Template-based approach in the preparation of nanoporous silicas and titania-silicas

Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titani...

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Datum:2001
Hauptverfasser: Tertykh, V. A., Yanishpolskii, V. V., Pavlenko, A. N., Leboda, R., Skubiszewska-Zieba, J.
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Sprache:Englisch
Veröffentlicht: Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2001
Online Zugang:https://surfacezbir.com.ua/index.php/surface/article/view/48
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Surface
_version_ 1869291129379225600
author Tertykh, V. A.
Yanishpolskii, V. V.
Pavlenko, A. N.
Leboda, R.
Skubiszewska-Zieba, J.
author_facet Tertykh, V. A.
Yanishpolskii, V. V.
Pavlenko, A. N.
Leboda, R.
Skubiszewska-Zieba, J.
author_institution_txt_mv [ { "author": "V. A. Tertykh", "institution": "Інститут хімії поверхні НАН України" }, { "author": "V. V. Yanishpolskii", "institution": "Інститут хімії поверхні НАН України" }, { "author": "A. N. Pavlenko", "institution": "Інститут хімії поверхні НАН України" }, { "author": "R. Leboda", "institution": "Maria Curie-Sklodowska University" }, { "author": "J. Skubiszewska-Zieba", "institution": "Maria Curie-Sklodowska University" } ]
author_sort Tertykh, V. A.
baseUrl_str
collection OJS
datestamp_date 2018-11-27T09:42:39Z
description Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature.
first_indexed 2025-09-24T17:44:38Z
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fulltext 1 , : TЕMPLATЕ.BASЕD APPROAсII IN TIlЕ PRЕPARATION oF NANoPoRoUs sILIсAs AND TITANIA.SILICAS v.A. Tertykhl, v-.V. yanishpotskiir, A.N. pavlenkor, R. Lеboda 2, and J. Skubiszewska.Zieba2 IInstitute of Suфсе Сhemistrу, Nаtionаl Асаdеmу of Scieпces, ,!368'0 Kуу|64, Gеn' Nаumov str' 17, UKRАINE; е.mаil.: tе}tуnh@public.uа.net,Fасultу of Chеmistry, Mаriа Сurie-Sklodowslrл (Jniуersilу, 20lЬ1 Гiьiti, iol,ц-io Мesoporous siliсas and tiиnia-siliсas wеrе synthesized with usе as a tеmplatе cгnary ammonium salts aпd thеir hydroxidеs. Fumed siliсa, tetraethyl orthosiliсate andtrnium(IV) tetraisopro-p-o-хide wеre appliеd as prеsursors. Synthеsеs wеre са:тied out in FGsеnсе HCl and Nн4oI{. Мesoporous tiиnia-siliсas wlth тioz сontents from 1 up tо 70 *Нт.l'ЗT*- o.lы]:o samples !9v3 b^een сharaсtеrized by the powder. x-ray ff:''* 1* Pd nitrogеn adsorption at77 K. Speсifiс surfaсe areц total poгe volume,'lЕЕ volume and arеa distribution wеre detеrminеd from nitrogen adsorption isotherm foi AЬtraсt resizеd titаnia-siliсas. It was demonstratеd that thе ordйс struсЬs of MCМ-41 and bimоdal pororrs materials with maximum porе diametеr of 3 and 30 nm rnay be ;rвpаred dеpеnding ofa synthesis сonditions and a prеоuгsor natЦre. .lrtroduсtion Rеmarkable aсhiеvеmеnt