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Aside Stearic (SA) ikoreshwa nk'ibikoresho byo guhindura icyiciro (PCM) mu bikoresho byo kubika ingufu. Muri ubu bushakashatsi, uburyo bwa sol-gel bwakoreshejwe mu gufunga isafuriya ya SiO2. Ingano zitandukanye za SA (5, 10, 15, 20, 30, na 50 g) zashyizwe muri 10 mL ya tetraethyl orthosilicate (TEOS). Ibikoresho byo guhindura icyiciro bya microencapsulated (MEPCM) byagizwe na Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), na scanning electron microscopy (SEM). Ibisubizo by'imiterere byagaragaje ko SA yashyizwe muri SiO2 neza. Isesengura rya Thermogravimetric (TGA) ryagaragaje ko MEPCM ifite ubushyuhe bwiza kurusha CA. Hakoreshejwe differential scanning calorimetry (DSC), byagaragaye ko agaciro ka enthalpy ka MEPCM katigeze gahinduka na nyuma y'amasaha 30 yo gushyushya no gukonjesha. Mu bipimo byose bya microcapsule, garama 50 za SA zirimo MEPCM zari zifite ubushyuhe bwinshi bwo gushonga no gukomera, aribyo 182.53 J/g na 160.12 J/g. Agaciro k'ubushyuhe bwa paki kabazwe hakoreshejwe amakuru y'ubushyuhe kandi imikorere myiza cyane yabonetse kuri icyo gipimo kimwe cyari 86.68%.
Hafi 58% by'ingufu zikoreshwa mu nganda z'ubwubatsi zikoreshwa mu gushyushya no gukonjesha inyubako1. Kubwibyo, ikintu cyingenzi cyane ni ugushyiraho uburyo bwiza bw'ingufu zitabwaho mu kwanduza ibidukikije2. Ikoranabuhanga ry'ubushyuhe butica rikoresha ibikoresho bihindura imiterere y'imyanya (PCM) rishobora kubika ingufu nyinshi ku bushyuhe buke3,4,5,6 kandi rishobora gukoreshwa cyane mu bintu nko kohereza ubushyuhe, kubika ingufu z'izuba, ikirere n'ikirere gikonjesha7,8,9. PCM ifata ingufu z'ubushyuhe zituruka hanze y'inyubako ku manywa kandi igasohora ingufu nijoro10. Kubwibyo, ibikoresho bihindura imiterere y'imyanya birasabwa nk'ibikoresho byo kubika ingufu z'ubushyuhe. Byongeye kandi, hari ubwoko butandukanye bwa PCM nka solid-solid, solid-liquid, liquid-gaz na solid-gaz11. Muri byo, ibikoresho bikundwa cyane kandi bikunze gukoreshwa mu guhindura imiterere y'imyanya ni ibikoresho bihindura imiterere y'imyanya ...
PCM ifite uburyo butandukanye bwo kuyikoresha bitewe n’imiterere yayo: izishongesha ku bushyuhe buri munsi ya 15°C zishobora gukoreshwa muri sisitemu zikonjesha kugira ngo zigumane ubushyuhe bukonje, naho izishongesha ku bushyuhe buri hejuru ya 90°C zishobora gukoreshwa muri sisitemu zishyushya kugira ngo hirindwe inkongi12. Bitewe n’uburyo ikoreshwa n’aho ishongesha, ibikoresho bitandukanye byo guhindura icyiciro byakozwe mu binyabutabire bitandukanye by’umwimerere n’ibitari umwimerere13,14,15. Parafini ni yo ikoreshwa cyane mu guhindura icyiciro ifite ubushyuhe bwinshi buhishe, idashonga, umutekano kandi ishobora gushonga ku rugero runini16,17,18,19,20,21.
Ariko, bitewe n’ubushyuhe buke bw’ibikoresho bihindura icyiciro, bigomba gushyirwa mu gipfunyika (urwego rwo hanze) kugira ngo hirindwe ko ibikoresho by’ibanze biva mu nzira yo guhindura icyiciro22. Byongeye kandi, amakosa mu mikorere cyangwa igitutu cyo hanze bishobora kwangiza urwego rwo hanze (igipfunyika), kandi ibikoresho bihindura icyiciro byashongeshejwe bishobora gukorana n’ibikoresho by’ubwubatsi, bigatera ingese y’ibyuma byashongeshejwe, bityo bikagabanya ubushobozi bwo gukora inyubako23. Kubwibyo, ni ngombwa gukora ibikoresho bihindura icyiciro byashongeshejwe bifite ibikoresho bihagije by’igipfunyika, bishobora gukemura ibibazo byavuzwe haruguru24.
Gushyiramo ibikoresho bihindura imiterere y’imyanya bishobora kongera uburyo bwo kohereza ubushyuhe no kugabanya ingaruka ku bidukikije, no kugenzura impinduka z’ingano y’amazi. Uburyo butandukanye bwakozwe bwo gushyiramo ibikoresho bihindura imiterere y’imyanya y’amazi mu buryo bwa PCM, ari bwo polymerization hagati y’ibice 25,26,27,28, polymerization isanzwe 29,30,31,32, coacervation 33,34,35 na sol-gel processes 36,37,38,39. Resin ya formaldehyde ishobora gukoreshwa muri microencapsulation 40,41,42,43. Resin ya Melamine-formaldehyde na urea-formaldehyde ikoreshwa nk'ibikoresho by'ibumba, akenshi bisohora formaldehyde irimo uburozi mu gihe cyo gukora. Kubwibyo, ibi bikoresho birabujijwe gukoreshwa mu gupakira. Ariko, ibikoresho bihindura imiterere y’imyanya y’amazi bitagira ingaruka ku bidukikije kugira ngo bibe byakwiyongera bishobora gukorwa hakoreshejwe nanocapsules zivanze zishingiye kuri aside fatty na lignin 44.
