifake ngempumelelo i-SA (core) ngenkqubo yokufunxa kunye ne-polymerization ye-TEOS ene-hydrolyzed. Kwi-SA esezantsi, ubunzulu bencopho yebhendi ye-Si-O-Si buphezulu (Umzobo 3b-d). Njengoko ubungakanani be-SA busanda ukuya kuthi ga kwi-15 g, ubunzulu bencochoyi kunye nokwandiswa kwebhendi ye-Si-O-Si buyehla kancinci kancinci, nto leyo ebonisa ukwakheka komaleko omncinci we-SiO2 kumphezulu we-SA.
Iispectra ze-FTIR ze-(a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 kunye (g) SATEOS6.
Iipateni ze-XRD ze-bulk SA kunye ne-microencapsulated SA ziboniswe kuMfanekiso 4. Iincopho ze-XRD zifumaneka kwi-2θ = 6.50° (300), 10.94° (500), 15.46° (700), 20.26° \((\overline {5}ngokwe-JCPDS No. 0381923, 02)\), 21.42° kuzo zonke iisampuli (311), 24.04° (602) kunye ne-39.98° (913) zinikwe i-SA. Ukuphazamiseka kunye nokudibanisa nge-bulk CA ngenxa yezinto ezingaqinisekanga ezifana ne-surfactant (SLS), ezinye izinto ezisele kunye ne-microencapsulation ye-SiO250. Emva kokuba i-encapsulation yenzekile, amandla eencopho eziphambili (300), (500), (311), kunye ne-(602) ancipha kancinci xa kuthelekiswa ne-bulk CA, nto leyo ebonisa ukwehla kwe-crystallinity yesampuli.
Iipateni ze-XRD ze-(a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 kunye (g) SATEOS6.
Ubunzulu be-SATEOS1 buyehla kakhulu xa kuthelekiswa nezinye iisampuli. Akukho zikho ezinye iincopho ezibonwe kuzo zonke iisampuli ezifakwe ii-microcapsulated (Umzobo 4b–g), nto leyo eqinisekisa ukuba ukufunxwa kwe-SiO252 ngokwasemzimbeni kunokuba kubekho ukusebenzisana kweekhemikhali kwenzeka kumphezulu we-SA. Ukongeza, kwagqitywa kwelokuba i-microcapsulation ye-SA ayizange ikhokelele ekubonakaleni kwezakhiwo ezintsha. I-SiO2 ihlala ihleli kumphezulu we-SA ngaphandle kwempendulo yeekhemikhali, kwaye njengoko ubungakanani be-SA buncipha, iincopho ezikhoyo ziyacaca ngakumbi (SATEOS1). Esi siphumo sibonisa ukuba i-SiO2 igubungela umphezulu we-SA ngokubanzi. Incopho kwi-(700) iyanyamalala ngokupheleleyo, kwaye incopho kwi-\((\overline{5}02)\) iba yi-hump kwi-SATEOS 1 (Umzobo 4b), enxulunyaniswa nokuncipha kwekristalinity kunye nokwanda kwe-amorphism. I-SiO2 ayiguquki ngokwendalo, ngoko ke iincopho ezibonwa ukusuka kwi-2θ = 19° ukuya kwi-25° zine-hump kunye nobubanzi53 (Umzobo 4b–g), nto leyo eqinisekisa ukubakho kwe-SiO252 engaguqukiyo. Ubunzulu obuphantsi bencopho yokusasazeka kwe-microencapsulated SA bubangelwa yimpembelelo ye-nucleation yodonga lwangaphakathi lwe-silica kunye nokuziphatha okukhawulezileyo kwe-crystallization49. Kukholelwa ukuba ngomxholo we-SA ophantsi, igobolondo le-silica elijiyileyo lenziwa ngenxa yokubakho kwenani elikhulu le-TEOS, elifunxwa kakhulu kumphezulu wangaphandle we-SA. Nangona kunjalo, njengoko ubungakanani be-SA busanda, indawo yomphezulu wamaconsi e-SA kwisisombululo se-emulsion iyanda kwaye kufuneka i-TEOS engaphezulu ukuze kufakwe i-capsulation efanelekileyo. Ke ngoko, ngomxholo we-SA ophezulu, incopho ye-SiO2 kwi-FT-IR iyacinezelwa (Umzobo 3), kwaye ubunzulu bencopho yokusasazeka kufutshane ne-2θ = 19–25° kwi-XRF (Umzobo 4) buyancipha kwaye nokwanda nako kuncipha. Akubonakali. Nangona kunjalo, njengoko kunokubonwa kuMfanekiso 4, kwangoko nje ukuba ubungakanani be-SA bunyuswe ukusuka kwi-5 g (SATEOS1) ukuya kwi-50 g (SATEOS6), iincopho zisondela kakhulu kwi-bulk SA, kwaye incopho kwi-(700) ibonakala kunye nazo zonke iincopho ezichongiweyo. Esi siphumo sihambelana neziphumo ze-FT-IR, apho ubunzulu bencopho ye-SiO2 SATEOS6 buncipha kwi-1103 cm-1 (Umzobo 3g).