of the lаst dеcade in the fiеld of synthesis of orderrd ъоstruсtural matеrials is pгepаration of a new сlass МCМ-41 periodiс silicatеs, &шinosiliсatеs [l.2] and non.siliсa pеriodiс mesostructurеd matеrials t3] with nore tЁameter from 15 up to 100 A and high spесifiс surfaсe area (morе than tо.orj 1nъ ;'h tс use of surfaоtants as suprаInolесular tеmplates. Suсh matеrials are used as Jutяy.t Cшriегs due to thеir unique geomеtriсal struсture, high thеrmal stability and adsorptivф [tЬ5]. Considеrablе rrсent attention has bееn foсusеd on synthеsis of MCМ.4l materiats mtаinеd in their strшсture the ions of hansition metals, in partiсular tiиnium [5-11], foт ре'paratiоn of matеrials with high сatalytiс aсtivity and whiсh are stablе at hеaйg й ; mditions оf hydrоthermal treatment [51. so in thе work [5], hydrothermal stabiliiy up to ш0 oC and stability in acid mеdium фH=2) was distingui.ii.с гo. obиined тi-мbй-+r шяteгials in сontradistinсtion to zeolites whiсh aте muсh less stable in the same сonditions. hсlusion of tiиnium into the skеlеton of mesoporous siliсa matriсеs permits one to creatе сw matегials йth porе diamеtеr in thе range 15.100 A, high spесifiс surfaсe area аnd пith сatalytiс aсtivity in oxidation rеaсtions of largе organiс moleсulеs, for whiсh dsorption spaсe of known pеrspeсtive Ti.сonиining сatalysts of a ТS.1, ТS.2 and Тi-p t1pеs is inaссеssiЬle [6]. The works [7,8] dealing with synthesis of Ti-МCМ*41 and Ti. HМS must bе pointed out in this dirесtion. It has been shown, in partiсular, that Ti-МCМ. |l matеrials, alongside йth Ts-l and Ti.tIMS, arе rffective сatalysts foг hydroxylation rcaсtion of bеnzenе to phenol' The сaиlytiс aсtivity of Ti-HМS and Ti.МCМ.41 in thе rcaсtion of 2,6-di-tеrt-buф phenol oxidation wаs also dеmonstratе d t7J, Titanium сonиining siliсatеs drmonstatе also photoсatalytiс aсtivity [ 1 l. 1 3] 59 Тhе aim of this woгk is to оontinuе systеmatiс rеsеarсh in thе fiеld of synthesis and сharaсtеrization of nanoporous purе silicas and titania-siliсas braring vаrious amоunts of titanium. Ехpеrimеntal For prеpаration of mesoporous siliсa аrrd titania.siliсas tеtraеthyl orthosiliсatе (TЕos) and дerosil 300 was usеd as a siliсa sourсe and titаnium(IV) tеtraisopropoхide was сhosen as a titаnium sorrrсe' Quatеmary ammonium salts oсtadeсyltrimеtфlammonium chloridе (oDTМAсl, сl8сl) and hеxadесyltrimеthylammonium bromidе (HDTMABr, C16Br) and tеtramеthylammonium bromidе. (TМAв;, ClBr) was applied as tеmplate' These salts чrеre transformed intо hydroxyl form with an use of thе ion-ехоhangе сolumn filled by thе AB.17-8 anionitе in hydroxyl form.. .Sуnthеsis of mеSoporous silicаs frоm fumеd sl/iсс. Fumеd siliсa (aеrosil) was suspеndrd in water or in aquеous solution of quaternаry amine hydroxidе at intensivе stirring" Rеsulting siliоa