Zhang n'abandi 45 n'abandi bakoranye aside laurike iva muri tetraethyl orthosilicate maze bemeza ko uko ingano ya methyltriethoxysilane na tetraethyl orthosilicate yiyongera, ubushyuhe butihishe buragabanuka kandi ubwiyongere bw'amazi ku buso bwiyongera. Aside Laurike ishobora kuba igikoresho cy'ingenzi kandi gifatika cya fibre za kapok46. Byongeye kandi, Latibari n'abandi 47 bakoranye PCM zishingiye kuri aside stearic bakoresheje TiO2 nk'ibikoresho by'igishishwa. Zhu n'abandi bateguye n-octadecane na silicone nanocapsules nk'ibikoresho bishobora gukoreshwa 48. Dukurikije isuzuma ry'inyandiko, biragoye gusobanukirwa ingano isabwa yo gukora ibikoresho bihindura imiterere y'impinduka mu buryo bufatika kandi buhamye.
Kubwibyo, nk'uko abanditsi babizi, ingano y'ibikoresho bihindura icyiciro bikoreshwa mu gupima icyiciro ni ikintu cyingenzi mu gukora ibikoresho bihindura icyiciro bito kandi bihamye. Gukoresha ingano itandukanye y'ibikoresho bihindura icyiciro bizadufasha gusobanura imiterere itandukanye n'uburyo ibintu bihindura icyiciro bito bito bito bihinduka. Aside stearike (aside irike) ni ikintu kitangiza ibidukikije, gifite akamaro mu buvuzi kandi gihendutse gishobora gukoreshwa mu kubika ingufu z'ubushyuhe kuko gifite agaciro ka enthalpy kanini (~200 J/g) kandi gishobora kwihanganira ubushyuhe bugera kuri 72 °C. Byongeye kandi, SiO2 ntishobora gushya, itanga imbaraga nyinshi za mekanike, ikora neza mu bushyuhe kandi irwanya neza ibikoresho by'ibanze, kandi ikora nk'ibikoresho bitera ubwoba mu bwubatsi. Iyo sima ivanze n'amazi, PCM zidafite icyiciro kinini zishobora kwangirika bitewe no kwangirika kwa mekanike n'ubushyuhe bwinshi (ubushyuhe bw'amazi) bikomoka mu nyubako nini za beto. Kubwibyo, gukoresha CA ifite icyiciro gito hamwe n'igitambaro cya SiO2 bishobora gukemura iki kibazo. Kubwibyo, intego y'ubu bushakashatsi kwari ukwiga imikorere n'ubushobozi bwa PCMs zakozwe na sol-gel mu bikorwa by'ubwubatsi. Muri ubu bushakashatsi, twize ku buryo burambuye ingano zitandukanye za SA (nk'ibikoresho by'ibanze) za 5, 10, 15, 20, 30 na 50 g zifungishijwe mu bishishwa bya SiO2. Ingano idahinduka ya tetraethylorthosilicate (TEOS) mu gipimo cya 10 ml yakoreshejwe nk'igisubizo cy'ibanze cyo gukora bishishwa bya SiO2.
Acide stearic yo mu rwego rwo gukora (SA, C18H36O2, aho gushonga: 72°C) nk'ibikoresho by'ingenzi byaguzwe muri Daejung Chemical & Metals Co., Ltd., Gyeonggi-do, Koreya y'Epfo. Tetraethylorthosilicate (TEOS, C8H20O4Si) nk'umuti w'ibanze yaguzwe muri Acros Organics, Geel, mu Bubiligi. Byongeye kandi, ethanol (EA, C2H5OH) na sodium lauryl sulfate (SLS, C12H25NaO4S) byaguzwe muri Daejung Chemical & Metals Co., Ltd, Gyeonggi-do, Koreya y'Epfo, kandi byakoreshejwe nk'ibishongesha n'ibisuguti, uko bikurikirana. Amazi yakuwemo amavuta nayo akoreshwa nk'ibishongesha.
Ingano zitandukanye za SA zavanzwe n'ibipimo bitandukanye bya sodium lauryl sulfate (SLS) muri 100 mL y'amazi yaciwe hakoreshejwe icyuma gikurura magnetic stirrer kuri 800 rpm na 75 °C mu gihe cy'isaha 1 (Imbonerahamwe ya 1). SA emulsions zagabanijwemo amatsinda abiri: (1) 5, 10 na 15 g bya SA byavanzwe na 0.10 g bya SLS muri 100 ml y'amazi yaciwe (SATEOS1, SATEOS2 na SATEOS3), (2) 20, 30 na 50 g bya SA byavanzwe na 0.15, 0.20 na 0.25 g bya SLS byavanzwe na 100 ml y'amazi yaciwe (SATEOS4, SATEOS5 na SATEOS6). 0.10 g ya SLS yakoreshejwe na 5, 10 na 15 g bya SA kugira ngo hakorwe emulsions. Nyuma yaho, hatanzwe igitekerezo cyo kongera umubare wa SLS kuri SATEOS4, SATEOS5 na SATEOS6. Imbonerahamwe ya 1 igaragaza ikigereranyo cya CA na SLS cyakoreshejwe kugira ngo haboneke ibisubizo bya emulsion bihamye.