Iimeko zeekhemikhali zezinto ezikhoyo kwi-SA, i-SATEOS1 kunye ne-SATEOS6 ziboniswe kwiMifanekiso 1 kunye ne-2. Imifanekiso 5, 6, 7 kunye ne-8 kunye neTheyibhile 2. Izikena zokulinganisa ze-bulk SA, i-SATEOS1 kunye ne-SATEOS6 ziboniswe kwiMifanekiso 5 kwaye izikena ezinesisombululo esiphezulu se-C 1s, i-O 1s kunye ne-Si 2p ziboniswe kwiMifanekiso 5, 6, 7 kunye ne-8 kunye neTheyibhile 2. 6, 7 kunye ne-8 ngokulandelelana. Amaxabiso amandla okubopha afunyenwe yi-XPS ashwankathelwe kwiTheyibhile 2. Njengoko kunokubonwa kwiMifanekiso 5, iincopho ezicacileyo ze-Si 2s kunye ne-Si 2p zibonwe kwi-SATEOS1 kunye ne-SATEOS6, apho kwenzeka khona i-microencapsulation yegobolondo le-SiO2. Abaphandi bangaphambili baxele ngencopho efanayo ye-Si 2s kwi-155.1 eV54. Ubukho beencopho zeSi kwi-SATEOS1 (Umzobo 5b) kunye ne-SATEOS6 (Umzobo 5c) buqinisekisa idatha ye-FT-IR (Umzobo 3) kunye ne-XRD (Umzobo 4).
Njengoko kubonisiwe kuMfanekiso 6 a, ii-C1s ze-bulk SA zineencam ezintathu ezahlukeneyo ze-CC, i-caliphatic, kunye ne-O=C=O kumandla okubopha, eziyi-284.5 eV, 285.2 eV, kunye ne-289.5 eV, ngokulandelelana. Iincochoyi ze-C–C, i-caliphatic kunye ne-O=C=O nazo zibonwe kwi-SATEOS1 (Umzobo 6b) kunye ne-SATEOS6 (Umzobo 6c) kwaye zishwankathelwe kwiTheyibhile 2. Ukongeza koku, incochoyi ye-C1s ikwahambelana nencochoyi eyongezelelweyo ye-Si-C kwi-283 .1 eV (SATEOS1) kunye ne-283.5 eV (SATEOS6). Amandla ethu okubopha abonwayo e-C–C, i-caliphatic, i-O=C=O kunye ne-Si–C ahambelana kakuhle neminye imithombo55,56.
Iispectra ze-XPS ze-O 1 SA, i-SATEOS1 kunye ne-SATEOS6 ziboniswe kwiMifanekiso 7a–c, ngokulandelelana. Incochoyi ye-O 1s ye-bulk SA ayiguquki kwaye ineencochoyi ezimbini, ezizezi C=O/C–O (531.9 eV) kunye ne-C–O–H (533.0 eV), ngelixa i-O 1 ye-SATEOS1 kunye ne-SATEOS6 zihambelana. Kukho iincochoyi ezintathu kuphela: C=O/C–O, C–O–H kunye ne-Si–OH55,57,58. Amandla okubopha e-O 1s kwi-SATEOS1 kunye ne-SATEOS6 atshintsha kancinci xa kuthelekiswa ne-bulk SA, enxulunyaniswa notshintsho kwiqhekeza leekhemikhali ngenxa yokubakho kwe-SiO2 kunye ne-Si-OH kwizinto zegobolondo.
Iispectra zeSi 2p XPS ze-SATEOS1 kunye ne-SATEOS6 ziboniswe kuMfanekiso 8a kunye no-b, ngokulandelelana. Kwi-CA enkulu, i-Si 2p ayizange ibonwe ngenxa yokungabikho kwe-SiO2. Incochoyi yeSi 2p ihambelana ne-105.4 eV ye-SATEOS1 kunye ne-105.0 eV ye-SATEOS6, ehambelana ne-Si-O-Si, ngelixa incochoyi ye-SATEOS1 iyi-103.5 eV kwaye incochoyi ye-SATEOS6 iyi-103.3 eV, ehambelana ne-Si-OH55. Ukufakwa kwencochoyi yeSi-O-Si kunye ne-Si-OH kwi-SATEOS1 kunye ne-SATEOS6 kubonakalise impumelelo ye-microencapsulation ye-SiO2 kumphezulu ongundoqo we-SA.
Imo yezinto ezifakwe kwi-microcapsulation ibaluleke kakhulu, ichaphazela ukunyibilika, uzinzo, ukusabela kweekhemikhali, ukuhamba kwamanzi kunye namandla59. Ke ngoko, i-SEM yasetyenziswa ukuchaza imo ye-bulk SA (100×) kunye ne-microcapsulated SA (500×), njengoko kubonisiwe kuMfanekiso 9. Njengoko kunokubonwa kuMfanekiso 9a, ibhloko ye-SA inomfanekiso we-elliptical. Ubungakanani be-particle budlula i-500 microns. Nangona kunjalo, xa inkqubo ye-microcapsulation iqhubeka, imo itshintsha kakhulu, njengoko kubonisiwe kuMfanekiso 9 b–g.
Imifanekiso ye-SEM ka-(a) SA (×100), (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 kunye (g) SATEOS6 kwi ×500.
Kwisampulu ye-SATEOS1, kubonwa amasuntswana amancinci e-SA agqunywe yi-SiO2-wrapped e-quasi-spherical anomphezulu orhabaxa (Umzobo 9b), okunokuba kungenxa ye-hydrolysis kunye ne-condensation polymerization ye-TEOS kumphezulu we-SA, okukhawulezisa ukusasazeka ngokukhawuleza kweemolekyuli ze-ethanol. Ngenxa yoko, amasuntswana e-SiO2 afakwa kwaye i-agglomeration ibonwa52,60. Eli qokobhe le-SiO2 linika amandla oomatshini kumasuntswana e-CA agqunywe nge-microcapsulated kwaye likwathintela ukuvuza kwe-CA enyibilikisiweyo kumaqondo obushushu aphezulu10. Esi siphumo sibonisa ukuba ii-microcapsules ze-SA eziqulethe i-SiO2 zingasetyenziswa njengezinto zokugcina amandla ezinokubakho61. Njengoko kunokubonwa kuMfanekiso 9b, isampulu ye-SATEOS1 inosasazo olufanayo lwamasuntswana olune-SiO2 engqindilili egqume i-SA. Ubungakanani bamasuntswana e-microencapsulated SA (SATEOS1) bumalunga ne-10–20 μm (Umzobo 9b), obuncinci kakhulu xa kuthelekiswa ne-bulk SA ngenxa yomxholo ophantsi we-SA. Ubukhulu bomaleko we-microcapsule bubangelwa yi-hydrolysis kunye ne-condensation polymerization yesisombululo se-precursor. I-Agglomeration yenzeka kwiidosi eziphantsi ze-SA, oko kukuthi ukuya kuthi ga kwi-15 g (Umzobo 9b-d), kodwa kwangoko nje ukuba idosi inyuswe, akukho agglomeration ibonwayo, kodwa amasuntswana acacileyo ajikelezayo ayabonwa (Umzobo 9e-g) 62.
Ukongeza, xa ubungakanani be-SLS surfactant buhlala bunjalo, umxholo we-SA (SATEOS1, SATEOS2 kunye ne-SATEOS3) nawo uchaphazela ukusebenza kakuhle, imo kunye nokusasazwa kobungakanani be-particle. Ngoko ke, i-SATEOS1 ifunyenwe ibonisa ubungakanani be-particle obuncinci, ukusasazwa okufanayo kunye nomphezulu oxineneyo (Umzobo 9b), obangelwe yi-hydrophilic nature ye-SA ekhuthaza i-nucleation yesibini phantsi kwe-surfactant engaguqukiyo63. Kukholelwa ukuba ngokunyusa umxholo we-SA ukusuka kwi-5 ukuya kwi-15 g (SATEOS1, SATEOS2 kunye ne-SATEOS3) kunye nokusebenzisa ubungakanani obuhlala bunjalo be-surfactant, oko kukuthi i-0.10 g SLS (Itheyibhile 1), igalelo le-particle nganye ye-surfactant molecule liya kuncipha, ngaloo ndlela kunciphisa ubungakanani be-particle kunye nobukhulu be-particle. Ukusasazwa kwe-SATEOS2 (Umzobo 9c) kunye ne-SATEOS3 (Umzobo 9d) kwahlukile kukusasazwa kwe-SATEOS 1 (Umzobo 9b).
Xa kuthelekiswa ne-SATEOS1 (Umzobo 9b), i-SATEOS2 ibonise imo exineneyo ye-SA efakwe i-microcapsulated kwaye ubungakanani be-particle buyanda (Umzobo 9c). Oku kungenxa ye-agglomeration 49, enciphisa izinga lokujiya (Umzobo 2b). Njengoko ubungakanani be-SC busanda ngokwanda kwe-SLS, ii-microcapsules zibonakala ngokucacileyo, njengoko kuboniswe kwi-Fig. indlela ukuhlanganiswa okwenzeka ngayo. Ukongeza, iMifanekiso 9e-g ibonisa ukuba zonke ii-particles zicacile ukuba ziyi-spherical ngesimo kunye nobukhulu. Kuye kwaqatshelwa ukuba xa kukho inani elikhulu le-SA, inani elifanelekileyo le-oligomers ye-silica linokufunyanwa, nto leyo ebangela ukujiya kunye nokugqunywa okufanelekileyo kwaye ngaloo ndlela kudalwa ii-microcapsules ezichazwe kakuhle49. Kwiziphumo ze-SEM, kuyacaca ukuba i-SATEOS6 yenze ii-microcapsules ezifanayo xa kuthelekiswa nenani elincinci le-SA.
Iziphumo ze-energy dispersive X-ray spectroscopy (EDS) ye-bulk SA kunye ne-microcapsule SA ziboniswe kwiTheyibhile 3. Njengoko kunokubonwa kule theyibhile, umxholo we-Si uyancipha kancinci kancinci ukusuka kwi-SATEOS1 (12.34%) ukuya kwi-SATEOS6 (2.68%). Ukwanda kwi-SA. Ke ngoko, singatsho ukuba ukwanda kobungakanani be-SA kukhokelela ekunciphiseni kokufakwa kwe-SiO2 kumphezulu we-SA. Akukho maxabiso ahambelanayo omxholo we-C kunye ne-O kwiTheyibhile 3 ngenxa yohlalutyo oluyi-semi-quantitative lwe-EDS51. Umxholo we-Si we-microencapsulated SA unxulumene neziphumo ze-FT-IR, XRD kunye ne-XPS.
Indlela yokunyibilika nokuqina kwe-bulk SA kunye ne-microencapsulated SA ene-SiO2 shell iboniswe kwiMifanekiso 1 kunye ne-2. Iboniswe kwiMifanekiso 10 kunye ne-11 ngokulandelelana, kwaye idatha yobushushu iboniswe kwiTheyibhile 4. Amaqondo obushushu okunyibilika nokuqina kwe-microencapsulated SA afunyenwe ahlukile. Njengoko ubungakanani be-SA bukhula, amaqondo obushushu okunyibilika nokuqina ayanda kwaye asondela kumaxabiso e-bulk SA. Emva kwe-SA microencapsulation, udonga lwe-silica lonyusa amaqondo obushushu e-crystallization, kwaye udonga lwalo lusebenza njengesiseko sokukhuthaza ukungafani. Ke ngoko, njengoko ubungakanani be-SA bukhula, amaqondo obushushu okunyibilika (Umzobo 10) kunye nokuqina (Umzobo 11) nawo ayanda kancinci kancinci49,51,64. Kuzo zonke iisampulu ze-SA ezincinci, i-SATEOS6 ibonise amaqondo obushushu aphezulu okunyibilika nokuqina, ilandelwa yi-SATEOS5, SATEOS4, SATEOS3, SATEOS2, kunye ne-SATEOS1.
I-SATEOS1 ibonisa indawo esezantsi yokunyibilika (68.97 °C) kunye nobushushu bokuqina (60.60 °C), okubangelwa bubungakanani obuncinci be-particle apho intshukumo yee-particles ze-SA ngaphakathi kwi-microcapsules incinci kakhulu kwaye i-shell ye-SiO2 yenza umaleko otyebileyo kwaye yiyo loo nto iCore Material inciphisa ukunwebeka kunye nokuhamba49. Le ngcamango inxulumene neziphumo ze-SEM, apho i-SATEOS1 ibonise ubungakanani obuncinci be-particles (Umzobo 9b), okubangelwa kukuba iimolekyuli ze-SA zivaleleke kwindawo encinci kakhulu yee-microcapsules. Umahluko kumaqondo obushushu okunyibilika kunye nokuqina kobunzima obuphambili, kunye nazo zonke ii-microcapsules ze-SA ezinee-shells ze-SiO2, ukwi-6.10–8.37 °C. Esi siphumo sibonisa ukuba i-SA ene-microcapsulated ingasetyenziswa njengesixhobo sokugcina amandla esinokubakho ngenxa yokuqhuba kakuhle kobushushu be-shell ye-SiO2 65.
Njengoko kunokubonwa kwiTheyibhile 4, i-SATEOS6 ine-enthalpy ephezulu phakathi kwazo zonke ii-SC ezifakwe i-microcapsulated (Umzobo 9g) ngenxa yokufunxwa okufanelekileyo okubonwe yi-SEM. Izinga lokupakisha le-SA lingabalwa kusetyenziswa i-equation (1). (1) Ngokuthelekisa idatha yobushushu obufihlakeleyo be-microcapsulated SA49.
Ixabiso le-R limele idigri yokugquma (%) ye-SC egqumayo encinci, i-ΔHMEPCM, m imele ubushushu obufihlakeleyo bokuhlanganiswa kwe-SC egqumayo encinci, kwaye i-ΔHPCM, m imele ubushushu obufihlakeleyo bokuhlanganiswa kwe-SC. Ukongeza, ukusebenza kakuhle kokupakisha (%) kubalwa njengenye iparameter ebalulekileyo yobugcisa, njengoko kubonisiwe kwi-Equation (1). (2)49.
Ixabiso le-E limele ukusebenza kakuhle kwe-encapsulation (%) ye-microencapsulated CA, i-ΔHMEPCM,s imele ubushushu obufihlakeleyo bokuphiliswa kwe-microencapsulated CA, kwaye i-ΔHPCM,s imele ubushushu obufihlakeleyo bokuphiliswa kwe-CA.
Njengoko kubonisiwe kwiTheyibhile 4, inqanaba lokupakisha kunye nokusebenza kakuhle kwe-SATEOS1 yi-71.89% kunye ne-67.68%, ngokwahlukeneyo, kwaye inqanaba lokupakisha kunye nokusebenza kakuhle kwe-SATEOS6 yi-90.86% kunye ne-86.68%, ngokwahlukeneyo (Itheyibhile 4). Isampuli ye-SATEOS6 ibonisa i-coefficient ephezulu ye-encapsulation kunye nokusebenza kakuhle phakathi kwazo zonke ii-SA ezifakwe kwi-microcapsulated, nto leyo ebonisa amandla ayo aphezulu obushushu. Ke ngoko, utshintsho ukusuka kwi-solid ukuya kwi-liquid lufuna amandla amaninzi. Ukongeza, umahluko kumaqondo obushushu okunyibilika kunye nokuqina kwawo onke ama-microcapsule e-SA kunye ne-bulk SA ngexesha lenkqubo yokupholisa lubonisa ukuba igobolondo le-silica livalelwe kwindawo ngexesha lokwenziwa kwe-microcapsule. Ke ngoko, iziphumo zibonisa ukuba njengoko ubungakanani be-SC busanda, isantya se-encapsulation kunye nokusebenza kakuhle kuyanda kancinci kancinci (Itheyibhile 4).
Iigophe ze-TGA ze-bulk SA kunye ne-microcapsule SA eneqokobhe le-SiO2 (i-SATEOS1, i-SATEOS3 kunye ne-SATEOS6) ziboniswe kuMfanekiso 12. Iimpawu zozinzo lobushushu be-bulk SA (i-SATEOS1, i-SATEOS3 kunye ne-SATEOS6) zithelekiswa neesampuli ze-microencapsulated. Kucacile kwigophe le-TGA ukuba ukulahleka kobunzima be-bulk SA kunye ne-microencapsulated SA kubonisa ukwehla okuthe tye nokuncinci kakhulu ukusuka kwi-40°C ukuya kwi-190°C. Kolu bushushu, i-bulk SC ayiboli ngobushushu, ngelixa i-microencapsulated SC ikhupha amanzi afakwe kwi-adsorbed nasemva kokuba yomile kwi-45°C kangangeeyure ezingama-24. Oku kubangele ukwehla kobunzima okuncinci,49 kodwa ngaphaya kobu bushushu izinto zaqala ukonakala. Kumxholo ophantsi we-SA (umz. i-SATEOS1), umxholo wamanzi afakwe kwi-adsorbed uphezulu kwaye ngenxa yoko ukulahleka kobunzima ukuya kuthi ga kwi-190 °C kuphezulu (i-inset kwiFig. 12). Kwakuba nje ubushushu bunyuke ngaphezu kwe-190 °C, isampuli iqala ukulahleka kobunzima ngenxa yeenkqubo zokubola. I-Bulk SA iqala ukubola kwi-190 °C kwaye yi-4% kuphela ehlala kwi-260 °C, ngelixa i-SATEOS1, i-SATEOS3 kunye ne-SATEOS6 zigcina i-50%, i-20% kunye ne-12% kobu bushushu, ngokwahlukeneyo. Emva kwe-300 °C, ukulahleka kobunzima be-bulk SA bekumalunga ne-97.60%, ngelixa ukulahleka kobunzima be-SATEOS1, i-SATEOS3, kunye ne-SATEOS6 bekumalunga ne-54.20%, i-82.40%, kunye ne-90.30% ngokwahlukeneyo. Ngokunyuka komxholo we-SA, umxholo we-SiO2 uyancipha (Itheyibhile 3), kwaye ukuncitshiswa kwegobolondo kubonwa kwi-SEM (Umzobo 9). Ngoko ke, ukulahleka kobunzima be-SA efakwe kwi-microcapsulated kuphantsi xa kuthelekiswa ne-bulk SA, echazwa ziimpawu ezilungileyo zeqokobhe le-SiO2, elikhuthaza ukwakheka komaleko we-carbonaceous silicate-carbonaceous kumphezulu we-SA, ngaloo ndlela lihlukanisa umongo we-SA kwaye licothisa ukukhululwa kweemveliso eziguquguqukayo ezivelayo10. Olu maleko we-char lwenza umqobo wokukhusela ngokomzimba ngexesha lokubola kobushushu, luthintela ukuguquka kweemolekyuli ezinokutsha ziye kwi-gas phase66,67. Ukongeza koku, sinokubona neziphumo ezibalulekileyo zokulahlekelwa bubunzima: I-SATEOS1 ibonisa amaxabiso aphantsi xa kuthelekiswa ne-SATEOS3, i-SATEOS6 kunye ne-SA. Oku kungenxa yokuba ubungakanani be-SA kwi-SATEOS1 bungaphantsi kune-SATEOS3 kunye ne-SATEOS6, apho iqokobhe le-SiO2 lenza umaleko otyebileyo. Ngokwahlukileyo koko, ukulahleka kobunzima bubonke be-bulk SA kufikelela kwi-99.50% kwi-415 °C. Nangona kunjalo, i-SATEOS1, i-SATEOS3, kunye ne-SATEOS6 zibonise ukwehla kobunzima ngama-62.50%, 85.50%, kunye nama-93.76%, ngokulandelelana, kwi-415 °C. Esi siphumo sibonisa ukuba ukongezwa kwe-TEOS kuphucula ukonakala kwe-SA ngokwenza umaleko we-SiO2 kumphezulu we-SA. Ezi layers zinokwenza umqobo wokukhusela ngokwasemzimbeni, kwaye ke ngoko ukuphucuka kozinzo lobushushu lwe-microencapsulated CA kunokubonwa.
Iziphumo zokuthembeka kobushushu ze-bulk SA kunye nesampulu engcono kakhulu ye-microencapsulated (oko kukuthi i-SATEOS 6) emva kwemijikelo yokufudumeza nokupholisa engama-30 ye-DSC51,52 ziboniswe kuMfanekiso 13. Kuyabonakala ukuba i-bulk SA (Umfanekiso 13a) ayibonisi mahluko kwixabiso lobushushu bokunyibilika. ukuqina kunye ne-enthalpy, ngelixa i-SATEOS6 (Umfanekiso 13b) ingabonisi mahluko kwixabiso lobushushu kunye ne-enthalpy nasemva komjikelo wama-30 wokufudumala. kunye nenkqubo yokupholisa. I-Bulk SA ibonise iqondo lokunyibilika elingama-72.10 °C, ubushushu bokuqina obungama-64.69 °C, kunye nobushushu bokudibanisa kunye nokuqina emva komjikelo wokuqala babuyi-201.0 J/g kunye ne-194.10 J/g, ngokwahlukeneyo. Emva komjikelo wama-30, iqondo lokunyibilika kwala maxabiso liye lehla laya kwi-71.24 °C, iqondo lokuqina lehla laya kwi-63.53 °C, kwaye ixabiso le-enthalpy lehla nge-10%. Utshintsho kumaqondo obushushu okunyibilika nokuqina, kunye nokwehla kwamaxabiso e-enthalpy, kubonisa ukuba i-bulk CA ayithembekanga kwizicelo ezingezizo ze-microencapsulation. Nangona kunjalo, emva kokuba kwenzeke i-microencapsulation efanelekileyo (SATEOS6), amaqondo obushushu okunyibilika nokuqina kunye namaxabiso e-enthalpy awatshintshi (Umzobo 13b). Nje ukuba ifakwe i-microencapsulated ngeegobolondo ze-SiO2, i-SA ingasetyenziswa njengesixhobo sokutshintsha isigaba kwizicelo zobushushu, ngakumbi ekwakheni, ngenxa yamaqondo obushushu ayo afanelekileyo okunyibilika nokuqina kunye ne-enthalpy ezinzileyo.
Ii-DSC curves ezifunyenweyo kwiisampulu ze-SA (a) kunye ne-SATEOS6 (b) kwimijikelo yoku-1 neye-30 yokufudumeza nokupholisa.
Kolu phononongo, uphando olucwangcisiweyo lwe-microencapsulation lwenziwe kusetyenziswa i-SA njengezinto eziphambili kunye ne-SiO2 njengezinto zegobolondo. I-TEOS isetyenziswa njengesandulela sokwenza umaleko wenkxaso ye-SiO2 kunye nomaleko okhuselayo kumphezulu we-SA. Emva kokuhlanganiswa ngempumelelo kwe-microencapsulated SA, iziphumo ze-FT-IR, XRD, XPS, SEM kunye ne-EDS zibonise ubukho be-SiO2. Uhlalutyo lwe-SEM lubonisa ukuba isampuli ye-SATEOS6 ibonisa amasuntswana acacileyo ajikelezwe ziigobolondo ze-SiO2 kumphezulu we-SA. Nangona kunjalo, i-MEPCM enomxholo we-SA ophantsi ibonisa i-agglomeration, nto leyo enciphisa ukusebenza kwe-PCM. Uhlalutyo lwe-XPS lubonise ubukho be-Si-O-Si kunye ne-Si-OH kwiisampulu ze-microcapsule, nto leyo etyhile ukufunxwa kwe-SiO2 kumphezulu we-SA. Ngokwendlela esebenza ngayo i-thermal analysis, i-SATEOS6 ibonisa amandla okugcina ubushushu athembisayo, kunye namaqondo obushushu okunyibilika nokuqina angama-70.37°C kunye nama-64.27°C, ngokwahlukeneyo, kunye nobushushu obufihlakeleyo bokunyibilika nokuqina obuyi-182.53 J/g kunye ne-160.12 J/g. G. ngokwahlukeneyo. Ukusebenza okuphezulu kokupakishwa kwe-SATEOS6 yi-86.68%. Uhlalutyo lomjikelo wobushushu we-TGA kunye ne-DSC luqinisekisile ukuba i-SATEOS6 isenozinzo oluhle lobushushu kunye nokuthembeka nasemva kweenkqubo zokufudumeza nokupholisa ezingama-30.
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