сonсentration was about 30 wt %. Siliса/aminе ratios arе indiсatеd in thе Тablе 1. obtained suspensions allow to stand for 24.28 hrs аt гoom tеmperaturr, thеn wеre driеd up at 150oC and сalсinated at 540 oC for 6 h on air. Sупthеsis of MСM-41 purе siliса paJ, weighеd portion of t}rе surfaсtant (8.3 g сTМAB;) wаs dissolvеd in 42 ml of сonсentratеd ammonia solution and intегmixed to homogеnеous milk.white miхture' After addition af 9,67 ml ТЕoS thе miхtuте obtаinеd was st.iкed up to gеl.likе produсt formation. Thе samplеs prepаrеd wеrе dгiеd up at air and сalсinatеd at 540 oс for 6 h on air. Sуnthеsis of titаniа.siliса in prеsеncе of HСl. Меsoporous titаnosiliсas with molar ratios Ti/(Ti + Si) еqual 1, 15,30,50, and 70oАwerc synthesized using thе tесhniquе desсribеd in thе work [7]' Тhе nесеssary Ti(ЁoCзF{z)4 amount was added by small pоrtions at stirring to TЕoS solution in miхturе of еthanоl and isopropаnol. Weighеd portion of oDTМACl was dissolved at intеnsivе stirring in watег with addition of small amount of сonсеntratеd HCl. obtainеd homogenеous milk.whitе suspеnsion was addеd to initial miхturе at intensive stirring and hеating up to 60 oC for the gel prrparation (for l.5 h). Тhe gel was subjесted to aging foт 18 h on air. Samples wеrе driеd up at l20 oC for 3 h, and thеn wеre calсinated at 540 oC fоr 6 h on air. Sуnthesis of titаniа.siliса in presence of NHaОH' 0.124 ml (0.00043 mol) TiPoT was addеd by small portions dt stirring to 9,52 ml (0.0426 mol) TЕos (Til(Ti+Si)х10й1%). ConЬеntratеd ammonia solution (a2 ml) was addеd at stirring to the *"igьeс portiоn of the srгfaсtant 8.3 g CTMAвr (0.0228) mol. obtainеd milk-white mixturе was drawn togethеr йth an initial solution and was stirred up to gel.likе produсt formation (5 hrs). Solid prоduсts wеrr сalсinatеd at 540 oC fоr 6 h on air. Samplеs йth thе titanium contents l5, 30, и' 50Yo were preparеd in a similar mannеr. Charaсtеrization of the synthesizеd samples was performеd by thе powdеr Х-гay diffraсtion (xRD) data (automatеd diffraсtomеtеr DRON-3M, CuК{l radiation) and nitrogеn adsorption isothеrm measurеments at 77 K on ASAP-2000 Мiсromeritiсs еquifmrnt. Averagе porе diarnеter was estimatеd by Gurviоh method (d=4VlS)' The ф"iл. sшfaсе *"u, Ъgg,, was dеtеrminrd from the linеaт part of thr BЕT equation (at o,,, = 0.05-0.з5). Poгe volume distribution was сalсulatеd from desorption branсh of an i'oЬ"* of nitтogеn adsoгption using thе Barrett-Joyner.Halеnda (BIII) formula [16'17]. Cоmparativе с-рlots [16,18,l9] wеre сonstгuсted using stаndard nitrogеn adsorption daи for siliсa ofJaтoniес at al. [20]. lсrotв en. Т}rc з Ёя:пrщ11 i6 Ciri( тЪцs lсr rmpoп \rзаgс hr .lrФal.'l d E} l. с'соr t-pac s S i rct6 I 16. I 6 I t .t\ А -{' т т т тl п п п п тт тт тE гЕ ! t r t r t I t l6ь l 6 t 6 t6 г@d я] саr} Ргас lA r фс t* цс und b cэdд $rcс ltЬв rс dlL prв b:rtт rn тЬ )! в 'Cr G r r в . 