Ama-Microcapsule e-SiO2 Shelled Stearic Acid njengezinto zokushintsha isigaba sokugcina amandla okungenzeka

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I-Stearic acid (SA) isetshenziswa njengezinto zokushintsha isigaba (PCM) kumadivayisi okugcina amandla. Kulolu cwaningo, indlela ye-sol-gel isetshenziswe ukufaka i-surfactant yegobolondo le-SiO2 nge-microcapsulate. Amanani ahlukahlukene e-SA (5, 10, 15, 20, 30, kanye no-50 g) afakwe ku-10 mL ye-tetraethyl orthosilicate (TEOS). Izinto zokushintsha isigaba ze-microencapsulated ezihlanganisiwe (MEPCM) zibonakaliswe yi-Fourier transform infrared spectroscopy (FT-IR), i-X-ray diffraction (XRD), i-X-ray photoelectron spectroscopy (XPS), kanye ne-scanning electron microscopy (SEM). Imiphumela yokuchaza ibonise ukuthi i-SA ifakwe ngempumelelo yi-SiO2. Ukuhlaziywa kwe-Thermogravimetric (TGA) kubonise ukuthi i-MEPCM inokuqina okungcono kokushisa kune-CA. Kusetshenziswa i-calorimetry yokuskena ehlukene (DSC), kutholakale ukuthi inani le-enthalpy le-MEPCM alishintshanga ngisho nangemva kwemijikelezo engu-30 yokupholisa ukushisa. Phakathi kwazo zonke izibonelo ezifakwe ema-microcapsulated, ama-50 g e-SA aqukethe i-MEPCM ayenokushisa okuphezulu kakhulu kokuncibilika nokuqina, okwakungu-182.53 J/g kanye no-160.12 J/g, ngokulandelana. Inani lokusebenza kahle kwephakeji libalwe kusetshenziswa idatha yokushisa futhi ukusebenza kahle okuphezulu kutholakale kusampula efanayo okwakungu-86.68%.
Cishe u-58% wamandla asetshenziswa embonini yokwakha asetshenziselwa ukushisa nokupholisa izakhiwo1. Ngakho-ke, into ebaluleke kakhulu ukudala izinhlelo zamandla ezisebenzayo ezicabangela ukungcola kwemvelo2. Ubuchwepheshe bokushisa obucashile obusebenzisa izinto zokushintsha isigaba (i-PCM) bungagcina amandla aphezulu ekushintsheni kwezinga lokushisa okuphansi3,4,5,6 futhi bungasetshenziswa kabanzi emikhakheni efana nokudluliselwa kokushisa, isitoreji samandla elanga, izindiza kanye ne-air conditioner7,8,9. I-PCM imunca amandla okushisa avela ngaphandle kwesakhiwo emini futhi ikhipha amandla ebusuku10. Ngakho-ke, izinto zokushintsha isigaba zinconywa njengezinto zokugcina amandla okushisa. Ngaphezu kwalokho, kunezinhlobo ezahlukene zama-PCM njenge-solid-solid, solid-liquid, liquid-gas kanye ne-solid-gas11. Phakathi kwazo, izinto zokushintsha isigaba ezithandwa kakhulu nezisetshenziswa njalo yizinto zokushintsha isigaba eziqinile kanye nezinto zokushintsha isigaba eziqinile. Kodwa-ke, ukusetshenziswa kwazo kunzima kakhulu ngenxa yezinguquko ezinkulu zevolumu zezinto zokushintsha isigaba eziqinile kanye ne-solid-gas.
I-PCM inezinhlelo zokusebenza ezahlukahlukene ngenxa yezakhiwo zayo: lezo ezincibilika emazingeni okushisa angaphansi kuka-15°C zingasetshenziswa ezinhlelweni zokupholisa umoya ukuze zigcine amazinga okushisa abandayo, kanti lezo ezincibilika emazingeni okushisa angaphezu kuka-90°C zingasetshenziswa ezinhlelweni zokushisa ukuvimbela imililo. Kuye ngokusetshenziswa kanye nobubanzi bamaphuzu okuncibilika, izinto ezahlukahlukene zokushintsha isigaba zenziwe ngamakhemikhali ahlukene e-organic kanye ne-inorganic13,14,15. I-paraffin iyinto esetshenziswa kakhulu yokushintsha isigaba enokushisa okuphezulu okucashile, ukungaboli, ukuphepha kanye nobubanzi bamaphuzu okuncibilika16,17,18,19,20,21.
Kodwa-ke, ngenxa yokushisa okuphansi kwezinto zokushintsha isigaba, zidinga ukumbozwa egobolondweni (ungqimba lwangaphandle) ukuvimbela ukuvuza kwezinto eziyisisekelo ngesikhathi senqubo yokushintsha isigaba22. Ngaphezu kwalokho, amaphutha okusebenza noma ingcindezi yangaphandle ingalimaza ungqimba lwangaphandle (ukumbozwa), futhi izinto zokushintsha isigaba ezincibilikisiwe zingasabela ezintweni zokwakha, okubangela ukugqwala kwemigoqo yensimbi ehlanganisiwe, ngaleyo ndlela kuncishiswe ukusebenza kwesakhiwo23. Ngakho-ke, kubalulekile ukuhlanganisa izinto zokushintsha isigaba ezimboziwe ngezinto ezanele zegobolondo, ezingaxazulula izinkinga ezingenhla24.
Ukufakwa kwe-microcapsulation kwezinto zokushintsha isigaba kungakhuphula ngempumelelo ukudluliselwa kokushisa futhi kunciphise ukusabela kwemvelo, futhi kulawule izinguquko zevolumu. Izindlela ezahlukahlukene ziye zathuthukiswa zokufakwa kwe-PCM, okungukuthi i-interfacial polymerization25,26,27,28, i-in situ polymerization29,30,31,32, i-coacervation33,34,35 kanye nezinqubo ze-sol-gel36,37,38,39. I-formaldehyde resin ingasetshenziswa kwi-microencapsulation40,41,42,43. Ama-Melamine-formaldehyde kanye nama-urea-formaldehyde resins asetshenziswa njengezinto zegobolondo, ezivame ukukhipha i-formaldehyde enobuthi ngesikhathi sokusebenza. Ngakho-ke, lezi zinto azivunyelwe ukusetshenziswa ezinqubweni zokupakisha. Kodwa-ke, izinto zokushintsha isigaba ezinobungani nemvelo zokugcina amandla okushisa angalinganiswa zingakhiwa kusetshenziswa ama-nanocapsules ahlanganisiwe asekelwe kuma-fatty acid kanye ne-lignin44.