Shyira TEOS 10 ml, ethanol 10 ml (EA) na 20 ml z'amazi yaciwe mu gikombe cya mililitiro 100. Kugira ngo wige uburyo bwo gufunga neza ibipimo bitandukanye by'ibice bya SA na SiO2, handitswe coefficient y'ibipimo byose. Uruvange rwavanzwe hakoreshejwe icyuma gikurura amashanyarazi kuri 400 rpm na 60 °C mu gihe cy'isaha 1. Hanyuma umuti wa precursor wongewemo mu buryo butonyanga kuri emulsion ya SA yateguwe, uvangwa cyane kuri 800 rpm na 75 °C mu gihe cy'amasaha 2, hanyuma uyungururwa kugira ngo haboneke ifu yera. Ifu yera yogejwe n'amazi yaciwe kugira ngo ikuremo SA yasigaye hanyuma yumishwa mu itanura ridafite umwuka kuri 45 °C mu gihe cy'amasaha 24. Kubera iyo mpamvu, habonetse SC yaciwe mu buryo buto ifite agace ka SiO2. Uburyo bwose bwo gukora no gutegura SA yaciwe mu buryo buto bugaragara ku Ishusho ya 1.
Udupira duto twa SA dufite igishishwa cya SiO2 twateguwe hakoreshejwe uburyo bwa sol-gel, kandi uburyo bwo gufunga bugaragara ku Ishusho ya 2. Intambwe ya mbere irimo gutegura emulsion ya SA mu gisubizo cy'amazi hamwe na SLS nk'umusemburo. Muri iki gihe, impera y'amazi ya molekile ya SA ihuzwa na SLS, naho impera y'amazi ihuzwa na molekile z'amazi, bigatuma emulsion ihoraho. Bityo, ibice bya SLS birindwa kandi bigatwikira ubuso bw'agatonyanga ka SA. Ku rundi ruhande, hydrolysis y'ibisubizo bya TEOS ibaho buhoro buhoro binyuze muri molekile z'amazi, bigatuma TEOS ihuzwa na hydrolyze imbere ya ethanol (Ishusho ya 2a) 49,50,51. TEOS ihuzwa na hydrolyze ikora reaction y'amazi, aho TEOS ihuzwa na n-hydrolyze ikora amatsinda ya silica (Ishusho ya 2b). Amatsinda ya silica yahujwe na SA52 imbere ya SLS (Ishusho ya 2c), byitwa inzira ya microencapsulation.
Ishusho y'icyitegererezo cy'ifungwa rya CA hamwe n'agasanduku ka SiO2 (a) hydrolysis ya TEOS (b) guhumeka kwa hydrolyzate na (c) gufunga CA hamwe n'agasanduku ka SiO2.
Isesengura rya chimique rya bulk SA na microencapsulated SA ryakozwe hakoreshejwe spectrometer ya Fourier transform infrared (FT-IR, Perkin Elmer UATR Two, USA) kandi spectra zafashwe mu ntera iri hagati ya cm 500 na cm 4000.
Igipimo cya X-ray diffractometer (XRD, D/MAX-2500, Rigaku, mu Buyapani) cyakoreshejwe mu gusesengura ibice bya SA byinshi n'ibikoresho bya microcapsule. Gusuzuma imiterere ya X-ray byakozwe mu ntera ya 2θ = 5°–95° hamwe n'umuvuduko wo gupima wa 4°/min, hakoreshejwe imirasire ya Cu-Kα (λ = 1.541 Å), imiterere y'imikorere ya 25 kV na 100 mA, mu buryo bwo gupima buhoraho. Amashusho ya X-ray yakozwe mu ntera ya 2θ = 5–50°, kubera ko nta gasongero kabonetse nyuma ya 50° mu ngero zose.
Isuzuma rya X-ray photoelectron spectroscopy (XPS, Scienta Omicron R3000, USA) ryakozwe hakoreshejwe Al Kα (1486.6 eV) nk'isoko ya X-ray kugira ngo humve imiterere ya chimique ya bulk SA ndetse n'ibintu biri mu bikoresho byo gufunga. Isuzuma rya XPS ryakusanyijwe ryashyizwe ku gasongero ka C 1s hakoreshejwe karuboni idasanzwe (ingufu zo gufatanya 284.6 eV). Nyuma yo gukosora inyuma hakoreshejwe uburyo bwa Shirley, imisozi miremire ya buri kintu yakuweho maze ishyirwa ku mikorere ya Gaussian/Lorentzian hakoreshejwe porogaramu ya CASA XPS.
Imiterere ya SC nini na SC ifite udupira duto twasuzumwe hakoreshejwe mikoroskopi ya electron scanning (SEM, MIRA3, TESCAN, Brno, Repubulika ya Tchèque) ifite spectroscopy ya X-ray ikwirakwiza ingufu (EDS) kuri kV 15. Mbere yo gufata amashusho ya SEM, ingero zasizwe na platinum (Pt) kugira ngo hirindwe ingaruka zo gusharija.
Imiterere y'ubushyuhe (aho bushongeshwa/bukomera n'ubushyuhe butihishe) hamwe n'ubwizerwe (guhindagurika kw'ubushyuhe) byagenwe hakoreshejwe calorimetry inyuranye yo gupima (DSC, TA Instrument, Discovery DSC, Newcastle, USA) ku gipimo cyo gushyushya/gukonjesha cya 10 °C/min kuri 40 °C. na 90 °C hamwe no gusukura azote mu buryo buhoraho. Isesengura ryo kugabanya ibiro ryakozwe hakoreshejwe isesengura rya TGA (TA Instrument, Discovery TGA, New Castle, USA) mu rujya n'uruza rwa azote rukomeza gutangirira ku bushyuhe bwa 40–600 °C, hamwe n'igipimo cyo gushyushya cya 10 °C/min.
Ishusho ya 3 igaragaza spectra ya FTIR ya SC nini ndetse na SC ifite uduce duto (SATEOS1, SATEOS2, SATEOS3, SATEOS4, SATEOS5 na SATEOS6). Imisozo yo kwinjiza kuri 2910 cm-1 na 2850 cm-1 mu bipimo byose (SA kimwe na SA ifite uduce duto) iterwa n'imitingito yo kuzenguruka y'amatsinda ya –CH3 na –CH2, uko bikurikirana10,50. Imisozo kuri 1705 cm-1 ihuye no kuzenguruka kw'umugozi wa C=O. Imisozo kuri 1470 cm-1 na 1295 cm-1 iterwa no kuzenguruka kw'itsinda ry'imikorere ya –OH, mu gihe imisozo kuri 940 cm-1 na 719 cm-1 ijyanye no kuzenguruka kw'itsinda ry'imikorere ya –OH, uko bikurikirana – itsinda rya OH. Impinga z’umunyu wa SA kuri 2910, 2850, 1705, 1470, 1295, 940 na 719 cm-1 nazo zagaragaye muri SA yose ifite microcapsulated. Byongeye kandi, impera nshya yavumbuwe kuri 1103 cm-1 ijyanye no kuzenguruka kwa Si-O-Si band yagaragaye muri microcapsule ya SA. Ibisubizo bya FT-IR bihuye na Yuan et al. 50 Bateguye neza microcapsulated SA muri amoniya/ethanol ratio kandi basanze nta mikoranire ya shimi yabaye hagati ya SA na SiO2. Ibisubizo by’ubushakashatsi bwa FT-IR bwerekana ko igishishwa cya SiO2 cyafashe neza SA (core) binyuze mu nzira yo gushonga no gupolima TEOS ya hydrolyzed. Iyo SA iri hasi, imbaraga z’umunyu wa Si-O-Si band ziba nyinshi (Ishusho ya 3b-d). Uko ingano ya SA yiyongera ikagera kuri garama zirenga 15, ubukana bw'agace k'umurambararo n'ubwiyongere bw'umugozi wa Si-O-Si bugenda bugabanuka buhoro buhoro, bigaragaza ko habayeho urwego rworoshye rwa SiO2 ku buso bwa SA.
Ishusho ya FTIR ya (a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 na (g) SATEOS6.
Imiterere ya XRD ya bulk SA na microcapsulated SA igaragara ku Ishusho ya 4. Impinga za XRD ziri kuri 2θ = 6.50° (300), 10.94° (500), 15.46° (700), 20.26° \((\overline {5}nk'uko bivugwa na JCPDS No. 0381923, 02)\), 21.42° mu bipimo byose (311), 24.04° (602) na 39.98° (913) bishyirwa kuri SA. Guhindagurika no guhuza CA bulk bitewe n'ibintu bitazwi nka surfactant (SLS), ibindi bintu bisigaye na microcapsulation ya SiO250. Nyuma yo gufunga, ubukana bw'impinga nkuru (300), (500), (311), na (602) bugenda bugabanuka ugereranije na CA bulk, bigaragaza igabanuka ry'ubucucike bw'icyitegererezo.
Imiterere ya XRD ya (a) SA, (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 na (g) SATEOS6.
Ubukana bwa SATEOS1 buragabanuka cyane ugereranije n'izindi ngero. Nta zindi nsongero zagaragaye mu ngero zose za microcapsulated (Ishusho ya 4b–g), yemeza ko kwinjizwa kwa SiO252 mu mubiri aho kuba imikorere ya shimi biba ku buso bwa SA. Byongeye kandi, byaje gufatwa umwanzuro ko microcapsulation ya SA itatumye habaho imiterere mishya. SiO2 iguma imeze neza ku buso bwa SA nta gikorwa na kimwe cya shimi, kandi uko ingano ya SA igabanuka, nsongero zihari zirushaho kugaragara (SATEOS1). Ibi bisubizo bigaragaza ko SiO2 ikubiyemo cyane ubuso bwa SA. Agasongero ka (700) karashira burundu, kandi agasongero ka \((\overline{5}02)\) kaba nk'agahu muri SATEOS 1 (Ishusho ya 4b), bifitanye isano no kugabanuka kwa kristali no kwiyongera kwa amorphism. SiO2 ni amorphous mu miterere yayo, bityo imisozi igaragara kuva kuri 2θ = 19° kugeza 25° ifite agahu no kwaguka53 (Ishusho ya 4b–g), ibi byemeza ko hariho SiO252 idahinduka. Ubukana bwo hasi bw'agahu ka microencapsulated SA buterwa n'ingaruka za nucleation z'urukuta rw'imbere rwa silica n'imyitwarire igabanya crystallization49. Bikekwa ko iyo SA iri hasi, silika ikomeye iraremwa bitewe n'uko hari TEOS nyinshi, ahanini ikwirakwira ku buso bwo hanze bwa SA. Ariko, uko ingano ya SA yiyongera, ubuso bw'ibitonyanga bya SA mu gisubizo cya emulsion buriyongera kandi TEOS nyinshi zirakenewe kugira ngo habeho agahu neza. Kubwibyo, iyo SA iri hejuru, agahu ka SiO2 muri FT-IR karagabanuka (Ishusho ya 3), kandi ubukana bw'agahu ka diffraction hafi ya 2θ = 19–25° muri XRF (Ishusho ya 4) buragabanuka kandi kwaguka nako kuragabanuka. Ntibigaragara. Ariko, nk'uko bigaragara ku Ishusho ya 4, iyo ingano ya SA yiyongereye kuva kuri 5 g (SATEOS1) ikagera kuri 50 g (SATEOS6), imisozi iba yegereye cyane SA y'ubunini, kandi uburebure kuri (700) bugaragara hamwe n'ubukana bwose bw'ubunini bwagaragajwe. Ibi bisubizo bifitanye isano n'ibyavuye muri FT-IR, aho ubukana bw'ubunini bwa SiO2 SATEOS6 bugabanuka kuri 1103 cm-1 (Ishusho ya 3g).
Imiterere y'ibinyabutabire by'ibintu biri muri SA, SATEOS1 na SATEOS6 igaragara ku ishusho ya 1 na 2. Ishusho ya 5, 6, 7 na 8 n'imbonerahamwe ya 2. Gupima SA, SATEOS1 na SATEOS6 bigaragara ku ishusho ya 5 naho gupima C 1s, O 1s na Si 2p bigaragara ku ishusho ya 5, 6, 7 na 8 n'imbonerahamwe ya 2. 6, 7 na 8. Agaciro k'ingufu zihuza zabonetse na XPS kari muri Imbonerahamwe ya 2. Nkuko bigaragara ku ishusho ya 5, imiterere ya Si 2s na Si 2p igaragara yagaragaye muri SATEOS1 na SATEOS6, aho habayeho microencapsulation y'agasanduku ka SiO2. Abashakashatsi ba mbere bavuze ko Si 2s isa na yo yari kuri 155.1 eV54. Kuba hariho uburebure bwa Si muri SATEOS1 (Ishusho ya 5b) na SATEOS6 (Ishusho ya 5c) byemeza amakuru ya FT-IR (Ishusho ya 3) na XRD (Ishusho ya 4).
Nkuko bigaragara ku Ishusho ya 6 a, C 1s za bulk SA zifite impera eshatu zitandukanye za CC, caliphatic, na O=C=O ku ngufu zihambira, ari zo 284.5 eV, 285.2 eV, na 289.5 eV, uko bikurikirana. C–C, caliphatic na O=C=O impera nazo zagaragaye muri SATEOS1 (Ishusho ya 6b) na SATEOS6 (Ishusho ya 6c) kandi zikubiye mu mbonerahamwe ya 2. Uretse ibi, impera ya C 1s inahura n’impera ya Si-C iri kuri 283 .1 eV (SATEOS1) na 283.5 eV (SATEOS6). Ingufu zacu zihambira za C–C, caliphatic, O=C=O na Si–C zifitanye isano neza n’izindi nkomoko55,56.
Imiterere ya XPS ya O 1 SA, SATEOS1 na SATEOS6 igaragara ku ishusho ya 7a–c, uko bikurikirana. Isonga rya O 1s rya bulk SA riratandukanye kandi rifite imisozi ibiri, ari yo C=O/C–O (531.9 eV) na C–O–H (533.0 eV), mu gihe O 1 ya SATEOS1 na SATEOS6 zihuye. Hari imisozi itatu gusa: C=O/C–O, C–O–H na Si–OH55,57,58. Ingufu zo guhuza O 1s muri SATEOS1 na SATEOS6 zihinduka gato ugereranije na bulk SA, bifitanye isano n'impinduka mu gice cy'imiti bitewe no kuba hari SiO2 na Si-OH mu gikoresho cy'igikonoshwa.
Si 2p XPS spectra ya SATEOS1 na SATEOS6 igaragara ku Ishusho ya 8a na b. Muri CA nyinshi, Si 2p ntiyagaragaye kubera ko nta SiO2 yari ihari. Si 2p peak ihuye na 105.4 eV kuri SATEOS1 na 105.0 eV kuri SATEOS6, ihuye na Si-O-Si, mu gihe SATEOS1 peak ari 103.5 eV naho SATEOS6 peak ikaba 103.3 eV, ihuye na Si-OH55. Si-O-Si na Si-OH peak mount muri SATEOS1 na SATEOS6 byagaragaje ko SiO2 yakozwe neza ku buso bwa SA.
Imiterere y'ibintu bicukuwe mu mfuruka ni ingenzi cyane, igira ingaruka ku gushonga, guhagarara, gukora neza kw'ibinyabutabire, ubushobozi bwo gutembera no gukomera59. Kubwibyo, SEM yakoreshejwe mu kugena imiterere ya SA nyinshi (100×) na SA ifite mfuruka nke (500×), nk'uko bigaragara ku Ishusho ya 9. Nk'uko bigaragara ku Ishusho ya 9a, agace ka SA gafite ishusho y'uruziga. Ingano y'uduce irenga mikoroni 500. Ariko, iyo inzira yo gucukuwe mu mfuruka nke ikomeje, imiterere irahinduka cyane, nk'uko bigaragara ku Ishusho ya 9 b–g.
Amashusho ya SEM ya (a) SA (×100), (b) SATEOS1, (c) SATEOS2, (d) SATEOS3, (e) SATEOS4, (f) SATEOS5 na (g) SATEOS6 kuri ×500.
Mu gipimo cya SATEOS1, hagaragara uduce duto twa SA twa SiO2 dupfunyitse dufite ubuso buto (Ishusho ya 9b), dushobora guterwa na hydrolysis na condensation polymerization ya TEOS ku buso bwa SA, bigatuma molekile za ethanol zikwirakwira vuba. Ingaruka zabyo ni uko uduce twa SiO2 dushyirwa hamwe kandi hakagaragara agglomeration52,60. Iki gikoresho cya SiO2 gitanga imbaraga za mekanike ku duce twa CA dupfunyitse kandi kikarinda gusohoka kwa CA ishongeshejwe ku bushyuhe bwinshi10. Ibi bisubizo bigaragaza ko uduce duto twa SA turimo SiO2 dushobora gukoreshwa nk'ibikoresho bishobora kubika ingufu61. Nkuko bigaragara ku Ishusho ya 9b, icyitegererezo cya SATEOS1 gifite ikwirakwizwa ry'uduce duto dufite urwego runini rwa SiO2 rutwikira SA. Ingano y'uduce twa SA dupfunyitse (SATEOS1) ni hafi 10–20 μm (Ishusho ya 9b), ni nto cyane ugereranije na SA nyinshi bitewe n'ingano nto ya SA. Ubunini bw'urwego rwa microcapsule buterwa na hydrolysis na condensation polymerization y'umuti ubanziriza. Agglomeration iba ku gipimo gito cya SA, ni ukuvuga kugeza kuri 15 g (Ishusho ya 9b-d), ariko iyo dose yiyongereye, nta agglomeration igaragara, ariko uduce tw’uruziga twagaragaye neza turagaragara (Ishusho ya 9e-g) 62.
Byongeye kandi, iyo ingano ya SLS surfactant ihoraho, ingano ya SA (SATEOS1, SATEOS2 na SATEOS3) igira ingaruka ku mikorere myiza, imiterere n'ingano y'uduce. Bityo, SATEOS1 yagaragaye ko igaragaza ingano nto y'uduce, ikwirakwira rimwe n'ubuso bunini (Ishusho ya 9b), byatewe n'imiterere ya SA ituma habaho urusobe rw'inyongera munsi ya surfactant ihoraho63. Bikekwa ko kongera ingano ya SA kuva kuri 5 kugeza kuri 15 g (SATEOS1, SATEOS2 na SATEOS3) no gukoresha ingano ihoraho ya surfactant, ni ukuvuga 0.10 g SLS (Imbonerahamwe ya 1), uruhare rwa buri gace k'umusemburo wa surfactant ruzagabanuka, bityo ingano y'uduce n'ingano y'uduce. Ikwirakwira rya SATEOS2 (Ishusho ya 9c) na SATEOS3 (Ishusho ya 9d) bitandukanye n'ikwirakwira rya SATEOS 1 (Ishusho ya 9b).
Ugereranije na SATEOS1 (Ishusho ya 9b), SATEOS2 yagaragaje imiterere y’uturemangingo duto twa SA kandi ingano y’uturemangingo yiyongera (Ishusho ya 9c). Ibi biterwa no guhuza 49, bigabanya igipimo cyo guhuza (Ishusho ya 2b). Uko ingano ya SC yiyongera uko SLS yiyongera, uturemangingo duto tugaragara neza, nk'uko bigaragara ku Ishusho. uburyo guterana bibaho. Byongeye kandi, Ishusho ya 9e-g igaragaza ko uturemangingo twose dufite ishusho n'ingano bigaragara. Byagaragaye ko iyo hari ingano nini ya SA, ingano ikwiye ya silica oligomers ishobora kuboneka, bigatera guhumeka no gufunga neza bityo bigatuma habaho uturemangingo duto twagenwe neza49. Dukurikije ibisubizo bya SEM, biragaragara ko SATEOS6 yakoze uturemangingo duto tujyanye ugereranije n'ingano nto ya SA.
Ibisubizo bya energy dispersive X-ray spectroscopy (EDS) ya bulk SA na microcapsule SA bigaragazwa mu mbonerahamwe ya 3. Nkuko bigaragara muri iyi mbonerahamwe, ingano ya Si igabanuka buhoro buhoro kuva kuri SATEOS1 (12.34%) kugera kuri SATEOS6 (2.68%). Kwiyongera kwa SA. Kubwibyo, dushobora kuvuga ko kwiyongera k'ingano ya SA bituma SiO2 igabanuka ku buso bwa SA. Nta gaciro gahoraho k'ibiri muri C na O muri mbonerahamwe ya 3 bitewe n'isesengura rya semi-quantitative rya EDS51. Ingano ya Si muri microcapsule SA yahujwe n'ibyavuye muri FT-IR, XRD na XPS.
Imyitwarire yo gushonga no gukomera kwa bulk SA ndetse na microcapsulated SA hamwe na SiO2 shell igaragara ku ishusho ya 1 na 2. Igaragara ku ishusho ya 10 na 11, kandi amakuru y'ubushyuhe agaragara ku mbonerahamwe ya 4. Ubushyuhe bwo gushonga no gukomera kwa microcapsulated SA bwagaragaye ko butandukanye. Uko ingano ya SA yiyongera, ubushyuhe bwo gushonga no gukomera buriyongera kandi bugera ku gaciro ka bulk SA. Nyuma ya microcapsulation ya SA, urukuta rwa silica rwongera ubushyuhe bwa crystallization, kandi urukuta rwarwo rukora nk'ishingiro ryo guteza imbere ubudasa. Kubwibyo, uko ingano ya SA yiyongera, ubushyuhe bwo gushonga (Ishusho ya 10) no gukomera (Ishusho ya 11) nabwo buriyongera buhoro buhoro49,51,64. Mu bipimo byose bya microcapsulated SA, SATEOS6 yagaragaje ubushyuhe bwo gushonga no gukomera bwo hejuru, hagakurikiraho SATEOS5, SATEOS4, SATEOS3, SATEOS2, na SATEOS1.
SATEOS1 igaragaza aho gushonga hasi cyane (68.97 °C) n'ubushyuhe bwo gushonga (60.60 °C), biterwa n'ingano nto y'uduce aho kugenda kw'uduce twa SA muri microcapsules ari nto cyane kandi agace ka SiO2 kagakora urwego runini bityo Core Material igabanya kwaguka no kugenda49. Iki gitekerezo gifitanye isano n'ibyavuye muri SEM, aho SATEOS1 yagaragaje ingano nto y'uduce (Ishusho ya 9b), biterwa nuko molekile za SA zifungiye mu gace gato cyane ka microcapsules. Itandukaniro mu bushyuhe bwo gushonga no gushonga bw'umubyimba mukuru, kimwe na microcapsules zose za SA zifite shells za SiO2, riri hagati ya 6.10–8.37 °C. Ibi bisubizo bigaragaza ko microcapsules SA ishobora gukoreshwa nk'ibikoresho bishobora kubika ingufu bitewe n'ubushyuhe bwiza bw'agace ka SiO2 65.
Nkuko bigaragara ku mbonerahamwe ya 4, SATEOS6 ifite enthalpy nyinshi kurusha izindi zose za SC za microcapsulated (Ishusho ya 9g) bitewe n'uburyo SEM yabyimbye neza. Igipimo cyo gupakira cya SA gishobora kubarwa hakoreshejwe ikigereranyo (1). (1) Hamwe n'amakuru y'ubushyuhe buhishe bwa microcapsulated SA49.
Agaciro ka R kagaragaza urugero rwa encapsulation (%) rwa SC ya microcapsulated, ΔHMEPCM, m ikagaragaza ubushyuhe buhishe bwo kwivanga kwa SC ya microcapsulated, naho ΔHPCM, m ikagaragaza ubushyuhe buhishe bwo kwivanga kwa SC. Byongeye kandi, ubushobozi bwo gupakira (%) bubarwa nk'ikindi gipimo cy'ingenzi cya tekiniki, nk'uko bigaragara muri Equation (1). (2)49.
Agaciro ka E kagaragaza imikorere myiza ya CA icukuweho (%), ΔHMEPCM,s ikagaragaza ubushyuhe buhishe bwo gukiza CA icukuweho ...
Nkuko bigaragara mu mbonerahamwe ya 4, urwego rwo gupakira n'ubushobozi bwa SATEOS1 ni 71.89% na 67.68%, uko bikurikirana, naho urwego rwo gupakira n'ubushobozi bwa SATEOS6 ni 90.86% na 86.68% uko bikurikirana (Imbonerahamwe ya 4). Icyitegererezo cya SATEOS6 kigaragaza ubushobozi bwo gupakira n'ubushobozi bwo hejuru mu ma SA yose ya microcapsulated, bigaragaza ubushobozi bwayo bwo gushyuha cyane. Kubwibyo, kuva ku kintu gikomeye kugera ku kintu gisaba ingufu nyinshi. Byongeye kandi, itandukaniro mu bushyuhe bwo gushonga no gukomera kwa microcapsules zose za SA na bulk SA mu gihe cyo gukonjesha rigaragaza ko igishishwa cya silica kiba gifungiranye mu gihe cyo gukora microcapsule. Bityo, ibisubizo bigaragaza ko uko ingano ya SC yiyongera, igipimo cyo gupakira n'ubushobozi bwo kwiyongera buhoro buhoro (Imbonerahamwe ya 4).
Imirongo ya TGA ya bulk SA na microcapsule SA ifite igishishwa cya SiO2 (SATEOS1, SATEOS3 na SATEOS6) igaragara ku Ishusho ya 12. Imiterere yo kudahungabana k'ubushyuhe bwa bulk SA (SATEOS1, SATEOS3 na SATEOS6) yagereranyijwe n'ingero za microcapsule. Biragaragara ko muri TGA curve ko kugabanuka k'uburemere bwa bulk SA ndetse na microcapsule SA bigaragaza kugabanuka gutoroshye kandi gato cyane kuva kuri 40°C kugeza kuri 190°C. Kuri ubu bushyuhe, bulk SC ntihinduka ubushyuhe, mu gihe microcapsule SC isohora amazi yakuwemo ndetse na nyuma yo kuma kuri 45°C mu gihe cy'amasaha 24. Ibi byatumye ibiro bigabanuka gato,49 ariko hejuru y'ubu bushyuhe ibikoresho byatangiye kwangirika. Iyo SA iri hasi (ni ukuvuga SATEOS1), amazi yakuwemo ari menshi bityo kugabanuka k'uburemere kugeza kuri 190°C ni hejuru (ishusho ya 12). Ubushyuhe bumaze kurenga 190 °C, icyitegererezo gitangira gutakaza uburemere bitewe n’uburyo bwo kubora. Ubunini bwa SA butangira kubora kuri 190 °C kandi 4% gusa ni byo bisigara kuri 260 °C, mu gihe SATEOS1, SATEOS3 na SATEOS6 bigumana 50%, 20% na 12% kuri ubu bushyuhe, uko bikurikirana. Nyuma ya 300 °C, igihombo cy’ubunini bwa SA cyari hafi 97.60%, mu gihe igihombo cya SATEOS1, SATEOS3, na SATEOS6 cyari hafi 54.20%, 82.40%, na 90.30% uko bikurikirana. Uko igipimo cya SA cyiyongera, igipimo cya SiO2 kiragabanuka (Imbonerahamwe ya 3), kandi agahu k’agahu kagaragara muri SEM (Ishusho ya 9). Bityo, kugabanuka k'uburemere bwa SA ifite ibinini biri hasi ugereranije na SA ifite ubunini, ibi bikaba bisobanurwa n'imiterere myiza y'igishishwa cya SiO2, gitera imbere kuremwa k'urwego rwa silicate-carbonaceous ku buso bwa SA, bityo kigatandukanya igice cya SA kandi kigatinda kurekurwa kw'ibikomoka ku bushyuhe10. Uru rwego rwa char rukora uruzitiro rukingira umubiri mu gihe cyo kubora kw'ubushyuhe, rugabanya ihinduka rya molekile zishobora gushya mu gice cya gaze66,67. Uretse ibi, dushobora kandi kubona ibisubizo bikomeye byo kugabanuka k'uburemere: SATEOS1 igaragaza agaciro ko hasi ugereranije na SATEOS3, SATEOS6 na SA. Ibi biterwa nuko ingano ya SA muri SATEOS1 ari nto ugereranyije na SATEOS3 na SATEOS6, aho igishishwa cya SiO2 kigize urwego runini. Mu buryo bunyuranye, kugabanuka k'uburemere kwa SA ifite ubunini kugera kuri 99.50% kuri 415 °C. Ariko, SATEOS1, SATEOS3, na SATEOS6 byagaragaje ko kugabanya ibiro kuri 62.50%, 85.50%, na 93.76%, uko bikurikirana, kuri 415 °C. Ibi bisubizo bigaragaza ko kongeramo TEOS byongera kwangirika kwa SA binyuze mu gukora urwego rwa SiO2 ku buso bwa SA. Utu duce dushobora gukora uruzitiro rurinda umubiri, bityo hakabaho iterambere mu buryo ubushyuhe bwa CA icukuweho.
Ibisubizo by’ubushyuhe byizewe bya bulk SA n’icyitegererezo cyiza cya microencapsulated (ni ukuvuga SATEOS 6) nyuma y’amasaha 30 yo gushyushya no gukonjesha ya DSC51,52 bigaragara ku Ishusho ya 13. Bigaragara ko bulk SA (Ishusho ya 13a) idafite itandukaniro mu bushyuhe bwo gushonga, gukomera no gukonjesha, mu gihe SATEOS6 (Ishusho ya 13b) idafite itandukaniro mu bushyuhe no gukomera no gukonjesha ndetse na nyuma y’amasaha 30 yo gushyushya. n’uburyo bwo gukonjesha. Bulk SA yagaragaje igipimo cyo gushonga cya 72.10 °C, ubushyuhe bwo gukomera bwa 64.69 °C, n’ubushyuhe bwo guhuza no gukomera nyuma y’amasaha 201.0 J/g na 194.10 J/g, uko bikurikirana. Nyuma y’izunguruka rya 30, igipimo cyo gushonga cy’izi gaciro cyagabanutse kigera kuri 71.24 °C, ubushyuhe bwo gushonga bwagabanutse bugera kuri 63.53 °C, naho agaciro ka enthalpy kagabanukaho 10%. Impinduka mu bushyuhe bwo gushonga no gushonga, ndetse no kugabanuka kw’agaciro ka enthalpy, bigaragaza ko CA nyinshi idakwiye kwizerwa ku bikorwa bitari microencapsulation. Ariko, nyuma yo kuba microencapsulation ikwiye (SATEOS6), ubushyuhe bwo gushonga no gushonga hamwe n’agaciro ka enthalpy ntibihinduka (Ishusho ya 13b). Iyo microencapsulated hamwe n’ibice bya SiO2, SA ishobora gukoreshwa nk’ibikoresho byo guhindura phase mu bikorwa by’ubushyuhe, cyane cyane mu bwubatsi, bitewe n’ubushyuhe bwayo bwiza bwo gushonga no gushonga hamwe na enthalpy ihamye.
Imirongo ya DSC yabonetse ku bipimo bya SA (a) na SATEOS6 (b) ku gihe cyo gushyushya no gukonjesha cya mbere n'icya 30.
Muri ubu bushakashatsi, hakozwe iperereza ku buryo bwimbitse ku gice cy’inyuma cya microcapsulation hakoreshejwe SA nk'igikoresho cy'ingenzi na SiO2 nk'ibikoresho by'igishishwa. TEOS ikoreshwa nk'intangiriro yo gukora urwego rw'inkunga ya SiO2 n'urwego rwo kurinda ku buso bwa SA. Nyuma yo gukora neza SA ya microcapsulated, ibisubizo bya FT-IR, XRD, XPS, SEM na EDS byagaragaje ko SiO2 ihari. Isesengura rya SEM ryerekana ko icyitegererezo cya SATEOS6 kigaragaza uduce tw’uruziga twagaragajwe neza tuzengurutswe n'ibishishwa bya SiO2 ku buso bwa SA. Ariko, MEPCM ifite SA nke igaragaza agglomeration, ibi bigabanya imikorere ya PCM. Isesengura rya XPS ryerekanye ko Si-O-Si na Si-OH biri mu bipimo bya microcapsule, byagaragaje ko SiO2 ikwirakwizwa ku buso bwa SA. Dukurikije isesengura ry’imikorere y’ubushyuhe, SATEOS6 igaragaza ubushobozi bwo kubika ubushyuhe bwiza cyane, aho ubushyuhe bwo gushonga no gukomera bwa 70.37°C na 64.27°C, uko bikurikirana, n’ubushyuhe butihishe bwo gushonga no gukomera bwa 182.53 J/g na 160.12 J/g. G. uko bikurikirana. Ingufu ntarengwa zo gupfunyika za SATEOS6 ni 86.68%. Isesengura rya TGA na DSC ry’ingendo z’ubushyuhe ryemeje ko SATEOS6 igifite ubushyuhe bwiza kandi bwizewe nubwo nyuma y’ibikorwa 30 byo gushyushya no gukonjesha.
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