60 v d 3 е I в l. L and disсussion Thс sourсеs of siliоa aеrosil аnd tеtraеthyl orthosiliсatr praсtiсally dо not соntain of ions and sodium. All sрthesеs werе сanied оut also in absenсе of inorgаniс Thus, obtainеd siliсas and titania-siliсas do not сontain ехtrarrrous impurity, that is impоrtant for thrir usе in сatalysis. Bсsidеs usr of TЕoS allows onе to avoid a hydrotermal trеatnеnt arrd tо сarry out of synthesis at room temperatuте. Somс сhаraсtеristiсs of thе prеparеd samples arе submittеd in thе Тable 1. l. Geomеtriсal сhaгaсtеristiсs of mеsoporous siliсas anf titаrria.siliсas. si Aсrosil l Aеrosil AеrosiI l TЕos |6a TЕos 16 TEOS l8 TЕos l8 ТЕos l8 TЕos 8 TЕos 8 ТЕos l6b ТЕos 16 TЕos 16 TЕos t6 TEOS TМA-o}I сl6-CIн Cl6-Br C16-Bг Cl6-Br сl8сl с l8Cl с l8с l с l8с l с l8C l Cl6-8r Cl6-Br Cl6-8г C16-Br . н2o 0.20 Hzo 0.10 Hzo 0.53 NI{4oн o,27 нсl 0'27 }Iсl 0.2,| I{сl 0'27 нсl 0'27 tlсl 0.27 нсl a.27 нсl 0.53 NI{4OI{ 0.5з NI{4oн 0.53 NTI4Oн 0.5з NtI{oII Sioz Tio2 Tеmplatе preсrrгsor сontent s, moL'Уo Tеmplatе Меdia /oхide molar тatio вЕT Toиl Poгс surfaсе pore diamеtеr, arеa' volumr, A' iц сm3/g 25з I.32 208 206 1.08 2r0 4|6 |.42 |з6 |29| l.з0 40 1284 0.89 28 987 o'79 з2 924 0.47 20 805 0.45 22'702 0.52 30 529 0.59 46 35з 0.45 5l 900 0.98 4з 618 1.04 67 459 0.94 82 з40 0.48 57 0 0 0 0 I l 5 I l 5 30 50 70 I l 5 30 50 Fшtеd siliсa is oftеn appliеd for prepаration of aеrosilogеl, suitablе foг usе as a сaгriеr сatalysts inсluding enzymrs. As it is visiblе from Fig.l aerosilogеl has no Praсtiсally all its spесifiс srrrfaсе сonsists from a suгfaоe of mсsopore urall йth 200A аnd abovе. At rеalizatiоn of sщthеsеs at prеsеnсе of tymеttlylammonium the total speсifiс surfaсe arеa f$dесгеased and pore diamеtеr сalculatеd by Gurviсh was unсhanged. Howevеr, as shown in Fig 2 the sample has miсroporоsity. It is to ехplain this faсt by aсtion teframethylammonium ions as a tеmplate. Usе mоrе tспrplate с16oн rrsults to bimodal mсsoporous samplе (Fig. 3). As shown in Fig.3, 2 thеrе aге two maxima on aсurvr of pоre disfribution at 30 and 300A аnd praсtiсally howеver in ХRD pattегn of this samplе doеs not find out prеsеnсе of thс ordrrеd шс' Thе ХRD diffraсtоgram for МCМ-4l samplе is slrown in Fig.4 аnd lattiсе is rеprеsеntеd in Тable 2. This samplе eйibitеd ХRD pattеm with diftaсtion whiсh аrе сharaсteristiс of wеll.ordеrеd hеxagonal struоhше (4 reflесtions). Fig. 5 il of thе pores whiсh diameter are eguаl to those сalсulatеd by Gurviоh mеtltod (136 А), ;юrе diametеr 30 A in this sample сorrеsponds to pore diamеtеr of materials МсМ-41 6 l dеmonstrates irdsorption isotherm шrd porе distribution whiсh is typical for hiфquality matedals of МCМ-41 typе. t000 800 600 G t-Ф o a)() тi o ll oo tlб o Е эo 400 200 0 0.5 r.o 1.5 2.0 2'3 Standard Adвorption сl. Fig. l. Comparativе сo.plot for aеrosilogel (Sample Si.in Tablеl) Fis. 2. Comparativе щ-plot for arrosilogll- гrеpаrеd in the prеsоnсe of TМAOH (Sarrple siсl i,I ;;i;ri.i*;isс .;fЁ,-ъ*.;=50 m2lg, d--l6 A, V'i=0.02mУg o 600 o tt (t ч 40(т'Фд oв' Е 2o . o Еэ o 1.0 1.5 2-O ш lqю 800 600 140 120 < 100 вq 8 oЕ з 6 0gt < 4 0 20 0 o.7 0.6 0.5 в 0.o Ё o. 