UZhang nabanye 45 nabanye bahlanganisa i-lauric acid kusuka ku-tetraethyl orthosilicate futhi baphetha ngokuthi njengoba isilinganiso sevolumu se-methyltriethoxysilane kuya ku-tetraethyl orthosilicate sanda, ukushisa okucashile kwehla futhi i-surface hydrophobicity yanda. I-Lauric acid ingaba yinto eyinhloko engaba khona futhi ephumelelayo ye-kapok fibers46. Ngaphezu kwalokho, uLatibari nabanye 47 bahlanganisa ama-PCM asekelwe ku-stearic acid besebenzisa i-TiO2 njengento yegobolondo. UZhu nabanye balungiselela ama-nanocapsule e-n-octadecane kanye ne-silicone njenge-PCMs engaba khona 48. Kusukela ekubuyekezweni kwezincwadi, kunzima ukuqonda umthamo onconywayo wokwakheka kwezinto zokushintsha isigaba ezisebenza kahle nezizinzile ze-microencapsulated.
Ngakho-ke, ngokwazi kwababhali, inani lezinto zokushintsha isigaba ezisetshenziselwa i-microencapsulation liyipharamitha ebalulekile yokukhiqizwa kwezinto zokushintsha isigaba ezisebenza kahle futhi ezizinzile. Ukusebenzisa amanani ahlukene ezinto zokushintsha isigaba kuzosenza sikwazi ukucacisa izakhiwo ezahlukene kanye nokuqina kwezinto zokushintsha isigaba ezifakwe i-microencapsulated. I-Stearic acid (i-fatty acid) iyisithako esinobungani nemvelo, esibalulekile kwezokwelapha futhi esingabizi esingasetshenziswa ukugcina amandla okushisa ngoba inenani eliphezulu le-enthalpy (~200 J/g) futhi ingamelana namazinga okushisa afinyelela ku-72 °C. Ngaphezu kwalokho, i-SiO2 ayishisi, inikeza amandla aphezulu omshini, ukuqhuba ukushisa kanye nokumelana okungcono kwamakhemikhali ezintweni eziyinhloko, futhi isebenza njengezinto ezi-pozzolanic ekwakheni. Lapho usimende uxutshwa namanzi, ama-PCM afakwe i-capsulation angaqhekeka ngenxa yokuguguleka komshini kanye namazinga okushisa aphezulu (ukushisa komswakama) akhiqizwa ezakhiweni ezinkulu zekhonkrithi. Ngakho-ke, ukusetshenziswa kwe-CA efakwe i-microencapsulated enegobolondo le-SiO2 kungaxazulula le nkinga. Ngakho-ke, inhloso yalolu cwaningo kwakuwukuphenya ukusebenza kahle kwama-PCM akhiwe yinqubo ye-sol-gel ekusetshenzisweni kokwakha. Kulo msebenzi, sifunde ngokuhlelekile amanani ahlukene e-SA (njengezinto eziyisisekelo) angu-5, 10, 15, 20, 30 kanye no-50 g afakwe emagobolondweni e-SiO2. Inani elinqunyiwe le-tetraethylorthosilicate (TEOS) kumthamo we-10 ml lasetshenziswa njengesixazululo sokuqala sokwakheka kwegobolondo le-SiO2.
I-stearic acid ye-reactive grade (SA, C18H36O2, iphuzu lokuncibilika: 72°C) njengoba izinto eziyinhloko zathengwa kwa-Daejung Chemical & Metals Co., Ltd., Gyeonggi-do, eNingizimu Korea. I-Tetraethylorthosilicate (TEOS, C8H20O4Si) njengesixazululo sangaphambi kwalokhu yathengwa kwa-Acros Organics, Geel, eBelgium. Ngaphezu kwalokho, i-absolute ethanol (EA, C2H5OH) kanye ne-sodium lauryl sulfate (SLS, C12H25NaO4S) zathengwa kwa-Daejung Chemical & Metals Co., Ltd, Gyeonggi-do, eNingizimu Korea, futhi zasetshenziswa njengezinyibilikisi kanye nama-surfactants, ngokulandelana. Amanzi ahluziwe nawo asetshenziswa njengesinyibilikisi.
Amanani ahlukene e-SA axutshwe nezilinganiso ezahlukene ze-sodium lauryl sulfate (SLS) ku-100 mL wamanzi acwecwe kusetshenziswa i-magnetic stirrer ku-800 rpm kanye no-75 °C ihora eli-1 (Ithebula 1). Ama-emulsion e-SA ahlukaniswe ngamaqembu amabili: (1) 5, 10 kanye no-15 g we-SA axutshwe no-0.10 g we-SLS ku-100 ml wamanzi acwecwe (SATEOS1, SATEOS2 kanye no-SATEOS3), (2) 20, 30 kanye no-50 g we-SA axutshwe no-0.15, 0.20 kanye no-0.25 g we-SLS axutshwe no-100 ml wamanzi acwecwe (SATEOS4, SATEOS5 kanye no-SATEOS6). 0.10 g SLS yasetshenziswa ne-5, 10 kanye no-15 g SA ukwakha ama-emulsion afanele. Ngemva kwalokho, kwaphakanyiswa ukwandisa inani le-SLS ye-SATEOS4, SATEOS5 kanye no-SATEOS6. Ithebula 1 libonisa izilinganiso ze-CA kanye ne-SLS ezisetshenziswa ukuthola izixazululo ze-emulsion ezizinzile.