'з 0.2 < 0.12сю 0 10 1ф 1oo0 Pore dlemetвr (Aagstrom) t0.5 RЕlative preзз uгo, P/P0 'f .0 .t.5 2.0 2.5 3.0 Standard Adsorptlon с. F.ig.3. Nifrogеn isotherm at -l96oC (/), porе volume and porе surfaсe arеa distributions (2) and сomp#ativе щ-plot (3) for bimodal mesoporous siliсa (Samplе siсl6 in Tablel). 63 Tablо 2. Х-тay diftaоtion datдof МCM-4l d;;;Ы;. сеll pшrrrеtеr, a=453 A bkl ffiы Catсulatеd i.valuеs, d-valuеs, Angstrom Angstrom ffi iio 22.66 22.СI ioo |9.Ф 19.63 11o 14E5 14'84 4 O 2 o(dcgrcв) Fie. 4. Х.ray diffiaсtion Pattеrns.oflvICM4l t1рe silica . .'. -- Gйlе MCМ-41 in Tablеl). $ E ri йo toш A E os" & !, coo I eoo o .. тoo E o 6 0 0 a Ь э o o o ! roo ! зooЕ 2 zo< o ) r o t o .o 0 ' 5 s t r n d l r d A d t o r p t l o n с . Fis. 5. Niшogеn isothеrm at -l96oC (l), .pore volume аnd por€ surfaсе disшibшioпs d;d i.йin" *.piot (3) for МсМ41 prrre siliсa. t10 900 800 7о0 600 500 400 з00 200 ioo 0 tt Е ta Еo Ё J o Еб в € o o Е ш 0.6 0.8 Rg|etlv € proвзurэ,P|Po o.2 0.4 900 1 l 8(ю ] 7 Ф ' G00 500 400 300 200 tФ 0 ' ] o r . ь 2 . 0 64 ш O o t' I t s € Б a t E 6 OW 50о 400 300 200 100 0 t 7oo Ч о00 Е 5o0 i F- a00 € 6 з o o 3 zoo ! roo эo, | 2 з stаndard Adзorptlon сr. 1 2 з standard Adsorption с. n,,6. Comparative сu-plot fоr mesoporous titania-siliсa prеpаrеd in HCl media (1) (BЕT surfaсе arca1.284 m./g, S3*1=l4 m./g, Samplе TilSiCl6a) and in NIl4oH mеdia (2), (BЕТ surfaсr area 900 m./g, 3"*1=21| m.lg, Samplе тi ls ic l6b). a c i € a aсэ c з 0 Tablе 3. Х-ray diffraction data оf titania. siliсa withl5% Ti. Hеxagonal unit сеll paramеtеt, a=50,3 A 2 0 1 0 hkr Ехpеri. mental d-valuеs, Ansstrorт Calсu- latrd d.valuсs, A noсff^fr 100 46.59 l l 0 25.46 25.17 240 2t.92 2l -802 3 1 2 @ ( d e g r e в s ) J|1 . X-raу diffraсtion pattеrns of tiиnia-siliсa with |5% Ti (SamplеTil5C16 in Tablеl) prеparеd in NHloH mеdia. From Fig. 6, сurvе l is visiblс that titania-siliсa obtainеd in HCl media has not -3nifiсаrrt еxtemal surfaое in сontrast of thе samplе prepared in N}I+OH mеdia (Fig. 6, Crc 2). At synthesis titаnia-siliсa by.tесhniquе usеd for synthesis of purе MCМ-4l siliсa Ьrgonal struсture is kept up to 15 % of thе сontеnts of tiиnium (Fig.7 and Tablе 3). DiffIaсtoglаms of the obtainеd titanium-сontaining matеrials prеparеd in HCl arе q1lsсntеd on Fig. 8. It is nесеssary to notе that thouф samplеs of titania.siliсas rесеivеd bу f iп нсl mеdia havе a еxtrеmеly high spесifiс surfaсе arеa and uniform poте distгibution tу arе not well ordеred. 65 Е AYa t 6 с ! h1 а c ii Is 5 2 e . D э 3 r э з l Fic.8.,Ёray фqry-*T#Ё;!*ЕъТЁi;:s йttr vшious titаrrium сontents (in шol Уo) prepared intlсl 0.1 0.08 d d 0.06 Еf,:.il 0 ,ю 80 t2o .160 2fll dд 0.15 .; S o'r Е l ' Е Е o.os 0.15 с' < 0.l э о Е B o'os 0 'Еl Ф so 12o 160 200 d,A А" o 40 Ф t2o t60 дl0 d ,A o12 0.1 .i < 0.08 з Е 0.06 = g o.o1- - o.o2 0 Tig. ?. r.9:.".:lу: uif.lЁI38''iJu1iГ#Г}. lжl,ii''ifr ъTJ#Ы' ;;;й;" . с t всt ь нсl.04080ТTТ d ' A 5 0 t J O $ t l t 6 * t t Е Е 66 Цs Vr iп Availabilф of small.angle pеak on ХRD pattсгn of thе mеsoporous siliса" сontaining l mol. % of titanium, tеstifirs about ехistеnсе in this samplе of ordеrеd struсfule, but nо stгuсtural information сan bе ехtraсtеd from this diffraсtograms [21]. Pеaks at 20 в 25o is сharaсtеristiс of anatаsе struсturе tеndеd to inсrеasе with inсrеasе in mеtal сontents in titаnium-сontaining siliсas. Basеd on adsorption rеsеarсh it rvas shorпn that valuеs of speсifiс srrrfaсe атea in thе titаrrium.сontaining siliсas, dеtеrmined by BЕТ method, dесrеasе with thе inстеаsе of tiиnium сontrnts both in aсid and basе сonditions (Tablel)' For samplе obtainеd in HCl mеdia with Cl8сl template thе pore diameters, сalсulatеd by Glrrviсh mеthod, arе inсreased from 20 up to 51 A at slightly varying total porе volumе (0.45.0.60 с-3/g;. As thе tiиnium сontrnt in the samples is inсгеasеd, the йapе of thе пitrogеn adsorрtion isothеrms is сhangеd from I up to IV typе with oссuпrnсr of hystеrеsis loops сharaсtrristiс of mеsoporous struсturеs and оlosе undеr form to Hl фpе [16]. .Thе сцryеs of porе volumе distributions on pore diametеr for thе synt}'еsizеd titanium-сontaining mсsoporоus matегials arс suЬmittеd on Fig. 9. At low titаnium сontents in samplеs (dоvrn to 30 mol' %) the ruшrow volumе pоrе distribution on porr diamеtеr is obsеrved. Conеlusion Thе obtainеd expеrimеntal data tеstify an oppor|unф of tеmplatс sytrthesis оf Einoрorous siliсa and titаnia-siliсas with high titanium сontеnts and advanсed spесifiс surfaсе зеаs. Мorе ordеred struоturеs of purе siliсa and titаnia siliсa MCМ-4l typе is possiblе to FrParr inNЦoH mеdia. Aсknorмlеdgement The rrsеarсh dеsсribed in this publiсation was suppoгted in part by NATO grant No.ЕST.CLG.976890 and by Forrndation of Fundamental Rеseаrсh of thе Мinisф for Еduсation and Sсiеnое ofUkrainе Rеferеnсes t. B€сk J.s., vаrtuli J.C., Roth V/.J., Leonowiсz М.Е., Kresgе C.Т., Sсhmitt K.D., Chц C.T-W., olson D.H., Sheppard Е.W., МсСullen S'B., Higgins J.B., аnd Sоhlеnkеr J.L. A nеw family of mеsoporous molесular siеvеs prеparеd with liquid сrystal templatеs // J. Am. Chem. Soс. . 1992. . v.114. - P.l0834.l0843. 2. Сiеsla U. аrrd Sсhtith F. ordеred mesoporous matеrials /l Мiсroporous and Меsoporous Мatеr.