Faka i-TEOS engu-10 ml, i-ethanol engu-10 ml (EA) kanye namanzi acwecwe angu-20 ml ku-beaker engu-100 ml. Ukuze kufundwe ukusebenza kahle kwe-encapsulation kwezilinganiso ezahlukene zamagobolondo e-SA kanye ne-SiO2, kwaqoshwa i-synthesis coefficient yawo wonke amasampula. Ingxube yavuselelwa nge-magnetic stirrer ku-400 rpm kanye no-60°C ihora eli-1. Isixazululo sangaphambi kwalokho safakwa nge-dropwise ku-SA emulsion elungisiwe, savuselelwa ngamandla ku-800 rpm kanye no-75 °C amahora ama-2, futhi sahlungwa ukuze kutholakale i-white powder. I-white powder yagezwa ngamanzi acwecwe ukuze kususwe i-SA esele futhi yomiswe kuhhavini we-vacuum ku-45°C amahora angama-24. Ngenxa yalokho, kwatholakala i-SC encane ene-shell ye-SiO2. Yonke inqubo yokwenziwa nokulungiswa kwe-microencapsulated SA iboniswe ku-Figure 1.
Ama-microcapsule e-SA anegobolondo le-SiO2 alungiswa ngendlela ye-sol-gel, futhi indlela yawo yokufaka i-capsulation iboniswe ku-Figure 2. Isinyathelo sokuqala sihilela ukulungiselela i-emulsion ye-SA kwisisombululo samanzi esine-SLS njenge-surfactant. Kulesi simo, ukuphela kwe-hydrophobic kwe-molecule ye-SA kubopha ku-SLS, kanye ne-hydrophilic kuma-molecule wamanzi, kwakha i-emulsion ezinzile. Ngakho-ke, izingxenye ze-hydrophobic ze-SLS zivikelwe futhi zimboza ubuso be-droplet ye-SA. Ngakolunye uhlangothi, i-hydrolysis yezixazululo ze-TEOS yenzeka kancane ngama-molecule wamanzi, okuholela ekwakhekeni kwe-hydrolyzed TEOS lapho kukhona i-ethanol (Fig. 2a) 49,50,51. I-Hydrolyzed TEOS idlula ekusabeleni kokujiya, lapho i-n-hydrolyzed TEOS yakha ama-silica clusters (Fig. 2b). Ama-silica clusters afakwe i-SA52 lapho kukhona i-SLS (Fig. 2c), ebizwa ngokuthi inqubo ye-microencapsulation.
Umdwebo weskimu we-microencapsulation ye-CA enegobolondo le-SiO2 (a) i-hydrolysis ye-TEOS (b) ukujiya kwe-hydrolyzate kanye (c) ukufakwa kwe-CA negobolondo le-SiO2.
Ukuhlaziywa kwamakhemikhali kwe-bulk SA kanye ne-microencapsulated SA kwenziwa kusetshenziswa i-Fourier transform infrared spectrometer (FT-IR, Perkin Elmer UATR Two, USA) kanti ama-spectra aqoshwa kusukela ku-500 kuya ku-4000 cm-1.
I-X-ray diffractometer (XRD, D/MAX-2500, Rigaku, Japan) yasetshenziswa ukuhlaziya izigaba ze-bulk SA kanye nezinto ze-microcapsule. Ukuskena kwesakhiwo se-X-ray kwenziwa ebangeni elingu-2θ = 5°–95° ngesivinini sokuskena esingu-4°/min, kusetshenziswa imisebe ye-Cu-Kα (λ = 1.541 Å), izimo zokusebenza ezingu-25 kV kanye ne-100 mA, kwimodi yokuskena eqhubekayo. Izithombe ze-X-ray zakhiwe ebangeni elingu-2θ = 5–50°, njengoba kungekho kuphakama okubonwe ngemuva kwama-50° kuzo zonke izibonelo.
I-X-ray photoelectron spectroscopy (XPS, Scienta Omicron R3000, USA) yenziwe kusetshenziswa i-Al Kα (1486.6 eV) njengomthombo we-X-ray ukuqonda isimo samakhemikhali se-bulk SA kanye nezakhi ezikhona ezintweni ezihlanganisiwe. Ama-XPS spectra aqoqwe alinganiswa ku-C 1s peak kusetshenziswa i-exotic carbon (amandla okubopha angu-284.6 eV). Ngemva kokulungiswa kwangemuva kusetshenziswa indlela ye-Shirley, iziqongo ezinesinqumo esiphezulu zesakhi ngasinye zasuswa futhi zafakwa emisebenzini ye-Gaussian/Lorentzian kusetshenziswa isofthiwe ye-CASA XPS.
Ukwakheka kwe-bulk SC kanye ne-microencapsulated SC kuhlolwe kusetshenziswa i-scanning electron microscopy (SEM, MIRA3, TESCAN, Brno, Czech Republic) ehlonyiswe nge-energy-dispersive X-ray spectroscopy (EDS) ku-15 kV. Ngaphambi kokuthwebula izithombe ze-SEM, amasampula agcotshwa nge-platinum (Pt) ukuze kugwenywe imiphumela yokushaja.
Izakhiwo zokushisa (indawo yokuncibilika/yokuqina kanye nokushisa okucashile) kanye nokuthembeka (ukujikeleza kokushisa) kunqunywe nge-differential scanning calorimetry (DSC, TA Instrument, Discovery DSC, Newcastle, USA) ngesilinganiso sokushisa/sokupholisa esingu-10 °C/min ku-40 °C. kanye no-90 °C ngokuhlanzwa kwe-nitrogen okuqhubekayo. Ukuhlaziywa kokulahlekelwa isisindo kwenziwa kusetshenziswa i-TGA analyzer (TA Instrument, Discovery TGA, New Castle, USA) ekugelezeni okuqhubekayo kwe-nitrogen okuqala ekushiseni okungu-40–600 °C, ngesilinganiso sokushisa esingu-10 °C/min.
Isithombe 3 sibonisa ama-spectra e-FTIR e-bulk SC kanye ne-SC efakwe i-microcapsulated (SATEOS1, SATEOS2, SATEOS3, SATEOS4, SATEOS5 kanye ne-SATEOS6). Iziqongo zokumuncwa ku-2910 cm-1 kanye no-2850 cm-1 kuzo zonke izibonelo (SA kanye ne-SA efakwe i-microcapsulated) zibangelwa ukudlidliza okunwebekayo kwamaqembu e-–CH3 kanye ne-–CH2, ngokulandelana okungu-10,50. Iziqongo ku-1705 cm-1 zihambisana nokudlidliza okunwebekayo kwesibopho se-C=O. Iziqongo ku-1470 cm-1 kanye no-1295 cm-1 zibangelwa ukudlidliza okugobile kweqembu elisebenzayo le-–OH, kuyilapho iziqongo ku-940 cm-1 kanye no-719 cm-1 zihambisana nokudlidliza okungaphakathi kwendiza kanye ne-yield. -plane deformation vibration, ngokulandelana - OH group. Iziqongo zokumunca ze-SA ku-2910, 2850, 1705, 1470, 1295, 940 kanye no-719 cm-1 nazo zabonwa kuzo zonke i-SA ezincane ezifakwe i-capsulated. Ngaphezu kwalokho, iqongo elisha elitholakale ku-1103 cm-1 elihambisana nokudlidliza okunwebekayo okungalingani kwebhendi ye-Si-O-Si labonwa ku-SA microcapsule. Imiphumela ye-FT-IR iyahambisana noYuan et al. 50 Balungiselele ngempumelelo i-SA encane efakwe i-capsulated ku-ammonia/ethanol ratio futhi bathola ukuthi akukho ukusebenzisana kwamakhemikhali okwenzeka phakathi kwe-SA ne-SiO2. Imiphumela yocwaningo lwamanje lwe-FT-IR ikhombisa ukuthi igobolondo le-SiO2 lifake i-SA (core) ngempumelelo ngenqubo yokujiya kanye ne-polymerization ye-TEOS ene-hydrolyzed. Ngokuqukethwe kwe-SA okuphansi, ukuqina okuphezulu kwebhendi ye-Si-O-Si kuphakeme (Isithombe 3b-d). Njengoba inani le-SA likhula lifinyelela ngaphezu kuka-15 g, ukuqina kwesiqongo kanye nokwanda kwebhendi ye-Si-O-Si kwehla kancane kancane, okubonisa ukwakheka kwengqimba encane ye-SiO2 ebusweni be-SA.
Ama-spectra e-FTIR ka-(a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 kanye (g) SATEOS6.
Amaphethini e-XRD e-bulk SA kanye ne-microencapsulated SA aboniswe ku-Figure 4. Iziqongo ze-XRD zitholakala ku-2θ = 6.50° (300), 10.94° (500), 15.46° (700), 20.26° \((\overline {5}ngokusho kwe-JCPDS No. 0381923, 02)\), 21.42° kuzo zonke izibonelo (311), 24.04° (602) kanye no-39.98° (913) zinikezwa i-SA. Ukuphambuka kanye nokuhlanganiswa ne-bulk CA ngenxa yezinto ezingaqinisekile njenge-surfactant (SLS), ezinye izinto ezisele kanye ne-microencapsulation ye-SiO250. Ngemva kokuba i-encapsulation yenzekile, ukuqina kweziqongo eziyinhloko (300), (500), (311), kanye ne-(602) kwehla kancane kancane uma kuqhathaniswa ne-bulk CA, okubonisa ukwehla kwe-crystallinity yesampula.
Amaphethini e-XRD ka-(a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 kanye (g) SATEOS6.
Ukuqina kwe-SATEOS1 kwehla kakhulu uma kuqhathaniswa nezinye izibonelo. Azikho ezinye iziqongo ezibonwe kuzo zonke izibonelo ezifakwe i-microcapsulated (Isithombe 4b–g), okuqinisekisa ukuthi ukumuncwa ngokomzimba kwe-SiO252 kunokuba kube ukusebenzisana kwamakhemikhali kwenzeka ebusweni be-SA. Ngaphezu kwalokho, kwaphethwa nangokuthi i-microcapsulation ye-SA ayizange iholele ekubonakaleni kwanoma yiziphi izakhiwo ezintsha. I-SiO2 ihlala ingashintshi ebusweni be-SA ngaphandle kokusabela kwamakhemikhali, futhi njengoba inani le-SA lehla, iziqongo ezikhona ziba sobala kakhulu (I-SATEOS1). Lo mphumela ubonisa ukuthi i-SiO2 ihlanganisa kakhulu ubuso be-SA. Isiqongo ku-(700) siyanyamalala ngokuphelele, kanti isiqongo ku-\((\overline{5}02)\) siba yi-hump ku-SATEOS 1 (Isithombe 4b), okuhlotshaniswa nokuncipha kwekristalinity kanye nokwanda kwe-amorphism. I-SiO2 ayiguquki ngokwemvelo, ngakho-ke iziqongo ezibonwa kusukela ku-2θ = 19° kuya ku-25° zinobugoxo nobubanzi53 (Isithombe 4b–g), okuqinisekisa ukuba khona kwe-SiO252 engaguquki. Ubukhulu obuphansi bokugqagqana kwe-SA encane bubangelwa umphumela we-nucleation wodonga lwangaphakathi lwe-silica kanye nokuziphatha okukhawulelayo kwe-crystallization49. Kukholelwa ukuthi ngokuqukethwe kwe-SA okuphansi, kwakheka igobolondo le-silica elijiyile ngenxa yokuba khona kwenani elikhulu le-TEOS, elinamathela kakhulu ebusweni bangaphandle be-SA. Kodwa-ke, njengoba inani le-SA landa, indawo engaphezulu yamaconsi e-SA esixazululweni se-emulsion iyanda futhi kudingeka i-TEOS eyengeziwe ukuze kufakwe kahle. Ngakho-ke, ngokuqukethwe kwe-SA okuphezulu, ukuphakama kwe-SiO2 ku-FT-IR kuyacindezelwa (Isithombe 3), futhi ukuqina kwe-diffraction peak eduze kuka-2θ = 19–25° ku-XRF (Isithombe 4) kuyancipha futhi nokwanda nakho kuyancipha. Akubonakali. Kodwa-ke, njengoba kungabonakala kuMfanekiso 4, ngokushesha nje lapho inani le-SA likhuphuka lisuka ku-5 g (SATEOS1) liye ku-50 g (SATEOS6), iziqongo ziba seduze kakhulu ne-bulk SA, futhi isiqongo ku-(700) sivela nazo zonke iziqongo eziveziwe. Lo mphumela uhambisana nemiphumela ye-FT-IR, lapho ukuqina kwesiqongo se-SiO2 SATEOS6 kwehla khona ku-1103 cm-1 (Umfanekiso 3g).
Izimo zamakhemikhali zezinto ezikhona ku-SA, SATEOS1 kanye ne-SATEOS6 ziboniswe kuZithombe 1 kanye no-2. Izibalo 5, 6, 7 kanye no-8 kanye neThebula 2. Ukuskena kokulinganisa kwe-bulk SA, i-SATEOS1 kanye ne-SATEOS6 kuboniswe kuMfanekiso 5 kanye nokuskena okuphezulu kwe-C 1s, O 1s kanye ne-Si 2p kuboniswe kuZithombe 5, 6, 7 kanye no-8 kanye neThebula 2. 6, 7 kanye no-8 ngokulandelana. Amanani wamandla okubopha atholwe yi-XPS afingqiwe kuThebula 2. Njengoba kungabonakala kuMfanekiso 5, iziqongo ezicacile ze-Si 2s kanye ne-Si 2p zabonwa ku-SATEOS1 kanye ne-SATEOS6, lapho kwenzeka khona i-microencapsulation yegobolondo le-SiO2. Abacwaningi bangaphambilini babike ukuthi i-Si 2s peak efanayo ku-155.1 eV54. Ukuba khona kwama-Si peaks ku-SATEOS1 (Umfanekiso 5b) kanye ne-SATEOS6 (Umfanekiso 5c) kuqinisekisa idatha ye-FT-IR (Umfanekiso 3) kanye ne-XRD (Umfanekiso 4).
Njengoba kuboniswe kuMfanekiso 6 a, ama-C1 e-bulk SA aneziqongo ezintathu ezihlukene ze-CC, i-caliphatic, kanye ne-O=C=O kumandla okubopha, okuyi-284.5 eV, 285.2 eV, kanye ne-289.5 eV, ngokulandelana. Iziqongo ze-C–C, i-caliphatic kanye ne-O=C=O nazo zabonwa ku-SATEOS1 (Umfanekiso 6b) kanye ne-SATEOS6 (Umfanekiso 6c) futhi zifingqiwe kuThebula 2. Ngaphezu kwalokhu, isiqongo se-C1s sihambisana nesiqongo se-Si-C esengeziwe ku-283 .1 eV (SATEOS1) kanye ne-283.5 eV (SATEOS6). Amandla ethu okubopha abonwayo e-C–C, i-caliphatic, i-O=C=O kanye ne-Si–C ahambisana kahle neminye imithombo55,56.
Ama-spectra e-XPS e-O 1 SA, i-SATEOS1 kanye ne-SATEOS6 aboniswe kuZithombe 7a–c, ngokulandelana. I-peak ye-O 1s ye-bulk SA isusiwe futhi ineziqongo ezimbili, okungukuthi i-C=O/C–O (531.9 eV) kanye ne-C–O–H (533.0 eV), kuyilapho i-O 1 ye-SATEOS1 kanye ne-SATEOS6 zihambisana. kuneziqongo ezintathu kuphela: i-C=O/C–O, i-C–O–H kanye ne-Si–OH55,57,58. Amandla okubopha e-O 1s ku-SATEOS1 kanye ne-SATEOS6 ashintsha kancane uma kuqhathaniswa ne-bulk SA, ehlotshaniswa noshintsho ku-fragment yamakhemikhali ngenxa yokuba khona kwe-SiO2 kanye ne-Si-OH ezintweni zegobolondo.
Ama-spectra e-Si 2p XPS e-SATEOS1 kanye ne-SATEOS6 aboniswe ku-Figure 8a kanye no-b, ngokulandelana. Ku-CA enkulu, i-Si 2p ayizange ibonwe ngenxa yokungabikho kwe-SiO2. I-Si 2p peak ihambelana ne-105.4 eV ye-SATEOS1 kanye ne-105.0 eV ye-SATEOS6, ehambelana ne-Si-O-Si, kuyilapho i-SATEOS1 peak ingu-103.5 eV kanti i-SATEOS6 peak ingu-103.3 eV, ehambelana ne-Si-OH55. Ukufakwa kwe-Si-O-Si kanye ne-Si-OH peak ku-SATEOS1 kanye ne-SATEOS6 kwembule impumelelo ye-microencapsulation ye-SiO2 ebusweni be-SA core.
Ukwakheka kwezinto ezifakwe ema-microcapsulation kubaluleke kakhulu, kuthinta ukuncibilika, ukuzinza, ukusabela kwamakhemikhali, ukugeleza kanye namandla59. Ngakho-ke, i-SEM yasetshenziswa ukuchaza ukwakheka kwe-bulk SA (100×) kanye ne-microcapsulated SA (500×), njengoba kuboniswe kuMfanekiso 9. Njengoba kungabonakala kuMfanekiso 9a, ibhulokhi le-SA linomumo we-elliptical. Usayizi wezinhlayiya udlula ama-micron angu-500. Kodwa-ke, uma inqubo ye-microcapsulation iqhubeka, ukwakheka kushintsha kakhulu, njengoba kuboniswe kuMfanekiso 9 b–g.
Izithombe ze-SEM zika-(a) SA (×100), (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 kanye (g) SATEOS6 ku-×500.
Kusampula ye-SATEOS1, kubonwa izinhlayiya ze-SA ezincane ezigoqwe nge-SiO2 ezine-spherical surface (Isithombe 9b), okungenzeka ukuthi kungenxa ye-hydrolysis kanye ne-condensation polymerization ye-TEOS ebusweni be-SA, okusheshisa ukusabalala okusheshayo kwama-molecule e-ethanol. Ngenxa yalokho, izinhlayiya ze-SiO2 ziyafakwa futhi i-agglomeration iyabonakala52,60. Leli gobolondo le-SiO2 linikeza amandla omshini ezinhlayiyeni ze-CA ezincane futhi livimbela nokuvuza kwe-CA encibilikisiwe emazingeni okushisa aphezulu10. Lo mphumela ubonisa ukuthi ama-microcapsule e-SA aqukethe i-SiO2 angasetshenziswa njengezinto zokugcina amandla ezingaba khona61. Njengoba kungabonakala kuMfanekiso 9b, isampula ye-SATEOS1 inokusabalalisa kwezinhlayiya okufanayo ngesendlalelo se-SiO2 esikhulu esimboza i-SA. Usayizi wezinhlayiya ze-SA encane (SATEOS1) cishe u-10–20 μm (Isithombe 9b), omncane kakhulu uma kuqhathaniswa ne-bulk SA ngenxa yokuqukethwe kwe-SA okuphansi. Ubukhulu besendlalelo se-microcapsule bubangelwa yi-hydrolysis kanye ne-condensation polymerization yesisombululo sangaphambi kokwelashwa. I-Agglomeration yenzeka ngemithamo ephansi ye-SA, okungukuthi kufika ku-15 g (Isithombe 9b-d), kodwa ngokushesha nje lapho umthamo ukhushuliwe, akukho agglomeration ebonwayo, kodwa izinhlayiya eziyindilinga ezichazwe ngokucacile ziyabonwa (Isithombe 9e-g) 62.
Ngaphezu kwalokho, uma inani le-surfactant ye-SLS lingaguquki, okuqukethwe kwe-SA (i-SATEOS1, i-SATEOS2 kanye ne-SATEOS3) nakho kuthinta ukusebenza kahle, ukuma kanye nokusatshalaliswa kosayizi wezinhlayiya. Ngakho-ke, i-SATEOS1 itholakale ikhombisa usayizi wezinhlayiya ezincane, ukusatshalaliswa okufanayo kanye nobuso obukhulu (Isithombe 9b), okwakubangelwa uhlobo lwe-SA oluthanda amanzi olukhuthaza i-nucleation yesibili ngaphansi kwe-surfactant engaguquki63. Kukholelwa ukuthi ngokwandisa okuqukethwe kwe-SA kusuka ku-5 kuya ku-15 g (i-SATEOS1, i-SATEOS2 kanye ne-SATEOS3) kanye nokusebenzisa inani elingaguquki le-surfactant, okungukuthi i-0.10 g SLS (Ithebula 1), umnikelo wezinhlayiya ngayinye ye-molecule ye-surfactant uzokwehla, ngaleyo ndlela kuncishiswe usayizi wezinhlayiya kanye nosayizi wezinhlayiya. Ukusatshalaliswa kwe-SATEOS2 (Isithombe 9c) kanye ne-SATEOS3 (Isithombe 9d) kuhlukile ekusatshalalisweni kwe-SATEOS 1 (Isithombe 9b).
Uma kuqhathaniswa ne-SATEOS1 (Umfanekiso 9b), i-SATEOS2 ibonise isimo esiqinile se-SA encane ehlanganisiwe kanye nosayizi wezinhlayiya wanda (Umfanekiso 9c). Lokhu kungenxa ye-agglomeration 49, okunciphisa izinga lokujiya (Umfanekiso 2b). Njengoba inani le-SC landa ngokwanda kwe-SLS, ama-microcapsule abonakala ngokucacile, njengoba kuboniswe ku-Fig. ukuthi ukuhlangana kwenzeka kanjani. Ngaphezu kwalokho, Izibalo 9e–g zibonisa ukuthi zonke izinhlayiya zicacile ngesimo nangosayizi. Kuye kwaqashelwa ukuthi lapho kukhona inani elikhulu le-SA, kungatholakala inani elifanele lama-oligomers e-silica, okubangela ukujiya okufanele kanye nokugoqwa kwamangqamuzana futhi ngaleyo ndlela kwakhiwe ama-microcapsules achazwe kahle49. Kusukela emiphumeleni ye-SEM, kusobala ukuthi i-SATEOS6 yakha ama-microcapsules ahambisanayo uma kuqhathaniswa nenani elincane le-SA.
Imiphumela ye-energy dispersive X-ray spectroscopy (EDS) ye-bulk SA kanye ne-microcapsule SA ivezwa kuThebula 3. Njengoba kungabonakala kuleli thebula, okuqukethwe kwe-Si kwehla kancane kancane kusuka ku-SATEOS1 (12.34%) kuya ku-SATEOS6 (2.68%). Ukwanda ku-SA. Ngakho-ke, singasho ukuthi ukwanda kwenani le-SA kuholela ekunciphiseni kokufakwa kwe-SiO2 ebusweni be-SA. Azikho izindinganiso ezihambisanayo zokuqukethwe kwe-C kanye ne-O kuThebula 3 ngenxa yokuhlaziywa kwesilinganiso se-EDS51. Okuqukethwe kwe-Si kwe-microencapsulated SA kuhlotshaniswe nemiphumela ye-FT-IR, XRD kanye ne-XPS.
Ukuziphatha kokuncibilika nokuqina kwe-bulk SA kanye ne-microencapsulated SA enegobolondo le-SiO2 kuboniswe kuZithombe 1 no-2. Kuboniswe kuZithombe 10 no-11 ngokulandelana, kanti idatha yokushisa iboniswe kuThebula 4. Amazinga okushisa okuncibilika nokuqina kwe-microencapsulated SA atholakale ehlukene. Njengoba inani le-SA landa, amazinga okushisa okuncibilika nokuqina ayanda futhi asondela kumanani e-bulk SA. Ngemuva kwe-SA microencapsulation, udonga lwe-silica lwandisa izinga lokushisa lokukristala, futhi udonga lwalo lusebenza njengesisekelo sokukhuthaza ukungafani. Ngakho-ke, njengoba inani le-SA landa, amazinga okushisa okuncibilika (Isithombe 10) kanye nokuqina (Isithombe 11) nawo ayanda kancane kancane49,51,64. Phakathi kwazo zonke izibonelo ze-SA ezincaneencapsulated, i-SATEOS6 ibonise amazinga okushisa aphezulu okuncibilika nokuqina, kulandelwa yi-SATEOS5, SATEOS4, SATEOS3, SATEOS2, kanye ne-SATEOS1.
I-SATEOS1 ikhombisa iphuzu lokuncibilika eliphansi kakhulu (68.97 °C) kanye nezinga lokushisa lokuqina (60.60 °C), okubangelwa ubukhulu bezinhlayiya ezincane lapho ukunyakaza kwezinhlayiya ze-SA ngaphakathi kwama-microcapsule kuncane kakhulu futhi igobolondo le-SiO2 lakha ungqimba olujiyile ngakho-ke i-Core Material ikhawulela ukwelula nokunyakaza49. Lo mbono uhlobene nemiphumela ye-SEM, lapho i-SATEOS1 ibonise khona ubukhulu bezinhlayiya ezincane (Umfanekiso 9b), okubangelwa iqiniso lokuthi ama-molecule e-SA avaleleke endaweni encane kakhulu yama-microcapsule. Umehluko emazingeni okushisa okuncibilika nokuqina kwesisindo esiyinhloko, kanye nawo wonke ama-microcapsule e-SA anamagobolondo e-SiO2, usebangeni eliphakathi kuka-6.10–8.37 °C. Lo mphumela ubonisa ukuthi i-SA efakwe ama-microcapsule ingasetshenziswa njengezinto zokugcina amandla ezingaba khona ngenxa yokushisa okuhle kwegobolondo le-SiO2 65.
Njengoba kungabonakala kuThebula 4, i-SATEOS6 ine-enthalpy ephezulu kakhulu phakathi kwazo zonke i-SC ezifakwe i-microcapsulated (Umfanekiso 9g) ngenxa yokufakwa kwe-SEM okufanele. Izinga lokupakisha le-SA lingabalwa kusetshenziswa i-equation (1). (1) Ngokuqhathanisa idatha yokushisa efihliwe ye-microcapsulated SA49.
Inani le-R limelela izinga lokuvaleka (%) le-SC evaleka kancane, i-ΔHMEPCM, m imelela ukushisa okucashile kokuhlanganiswa kwe-SC evaleka kancane, kanti i-ΔHPCM, m imelela ukushisa okucashile kokuhlanganiswa kwe-SC. Ngaphezu kwalokho, ukusebenza kahle kokupakisha (%) kubalwa njengenye ipharamitha yobuchwepheshe ebalulekile, njengoba kuboniswe ku-Equation (1). (2)49.
Inani le-E limelela ukusebenza kahle kwe-encapsulation (%) ye-microencapsulated CA, i-ΔHMEPCM,s imelela ukushisa okucashile kokwelashwa kwe-microencapsulated CA, kanti i-ΔHPCM,s imelela ukushisa okucashile kokwelashwa kwe-CA.
Njengoba kuboniswe kuThebula 4, izinga lokupakisha nokusebenza kahle kwe-SATEOS1 lingu-71.89% kanye no-67.68%, ngokulandelana, kanti izinga lokupakisha nokusebenza kahle kwe-SATEOS6 lingu-90.86% kanye no-86.68%, ngokulandelana (Ithebula 4). Isampula ye-SATEOS6 ibonisa i-coefficient ephezulu kakhulu ye-encapsulation kanye nokusebenza kahle phakathi kwawo wonke ama-SA afakwe i-microcapsulated, okubonisa amandla ayo aphezulu okushisa. Ngakho-ke, ukuguquka kusuka kokuqinile kuya kokuketshezi kudinga amandla amaningi. Ngaphezu kwalokho, umehluko emazingeni okushisa okuncibilika kanye nokuqina kwawo wonke ama-microcapsule e-SA kanye ne-bulk SA ngesikhathi senqubo yokupholisa ubonisa ukuthi igobolondo le-silica livalelwe endaweni ngesikhathi sokwenziwa kwe-microcapsule. Ngakho-ke, imiphumela ikhombisa ukuthi njengoba inani le-SC landa, izinga le-encapsulation kanye nokusebenza kahle kukhula kancane kancane (Ithebula 4).
Ama-TGA curves e-bulk SA kanye ne-microcapsule SA enegobolondo le-SiO2 (i-SATEOS1, i-SATEOS3 kanye ne-SATEOS6) aboniswe ku-Figure 12. Izakhiwo zokuzinza kokushisa kwe-bulk SA (i-SATEOS1, i-SATEOS3 kanye ne-SATEOS6) ziqhathaniswa namasampula afakwe i-microcapsulated. Kusobala kusuka ku-TGA curve ukuthi ukwehla kwesisindo kwe-bulk SA kanye ne-microcapsulated SA kukhombisa ukwehla okubushelelezi nokuncane kakhulu kusuka ku-40°C kuya ku-190°C. Kuleli zinga lokushisa, i-bulk SC ayiboli ngokushisa, kuyilapho i-microcapsulated SC ikhipha amanzi afakwe i-adsor ngisho nangemva kokoma ku-45 °C amahora angama-24. Lokhu kwaholela ekunciphiseni isisindo okuncane,49 kodwa ngale kwaleli zinga lokushisa izinto zaqala ukonakala. Kokuqukethwe kwe-SA okuphansi (okungukuthi i-SATEOS1), okuqukethwe kwamanzi afakwe i-adsor kuphakeme ngakho-ke ukulahleka kwesisindo kufika ku-190 °C kuphakeme (okufakwe ku-Fig. 12). Lapho nje izinga lokushisa likhuphuka ngaphezu kuka-190 °C, isampula iqala ukulahlekelwa isisindo ngenxa yezinqubo zokubola. I-Bulk SA iqala ukubola ku-190°C futhi u-4% kuphela ohlala ku-260°C, kanti i-SATEOS1, i-SATEOS3 kanye ne-SATEOS6 zigcina u-50%, 20% kanye no-12% kuleli zinga lokushisa, ngokulandelana. Ngemva kuka-300 °C, ukulahlekelwa isisindo kwe-bulk SA kwaba cishe ngu-97.60%, kuyilapho ukulahlekelwa isisindo kwe-SATEOS1, i-SATEOS3, kanye ne-SATEOS6 kwaba cishe ngu-54.20%, 82.40%, kanye no-90.30%, ngokulandelana. Ngokwanda kokuqukethwe kwe-SA, okuqukethwe kwe-SiO2 kwehla (Ithebula 3), futhi ukuncishiswa kwegobolondo kubonakala ku-SEM (Isithombe 9). Ngakho-ke, ukwehla kwesisindo se-SA encane efakwe emaphaketheni kuphansi uma kuqhathaniswa ne-SA enkulu, okuchazwa yizakhiwo ezinhle zegobolondo le-SiO2, elikhuthaza ukwakheka kwengqimba ye-silicate-carbonaceous ye-carbonaceous ebusweni be-SA, ngaleyo ndlela lihlukanise umongo we-SA futhi linciphise ukukhishwa kwemikhiqizo eguquguqukayo ephumayo10. Lolu ngqimba lwe-char lwakha isithiyo esivikelayo ngokomzimba ngesikhathi sokubola kokushisa, lukhawulela ukuguquka kwama-molecule avuthayo abe yi-gas phase66,67. Ngaphezu kwalokhu, singabona nemiphumela ebalulekile yokulahlekelwa isisindo: I-SATEOS1 ikhombisa amanani aphansi uma kuqhathaniswa ne-SATEOS3, i-SATEOS6 kanye ne-SA. Lokhu kungenxa yokuthi inani le-SA ku-SATEOS1 lingaphansi kune-SATEOS3 kanye ne-SATEOS6, lapho igobolondo le-SiO2 lakha khona ungqimba olujiyile. Ngokuphambene nalokho, ukulahleka kwesisindo okuphelele kwe-SA enkulu kufinyelela ku-99.50% ku-415 °C. Kodwa-ke, i-SATEOS1, i-SATEOS3, kanye ne-SATEOS6 zibonise ukwehla kwesisindo okungu-62.50%, 85.50%, kanye no-93.76%, ngokulandelana, ku-415 °C. Lo mphumela ubonisa ukuthi ukungezwa kwe-TEOS kuthuthukisa ukuwohloka kwe-SA ngokwenza ungqimba lwe-SiO2 ebusweni be-SA. Lezi zingqimba zingakha isithiyo esivikelayo ngokomzimba, ngakho-ke ukuthuthukiswa kokuzinza kokushisa kwe-CA encane ehlanganisiwe kungabonakala.
Imiphumela yokuthembeka kokushisa kwe-bulk SA kanye nesampula engcono kakhulu ye-microencapsulated (okungukuthi i-SATEOS 6) ngemva kwemijikelezo yokushisa nokupholisa engu-30 ye-DSC51,52 iboniswe ku-Figure 13. Kungabonakala ukuthi i-bulk SA (Isithombe 13a) ayibonisi mehluko ekushiseni okuncibilikayo. ukuqina kanye nenani le-enthalpy, kuyilapho i-SATEOS6 (Isithombe 13b) ingabonisi mehluko ekushiseni kanye nenani le-enthalpy ngisho nangemva komjikelezo wokushisa wama-30. kanye nenqubo yokupholisa. I-Bulk SA ibonise iphuzu lokuncibilika elingu-72.10 °C, izinga lokushisa lokuqina elingu-64.69 °C, kanye nokushisa kokuhlanganiswa kanye nokuqina ngemva komjikelezo wokuqala kwakuyi-201.0 J/g kanye ne-194.10 J/g, ngokulandelana. Ngemva komjikelezo wama-30, iphuzu lokuncibilika kwala manani lehle laya ku-71.24 °C, izinga lokushisa lokuqina lehla laya ku-63.53 °C, kanti inani le-enthalpy lehle ngo-10%. Izinguquko emazingeni okushisa okuncibilika nokuqina, kanye nokwehla kwamanani e-enthalpy, kubonisa ukuthi i-bulk CA ayithembekile ezinhlelweni ezingezona eze-microencapsulation. Kodwa-ke, ngemva kokuba kwenzeke i-microencapsulation efanele (SATEOS6), amazinga okushisa okuncibilika nokuqina kanye namanani e-enthalpy awashintshi (Isithombe 13b). Uma isifakwe i-microcapsulated ngamagobolondo e-SiO2, i-SA ingasetshenziswa njengento yokushintsha isigaba ekusetshenzisweni kokushisa, ikakhulukazi ekwakheni, ngenxa yokushisa kwayo okuncibilika nokuqina kanye ne-enthalpy ezinzile.
Ama-curve e-DSC atholwe kumasampula e-SA (a) kanye ne-SATEOS6 (b) emijikelezweni yoku-1 neyama-30 yokushisa nokupholisa.
Kulolu cwaningo, kwenziwa uphenyo oluhlelekile lwe-microencapsulation kusetshenziswa i-SA njengento eyinhloko kanye ne-SiO2 njengento yegobolondo. I-TEOS isetshenziswa njengesandulela ukwakha ungqimba lokusekela le-SiO2 kanye nongqimba oluvikelayo ebusweni be-SA. Ngemva kokuhlanganiswa ngempumelelo kwe-SA ene-microencapsulated, imiphumela ye-FT-IR, i-XRD, i-XPS, i-SEM kanye ne-EDS ibonise ukuba khona kwe-SiO2. Ukuhlaziywa kwe-SEM kukhombisa ukuthi isampula ye-SATEOS6 ibonisa izinhlayiya eziyindilinga ezichazwe kahle ezizungezwe amagobolondo e-SiO2 ebusweni be-SA. Kodwa-ke, i-MEPCM enokuqukethwe okuphansi kwe-SA ibonisa ukuhlangana, okunciphisa ukusebenza kwe-PCM. Ukuhlaziywa kwe-XPS kubonise ukuba khona kwe-Si-O-Si kanye ne-Si-OH kumasampula e-microcapsule, okwembule ukumuncwa kwe-SiO2 ebusweni be-SA. Ngokusho kokuhlaziywa kokusebenza kokushisa, i-SATEOS6 ikhombisa ikhono lokugcina ukushisa elithembisayo kakhulu, ngamazinga okushisa okuncibilika nokuqina angu-70.37°C kanye no-64.27°C, ngokulandelana, kanye nokushisa okucashile kokuncibilika nokuqina okungu-182.53 J/g kanye no-160.12 J/g. G. ngokulandelana. Ukusebenza kahle kokupakisha kwe-SATEOS6 kungu-86.68%. Ukuhlaziywa komjikelezo wokushisa we-TGA kanye ne-DSC kuqinisekisile ukuthi i-SATEOS6 isenokuqina okuhle kokushisa kanye nokuthembeka ngisho nangemva kwezinqubo zokushisa nokupholisa ezingama-30.
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Isikhathi sokuthunyelwe: Meyi-21-2024