- 1999'- У.2'I.. P.13 l.l49. 3. Sayari A. and Liu P. Non.siliсa pеriodiс mesostrцcturеd materials: recеnt progrеss// Мiсroporous Мatеr. - 1997. -У.|2,.p.|49-|77, l. Coгma A. From miсroporous to mesoporous mlесular siеvе materials and thеir use in саиlysis// Chem. Rеv. - l997. -v.97. -P.2373-247з' t. Chеn L'Y., Jaeniсkе S., and сhuah G.K. Thermal and hydrothermal sиbility of framеwork. substitutеd МсМ-4l mеsoporous mateia|sllМiсroporous Мatеr. - |997'-у.|2. - P'з2з- 330. Zhao Х.S., ф,(ax) Lu G.Q., and Millar G.J. Advanсеs in mesopoгous molесular siеve мсМ.4l // Ind. Еng. Chеm. Rеs. . l996' - v.35. .P.2075-2090, Тanеv P.T., Chibwе М., and Pinnavaia Т.J. Тitалium-сontaining mеsopororrs moleсulаr siеves for сatalfiiс оxidation of aromatiс сompounds// Naturс. - |994. -v.з68. -P'з2|-32з' 6',7 8. Zhang W.. .w*g .J.i Tanеv P.T', T1 ̂ '.'Ж:1Ь}l;iif*;,Bi:r]ДТжs. :"iffi: " ;;; iransition.mеtal substitutеd hеxagonы : v. в.. p.этs.T т*.u-i T. Synthesis of titanium-соntaining МсМ-41// Мiсroporous 9. KoYano K.A. шto l, й;;--1997..v.l0. -Р.259-21|' юrous molесulаr.sievе , o. ojil". Yo: : .l* .з "*-*жiTi, J :'lЁ."в;lЖ::' Ьъ'fi Ы -i .ill в-ztвz, МCМ-4l: syntIrеsrs 1flЦ-vuвсv*..;^.: D т wоns J.. and Pinnavata l.J. rvlc-ьUPvrt.'.',.ii***;чlч:^#$"ъ1"Т'н#"'*i'ж1з.д:,ffi;**'yiJry.:Щ* titanosiliсше mo]^е.с.$ar ']:T:'*Т"H:-1#;;;i,oiЪrpьy*iсal propеrtiеs andсatаlytiс *;T*:}Т*j:'lJ frfiЁ'!I.i"rii:#^ff;:Тй . v r r в" - i,g t вц.g ll t, 12. Мatthеws t,.к. ani;;Ъ. ть" i*gn9,"йЪi'i*iu into:nоdifiеd siliоatеs fof solаr photodеgrad*"' }ln"Ё"*,p""йl l: sТiЁ"ii"i""* and Tесhnology. . 1997.. V.8. - P,619.62з. 13. Stonо V.F. Jr' and Davis R.J. Sщthеsis, оhаraсtеrizatio1r, and Dhotoсatalytiс aсtivity of titаnia and niobia i,",Ьpo,oo, molrсular;;;Jiъh;*. Мatеr. ] tqgв. . v.10. . P'l468. 1,414. 14.AnpoM' ,Yamash i taH. , IkеuсK. , .Fu j i iY . ,ZhangS.G, , , . Iф inash iY . ,PаrkD.R. ' Suzukiv., кoy#l;,,й.i;,;,*r т "iЬ*Ь.JйiJ.rеduсtion of Coz with l{zo on тiMсM.41 ш,o.ii-йсм.48 mеsoporо.j..,,""ii," i"ыysts// Cata'ysis Today . 1998. . i.цi-p.зzl-ззэ. R. A 28.yеar-old synthesis of miоеllе-tеmplated '' ;j,ffffiI;,iffi','il",h"Hi''''ii.''.".ъй : v, iы. - P.2li3-286. t.. 16. Grеgg S.J. antl ii,щ к.s.w. дс,o,p,ion],s,*i""" д'""Ыо Pйsity, London: Aсademiс Pтеss, t982' 17.BarrеttЕ.P.,JoщеrL.J.,аndHalеndaP.P.Thеdеtеrminationofporеvolumеandaтеa distributions *',"."-,"J*,Ь.j..^l.^ё;;;й""s from nitrogen isothеrms// J. Am. Ёi;;. .;". . l95i. - v.73. - P. 3]'1'389. Mesopoте sizе. and surfaсе 1 8. Fenеlonou v.B,,,io;.йko" J N : Td Dеrеvyankin A.Yu. arеaсalсulati"";i;;;;й9".ly.'::9d;;;^й"'йсм-4.l,FsМ.16,еtс.)usinglow- anglе ХRD *u""i."*iiЫ iata ||Мi;,.;;;;.*а М",opo,ous Мatеr. - |999. - v.28. - P- 51.,72' 19. Sсhulz-Еkloff G.. kft"YЧ.j:, зnd Zukal A. Controlling of morphology and оharaсtетizatio., Ъi po," struсtче oi. o,а.,"a mеsoporous ..iii"*ll Мiоtoporous arrd ,.$ffijJff*'fl: .Jч,,]::i#,i,.J.'. o*u*o t,,oo*"o adsorг]i91 daи foт сharaсtеrizat,""Тr?*",orou; gi'сii,ril*Ь'i'. i!3я. ..v..rs. . P.5410.5413. 21. Sсhaсht ,"' ,J"ЁJй;*1-*"*.il?"J"rьc }:,uy.ry;;*- and TЕМ images of МсМ-41 // Мicroporоus and м..opo,*, й;й. - iqяв' -у.22,-P,485-493. 68 эo f ьЕ Ltt b -q - D
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spelling oai:ojs.pkp.sfu.ca:article-482018-11-27T09:42:39Z Template-based approach in the preparation of nanoporous silicas and titania-silicas Template-based approach in the preparation of nanoporous silicas and titania-silicas Template-based approach in the preparation of nanoporous silicas and titania-silicas Tertykh, V. A. Yanishpolskii, V. V. Pavlenko, A. N. Leboda, R. Skubiszewska-Zieba, J. Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2001-06-10 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/48 Surface; No. 4-6 (2001): Chemistry, Physics and Technology of Surface; 59-68 Поверхность; № 4-6 (2001): Химия, физика и технология поверхности; 59-68 Поверхня; № 4-6 (2001): Хімія, фізика та технологія поверхні; 59-68 3154-8091 3154-8083 en https://surfacezbir.com.ua/index.php/surface/article/view/48/47 Авторське право (c) 2001 V.A. Tertykh, V.V. Yanishpolskii, AN. Pavlenko, R. Leboda, and J. Skubiszewska-Zieba
spellingShingle Tertykh, V. A.
Yanishpolskii, V. V.
Pavlenko, A. N.
Leboda, R.
Skubiszewska-Zieba, J.
Template-based approach in the preparation of nanoporous silicas and titania-silicas
title Template-based approach in the preparation of nanoporous silicas and titania-silicas
title_alt Template-based approach in the preparation of nanoporous silicas and titania-silicas
Template-based approach in the preparation of nanoporous silicas and titania-silicas
title_full Template-based approach in the preparation of nanoporous silicas and titania-silicas
title_fullStr Template-based approach in the preparation of nanoporous silicas and titania-silicas
title_full_unstemmed Template-based approach in the preparation of nanoporous silicas and titania-silicas
title_short Template-based approach in the preparation of nanoporous silicas and titania-silicas
title_sort template-based approach in the preparation of nanoporous silicas and titania-silicas
url https://surfacezbir.com.ua/index.php/surface/article/view/48
work_keys_str_mv AT tertykhva templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas
AT yanishpolskiivv templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas
AT pavlenkoan templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas
AT lebodar templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas
AT skubiszewskaziebaj templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas