Name: synthesis and reaction chemistry of nanosize monosodium titanate
Uploaded: 2016-02-23T14:00:00.000+00:00
Duration: 8 min 44 s
Description: Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

The authors thank the Laboratory Directed Research and Development program at the Savannah River National Laboratory (SRNL) for funding. We thank Dr. Fernando Fondeur for collection and interpretation of the FT-IR spectra and Dr. John Seaman of the Savannah River Ecology Laboratory for the use of the DLS instrument for particle size measurements. We also thank the Dr. Daniel Chan of the University of Washington and the National Institute of Health (Grant #1R01DE021373-01), for funding experiments investigating the ion exchange reactions with Au(III). The Savannah River National Laboratory is operated by Savannah River Nuclear Solutions, LLC for the Department of Energy under contract DE-AC09-08SR22470.

1. Síntese de titanato Nano-monossódico (nMST) <ol><li> Preparar 10 ml de uma solução 1 # pela adição de 0,58 ml de uma solução de metóxido de sódio a 25% em peso e 7,62 mL de isopropanol seguido de 1,8 ml de isopropóxido de titânio. </li><li> Preparar 10 ml de uma solução # 2 por adição de 0,24 ml de água ultrapura com 9,76 mL de isopropanol. </li><li> Adicionar 280 ml de isopropanol a um balão de fundo redondo de 3 tubuladuras de 500 ml, seguido por 0,44 ml de Triton X-100 (MW média: 625 g / mol). Agita-se bem a solução com uma barra de agitação magnética. </li><li> Prepare uma bomba de seringa dupla canal para fornecer soluções # 1 e # 2 a uma taxa de 0,333 ml / min. </li><li> soluções de Carga # 1 e # 2 em duas seringas de 10 ml separados, equipados com uma extensão de tubagem que vai permitir a entrega da solução a partir da bomba de seringa para abaixo do nível da solução no balão de fundo redondo de 500 ml. </li><li> Enquanto se agita, adicionar todas as soluções # 1 e # 2 (10 ml de cada) à mistura reaccional usando a bomba de seringa programado no passo 1.4. </li> &lt;li&gt; Após a adição estar completa, a tampa do frasco e continuar a agitar durante 24 horas à TA. </li><li> Uncap o frasco e aquecer a mistura de reacção a ~ 82 ° C (isopropanol em refluxo) durante 45-90 minutos, seguido por purga com azoto enquanto se mantinha o aquecimento. Como isopropanol é evaporado, adicionar água ultrapura intermitentemente para substituir o isopropanol foi evaporado. </li><li> Depois de a maior parte do isopropanol ter evaporado e o volume de água adicionada é de cerca de 50 ml, remover o aquecimento e deixar a mistura reaccional arrefecer. </li><li> Recolhe-se o produto por filtração através de um papel de filtro de nylon de 0,1 um, e lava-se várias vezes com água para remover o surfactante e qualquer isopropanol residual. Não filtrar à secura. Após a lavagem estar completa, transferir a pasta a partir do filtro para um frasco ou frasco previamente pesado, e armazenar como uma pasta aquosa. </li><li> Determinar o rendimento através da determinação dos sólidos cento em peso da lama. Isto pode ser feito medindo-se o peso de uma aliquota dea suspensão antes e após a secagem. </li></ol> 2. Au (III) Troca Iônica <ol><li> Transferir 6,50 g de 4,23% em peso de pasta nMST para um tubo de centrífuga de 50 ml. Esta quantidade pode variar de acordo com a percentagem em peso real da lama nMST produzido no passo 1.10, e determinado na etapa 1.11. </li><li> Pesar 0,0659 g de HAuCl 4 · 3H 2 O em um frasco de vidro de 1-dram. O alvo Ti: relação de massa Au é de 4: 1. </li><li> Dissolve-se o HAuCl 4 · 3H 2 O em ~ 1 ml de água, em seguida, transferir para o tubo de centrifugação contendo o nMST. Lavar o frasco várias vezes com água adicional para garantir que todo o 3H HAuCl 4 · H2O é transferido para o tubo de centrifugação contendo o nMST. </li><li> Dilui-se a suspensão com água adicional, se necessário, para levar o volume total a 11 ml. Alvo uma concentração final Au (III) de cerca de 15 mM. </li><li> Envolver o tubo de centrifugação em papel de alumínio para manter a suspensão no escuro, umad, em seguida, secar a suspensão em uma rotisserie agitador durante um mínimo de 4 dias. </li><li> Recolhe-se o produto por centrifugação a 3000 xg durante 15 min para isolar os sólidos. Lavar os sólidos três vezes com água destilada por redispersão em água, e reisolate por centrifugação a 3000 xg durante 15 min para remover qualquer unexchanged Au (III). </li><li> Armazenar o produto final, quer como uma suspensão aquosa por redispersão em água, ou como um sólido húmido por decantação a água da lavagem final e capping do tubo. Armazene o produto no escuro. </li></ol> 3. Preparação do Peroxotitanate <ol><li> Transferir 5 g de uma suspensão 9,8% em peso de nMST a um pequeno frasco. </li><li> Pesar 0,154 g de H solução a 30% em peso de 2 O 2. O alvo H2O 2: razão molar Ti é 0,25: 1. </li><li> Enquanto se agita a suspensão nMST bem adicionar a 0,154 g de H 2 O 2 a solução gota a gota. Após a H 2 O 2 a adição, a suspensão de WHIte sólidos imediatamente fica amarelo. </li><li> Após a adição estar completa agita-se a reacção à temperatura ambiente durante 24 h. </li><li> Recolhe-se o produto por filtração através de um filtro de nylon de 0,1 um, e lava-se várias vezes com água para remover qualquer não reagido H 2 O 2. Não filtrar à secura. Após a lavagem estar completa, transferir a pasta a partir do filtro para um frasco ou frasco previamente pesado, e armazenar como uma pasta aquosa. </li></ol>

<ol>
	<li>O'Regan, B., Gr&#228;tzel, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+low-cost,+high-efficiency+solar+cell+based+on+dye-sensitized+colloidal+TiO2+films.">A low-cost, high-efficiency solar cell based on dye-sensitized colloidal TiO2 films.</a> Nature. 353, 737-740 (1991).</li><li>Frank, A. J., Kopidakis, N., van de Lagemaat, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrons+in+nanostructured+TiO2+solar+cells:+transport,+recombination+and+photovoltaic+properties.">Electrons in nanostructured TiO2 solar cells: transport, recombination and photovoltaic properties.</a> Coord. Chem. Rev. 248 (13-14), 1165-1179 (2004).</li><li>Mor, G. K., Varghese, O. K., Paulose, M., Shankar, K., Grimes, C. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+review+on+highly+ordered,+vertically+oriented+TiO2+nanotube+arrays:+fabrication,+material+properties,+and+solar+energy+applications.">A review on highly ordered, vertically oriented TiO2 nanotube arrays: fabrication, material properties, and solar energy applications.</a> Sol. Energy Mater. Sol. Cells. 90 (14), 2011-2075 (2006).</li><li>Dosch, R. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Use of titanates in decontamination of defense waste. Report RS-8232-2/50318. , (1978).</li><li>Sylvester, P., Clearfield, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+removal+of+strontium+from+simulated+Hanford+tank+wastes+containing+complexants.">The removal of strontium from simulated Hanford tank wastes containing complexants.</a> Sep. Sci. Technol. 34 (13), 2539-2551 (1999).</li><li>Manna, B., Dasgupta, M., Ghosh, U. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crystalline+hydrous+titanium(IV)+oxide+(CHTO):+an+arsenic(III)+scavenger+from+natural+water.">Crystalline hydrous titanium(IV) oxide (CHTO): an arsenic(III) scavenger from natural water.</a> J. Water Supply Res. T. 53, 483-495 (2004).</li><li>Elvington, M. C., Click, D. R., Hobbs, D. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Sorption+behavior+of+monosodium+titanate+and+amorphous+peroxotitanate+materials+under+weakly+acidic+conditions.">Sorption behavior of monosodium titanate and amorphous peroxotitanate materials under weakly acidic conditions.</a> Sep. Sci. Technol. 45 (1), 66-72 (2010).</li><li>Wataha, J. C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Titanates+deliver+metal+ions+to+human+monocytes.">Titanates deliver metal ions to human monocytes.</a> J. Mater. Sci.: Mater. Med. 21 (4), 1289-1295 (2010).</li><li>Chung, W. O., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Peroxotitanate-+and+monosodium+metal-titanate+compounds+as+inhibitors+of+bacterial+growth.">Peroxotitanate- and monosodium metal-titanate compounds as inhibitors of bacterial growth.</a> J. Biomed. Mater. Res., Part A. 97 (3), 348-354 (2011).</li><li>Hobbs, D. T., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Strontium+and+actinide+separations+from+high+level+nuclear+waste+solutions+using+monosodium+titanate+1.+Simulant+testing.">Strontium and actinide separations from high level nuclear waste solutions using monosodium titanate 1. Simulant testing.</a> Sep. Sci. Technol. 40 (15), 3093-3111 (2005).</li><li>Ramirez-Salgdo, J., Djrado, E., Fabry, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+sodium+titanate+composites+by+sol-gel+method+for+use+in+gas+potentiometric+sensors.">Synthesis of sodium titanate composites by sol-gel method for use in gas potentiometric sensors.</a> J. Eur. Ceram. Soc. 24 (8), 2477-2483 (2004).</li><li>Yang, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Study+on+composition,+structure+and+formation+process+of+nanotube+Na2Ti2O4(OH)2.">Study on composition, structure and formation process of nanotube Na2Ti2O4(OH)2.</a> Dalton Trans. 2003 (20), 3898-3901 (2003).</li><li>Chen, W., Guo, X., Zhang, S., Jin, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=TEM+study+on+the+formation+mechanism+of+sodium+titanate+nanotubes.">TEM study on the formation mechanism of sodium titanate nanotubes.</a> J. Nanopart. Res. 9 (6), 1173-1180 (2007).</li><li>Meng, X., Wang, D., Liu, J., Zhang, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+and+characterization+of+sodium+titanate+nanowires+from+brookite+nanocrystallites.">Preparation and characterization of sodium titanate nanowires from brookite nanocrystallites.</a> Mater. Res. Bull. 39 (14-15), 2163-2170 (2004).</li><li>Yada, M., Goto, Y., Uota, M., Torikai, T., Watari, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Layered+sodium+titanate+nanofiber+and+microsphere+synthesized+from+peroxotitanic+acid+solution.">Layered sodium titanate nanofiber and microsphere synthesized from peroxotitanic acid solution.</a> J. Eur. Ceram. Soc. 26 (4-5), 673-678 (2006).</li><li>Stewart, T. A., Nyman, M., deBoer, M. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Delaminated+titanate+and+peroxotitanate+photocatalysts.">Delaminated titanate and peroxotitanate photocatalysts.</a> Appl. Catal. B. 105 (1-2), 69-76 (2011).</li><li>Rejman, J., Oberle, V., Zuhorn, I. S., Hoekstra, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size-dependent+internalization+of+particles+via+the+pathways+of+clathrin-+and+caveolae-mediated+endocytosis.">Size-dependent internalization of particles via the pathways of clathrin- and caveolae-mediated endocytosis.</a> Biochem. J. 377 (1), 159-169 (2004).</li><li>Hobbs, D. T., Taylor-Pashow, K. M. L., Elvington, M. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Formation+of+nanosized+metal+particles+on+a+titanate+carrier.">Formation of nanosized metal particles on a titanate carrier.</a> US patent application. , (2015).</li><li>Elvington, M. C., Tosten, M., Taylor-Pashow, K. M. L., Hobbs, D. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+characterization+of+nanosize+sodium+titanates.">Synthesis and characterization of nanosize sodium titanates.</a> J. Nanopart. Res. 14, 1114 (2012).</li><li>Duff, M. C., Hunter, D. B., Hobbs, D. T., Fink, S. D., Dai, Z., Bradley, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanisms+of+strontium+and+uranium+removal+from+high-level+radioactive+waste+simulant+solutions+by+the+sorbent+monosodium+titanate.">Mechanisms of strontium and uranium removal from high-level radioactive waste simulant solutions by the sorbent monosodium titanate.</a> Environ. Sci. Technol. 38 (19), 5201-5207 (2004).</li><li>Puangpetch, T., Sreethawong, T., Chavadej, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+production+over+metal-loaded+mesoporous-assembled+SrTiO3+nanocrystal+photocatalysts:+effects+of+metal+type+and+loading.">Hydrogen production over metal-loaded mesoporous-assembled SrTiO3 nanocrystal photocatalysts: effects of metal type and loading.</a> Int. J. Hydrogen Energy. 35 (13), 6531-6540 (2010).</li><li>Fan, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Facile+method+to+synthesize+mesoporous+multimetal+oxides+(ATiO3,+A+=+Sr,+Ba)+with+large+specific+surface+areas+and+crystalline+pore+walls.">Facile method to synthesize mesoporous multimetal oxides (ATiO3, A = Sr, Ba) with large specific surface areas and crystalline pore walls.</a> Chem. Mater. 22 (4), 1276-1278 (2010).</li><li>Rossmanith, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Porous+anatase+nanoparticles+with+high+specific+area+prepared+by+miniemulsion+technique.">Porous anatase nanoparticles with high specific area prepared by miniemulsion technique.</a> Chem. Mater. 20 (18), 5768-5780 (2008).</li><li>Wu, Y., Zhang, Y., Xu, J., Chen, M., Wu, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One-step+preparation+of+PS/TiO2+nanocomposite+particles+via+miniemulsion+polymerization.">One-step preparation of PS/TiO2 nanocomposite particles via miniemulsion polymerization.</a> J. Colloid Interface Sci. 343 (1), 18-24 (2010).</li><li>Jiang, C., Ichihara, M., Honmaa, I., Zhou, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+particle+dispersion+on+high+rate+performance+of+nano-sized+Li4Ti5O12+anode.">Effect of particle dispersion on high rate performance of nano-sized Li4Ti5O12 anode.</a> Electrochim. Acta. 52 (23), 6470-6475 (2007).</li><li>Bouras, P., Stathatos, E., Lianos, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pure+versus+metal-ion-doped+nanocrystalline+titania+for+photocatalysis.">Pure versus metal-ion-doped nanocrystalline titania for photocatalysis.</a> Appl. Catal. B. 73 (1-2), 51-59 (2007).</li><li>Bonino, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ti-Peroxo+species+in+the+TS-1/H2O2/H2O+system.">Ti-Peroxo species in the TS-1/H2O2/H2O system.</a> J. Phys. Chem. B. 108 (11), 3573-3583 (2004).</li><li>Bordiga, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resonance+Raman+effects+in+TS-1:+the+structure+of+Ti(IV)+species+and+reactivity+towards+H2O,+NH3+and+H2O2:+an+in+situ+study.">Resonance Raman effects in TS-1: the structure of Ti(IV) species and reactivity towards H2O, NH3 and H2O2: an in situ study.</a> Phys. Chem. Chem. Phys. 2003 (5), 4390-4393 (2003).</li><li>Vacque, V., Sombret, B., Huvenne, J. P., Legrand, P., Suc, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+the+O-O+peroxide+band+by+vibrational+spectroscopy.">Characterization of the O-O peroxide band by vibrational spectroscopy.</a> Spectrochim. Acta Part A. 53 (1), 55-66 (1997).</li></ol>

The authors have nothing to disclose.

A presença de água estranha, por exemplo, a partir de reagentes impuros, podem alterar o resultado da reacção, levando a partículas maiores ou mais polidispersos. Portanto, devem ser tomados cuidados para assegurar reagentes secos são usados. O isopropóxido de titânio e metóxido de sódio deve ser armazenado num exsicador quando não estiver em uso. Alta pureza isopropanol também deve ser utilizado para a síntese. A temperatura foi encontrada a desempenhar um papel-chave na conver...

Dióxido de titânio e titanatos de metais alcalinos são amplamente utilizadas numa variedade de aplicações, tais como pigmentos em tinta e produtos de cuidados da pele e como fotocatalisadores de conversão de energia e a utilização. 1-3 titanatos de sódio têm mostrado ser eficazes para remover materiais uma gama de catiões sobre uma vasta gama de condições de pH, devido a reacções de permuta catiónica. 07/04 Para além das aplicações descritas acima, foram recentemente mostrado mícron de tamanho e os titanatos de sódio peroxotitanates de sódio para também servir como uma plataforma de entrega de metal terapêutico. Nesta aplicação, os iões metálicos terapêuticos, tais como Au (III), Au (I) e Pt (II) são trocados por iões de sódio de titanato de monossódio (MST). Testes in vitro com os titanatos permutados com metal nobre indicam supressão de o crescimento de cancro e as células bacterianas por um mecanismo desconhecido. 8,9 Historicamente, titanatos de sódio têm seren produzidos utilizando ambos de sol-gel e as técnicas de síntese hidrotermal resultando em pós finos com tamanhos de partícula que vão desde algumas centenas de microns para. 4,5,10,11 Mais recentemente, métodos sintéticos têm sido relatado que produziu nanosize dióxido de titânio, por metal óxidos de titânio dopado, e uma variedade de outros titanatos de metais. Exemplos incluem os nanotubos de sódio de óxido de titânio (ou nanofios NaTONT) por reacção de dióxido de titânio em excesso de hidróxido de sódio, à temperatura e pressão elevadas, de titanato de nanofibras 12-14 de sódio por reacção de ácido peroxotitanic com hidróxido de sódio em excesso, à temperatura e pressão elevadas, de 15 e de sódio e césio titanato de nanofibras por delaminação de titanatos micronizadas permutado com ácido. 16 A síntese de titanatos de sódio e nanosize peroxotitanates de sódio é de interesse para melhorar a cinética de troca de iões, que são normalmente controladas por difusão ou filme diffu intrapartículaSion. Estes mecanismos são largamente controlada pelo tamanho de partícula do permutador de iões. Além disso, como plataforma de administração de metal terapêutica, o tamanho de partícula do material de titanato seria de esperar que afectem significativamente a natureza da interacção entre o titanato permutado com metal e o cancro e as células bacterianas. Por exemplo, células bacterianas, que são tipicamente da ordem de 0,5-2 uM, teria provavelmente diferentes interacções com partículas de tamanho de micron em comparação com partículas nanométricas. Além disso, as células eucarióticas não fagocíticas foram mostrados para internalizar Somente as partículas com um tamanho inferior a 1 micron. 17 Assim, a síntese de titanatos de sódio de tamanho nanométrico é também de interesse para facilitar a entrega de metal e a incorporação celular da plataforma de entrega de titanato. A redução do tamanho de titanatos de sódio e peroxotitanates também irá aumentar a capacidade eficaz em separações de iões metálicos e melhorar as propriedades fotoquímicas do material. 16,18 &lt;/ sup&gt; Este documento descreve um protocolo desenvolvido para sintetizar nanosize monossódico titanato (nMST) em condições de sol-gel suaves 19 A preparação do peróxido correspondente modificado nMST.; juntamente com uma reacção de permuta de iões para carregar o nMST com Au (III) também são descritas.

<table><tbody><tr><td>Titanium(IV) isopropoxide</td><td>Sigma Aldrich</td><td>377996</td><td>99.999% trace metals basis</td></tr><tr><td>Isopropyl alcholol, 99.9%</td><td>Sigma Aldrich</td><td>650447</td><td>HPLC grade (Chomasolv)</td></tr><tr><td>Sodium methoxide in methanol</td><td>Sigma Aldrich</td><td>156256</td><td>25 wt%</td></tr><tr><td>Triton X-100</td><td>Sigma Aldrich</td><td>T9284</td><td>BioXtra</td></tr><tr><td>hydrogen tetrachloroaurate(III) trihydrate</td><td>Sigma Aldrich</td><td>G4022</td><td>ACS reagent grade</td></tr><tr><td>hydrogen peroxide (30&amp;nbsp;wt%)</td><td>Fisher</td><td>H325</td><td>Certified ACS</td></tr><tr><td>10-ml syringes</td><td>Fisher</td><td>14-823-16E</td><td></td></tr><tr><td>Dual channel syringe pump</td><td>Cole Parmer</td><td>EW-74900-10</td><td>Or equivalent programmable dual channel syringe pump</td></tr><tr><td>Tygon tubing 1/8 inch ID, 1/4 inch OD</td><td>Cole Parmer</td><td>EW-0640776</td><td></td></tr><tr><td>Tygon tubing 1/16 inch ID, 1/8 inch OD</td><td>Cole Parmer</td><td>EW-0740771</td><td></td></tr><tr><td>0.1-&amp;micro;m Nylon filter</td><td>Fisher</td><td>R01SP04700</td><td></td></tr><tr><td>Labquake shaker rotisserie</td><td>Thermo Scientific</td><td>4002110Q</td><td></td></tr></tbody></table>

synthesis and reaction chemistry of nanosize monosodium titanate

Este documento descreve a síntese e modificação de peróxido-titanato nanosize monossódico (nMST), juntamente com uma reacção de permuta de iões para carregar o material com iões Au (III). O método de síntese foi derivado a partir de um processo sol-gel utilizado para a produção de tamanho de micron monossódico titanato (MST), com várias modificações importantes, incluindo alterar as concentrações de reagentes, omitindo um passo partícula semente, e a introdução de um agente tensioactivo não iónico para facilitar o controlo de a formação de partículas e de crescimento. O material resultante nMST apresenta a morfologia das partículas de forma esférica com uma distribuição monodispersa de diâmetros de partículas no intervalo de 100 a 150 nm. O material nMST foi encontrada para ter uma área de superfície de Brunauer-Emmett-Teller (BET) de 285 m 2 g -1, o que é mais do que uma ordem de magnitude maior do que a MST de tamanho de micron. O ponto isoeléctrico da nMST medido 3,34 unidades de pH, o que é uma unidade de pH mais baixo do que o medido para a mícron de tamanho MST. Tele nMST material foi encontrado para servir como um permutador de iões eficaz sob condições fracamente ácidas para a preparação de uma Au (III) nanotitanato -Exchange. Além disso, a formação do correspondente peroxotitanate foi demonstrada por meio de reacção do nMST com peróxido de hidrogénio.

MST é sintetizada usando um método de sol-gel em que tetraisopropoxytitanium (IV) (TIPT), metóxido de sódio, e água são combinados e feitos reagir em isopropanol para formar partículas semente de MST. 4 partículas mícron de tamanho são então crescidas por adição controlada de adicional as quantidades dos reagentes. As partículas resultantes possuem um núcleo amorfo e uma região exterior fibrosa tendo dimensões de cerca de 10 nm de largura por 50 nm de comprimento 20. <p class="...

Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

Síntese e Reacção Química de nanosize monossódico Titanate

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the ...

synthesis-and-reaction-chemistry-of-nanosize-monosodium-titanate

Universidad de Cartagena UDEC

Research

Education

JoVE Core

JoVE Journal

Analytical Chemistry

Chemistry

Unit 1

Chemical Equilibria

SCIENTISTS IN ACTION

8.6K visualizações.  Savannah River Consulting, L.L.C.. The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

Vídeo: Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Química

Fabrication of Spatially Confined Complex Oxides

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from the inherent strong electron correlations that reside within them. These materials can also possess electronic phase separation in which regions of vastly different resistive and magnetic behavior can coexist within a single crystal alloy material. By reducing the scale of these materials to length scales at and below the inherent size of the electronic domains, novel behaviors can be exposed. Because of this and the fact that spin-charge-lattice-orbital order parameters each involve correlation lengths, spatially reducing these materials for transport measurements is a critical step in understanding the fundamental physics that drives complex behaviors. These materials also offer great potential to become the next generation of electronic devices 1-3. Thus, the fabrication of low dimensional nano- or micro-structures is extremely important to achieve new functionality. This involves multiple controllable processes from high quality thin film growth to accurate electronic property characterization. Here, we present fabrication protocols of high quality microstructures for complex oxide manganite devices. Detailed descriptions and required equipment of thin film growth, photo-lithography, and wire-bonding are presented.

We describe the use of pulsed laser deposition (PLD), photolithography and wire-bonding techniques to create micrometer scale complex oxides devices. The PLD is utilized to grow epitaxial thin films. Photolithography and wire-bonding techniques are introduced to create practical devices for measurement purposes.

Fabricação de óxidos complexos espacialmente confinados

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from ...

Engenharia

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

Templates atomicamente definidos para crescimento epitaxial do Complexo Óxido Filmes Finos

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and reduction half reactions, and fast electron (hole) diffusion and charge separation. Nanowires present suitable architectures to meet these requirements. Axially segmented Ag|ZnO and radially segmented (coaxial) TiO2-Ag nanowires with a diameter of 200 nm and a length of 6-20 &#181;m were made by templated electrodeposition within the pores of polycarbonate track-etched (PCTE) or anodized aluminum oxide (AAO) membranes, respectively. In the photocatalytic experiments, the ZnO and TiO2 phases acted as photoanodes, and Ag as cathode. No external circuit is needed to connect both electrodes, which is a key advantage over conventional photo-electrochemical cells. For making segmented Ag|ZnO nanowires, the Ag salt electrolyte was replaced after formation of the Ag segment to form a ZnO segment attached to the Ag segment. For making coaxial TiO2-Ag nanowires, a TiO2 gel was first formed by the electrochemically induced sol-gel method. Drying and thermal annealing of the as-formed TiO2 gel resulted in the formation of crystalline TiO2 nanotubes. A subsequent Ag electrodeposition step inside the TiO2 nanotubes resulted in formation of coaxial TiO2-Ag nanowires. Due to the combination of an n-type semiconductor (ZnO or TiO2) and a metal (Ag) within the same nanowire, a Schottky barrier was created at the interface between the phases. To demonstrate the photocatalytic activity of these nanowires, the Ag|ZnO nanowires were used in a photocatalytic experiment in which H2 gas was detected upon UV illumination of the nanowires dispersed in a methanol/water mixture. After 17 min&#160;of illumination, approximately 0.2 vol% H2 gas was detected from a suspension of ~0.1 g of Ag|ZnO nanowires in a 50 ml 80 vol% aqueous methanol solution.

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Procedures are outlined to prepare segmented and coaxial nanowires via templated electrodeposition in nanopores. As examples, segmented nanowires consisting of Ag and ZnO segments, and coaxial nanowires consisting of a TiO2 shell and a Ag core were made. The nanowires were used in photocatalytic hydrogen formation experiments.

Preparação e Utilização de fotocataliticamente atividade segmentada Ag | ZnO e Coaxial TiO<sub&gt; 2</sub&gt;-AG nanofios feitos por Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

Inversa Síntese mediada por Microemulsão de monometálicos e bimetálico precoce de Metais de Transição Carbide e nitreto Nanopartículas

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

Síntese e Caracterização de Fe-dopado alumino nanotubos com propriedades condutoras aprimorados Electron

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

In situ Síntese de Nanopartículas de Ouro sem agregação no espaço Interlayer de Layered titanato filmes transparentes

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The chemical bonding of particulate photocatalysts to supporting material surfaces is of great importance in engineering more efficient and practical photocatalytic structures. However, the influence of such chemical bonding on the optical and surface properties of the photocatalyst and thus its photocatalytic activity/reaction selectivity behavior has not been systematically studied. In this investigation, TiO2 has been supported on the surface of SiO2 by means of two different methods: (i) by the in situ formation of TiO2 in the presence of sand quartz via a sol-gel method employing tetrabutyl orthotitanium (TBOT); and (ii) by binding the commercial TiO2 powder to quartz on a surface silica gel layer formed from the reaction of quartz with tetraethylorthosilicate (TEOS). For comparison, TiO2 nanoparticles were also deposited on the surfaces of a more reactive SiO2 prepared by a hydrolysis-controlled sol-gel technique as well as through a sol-gel route from TiO2 and SiO2 precursors. The combination of TiO2 and SiO2, through interfacial Ti-O-Si bonds, was confirmed by FTIR spectroscopy and the photocatalytic activities of the obtained composites were tested for photocatalytic degradation of NO according to the ISO standard method (ISO 22197&#8722;1). The electron microscope images of the obtained materials showed that variable photocatalyst coverage of the support surface can successfully be achieved but the photocatalytic activity towards NO removal was found to be affected by the preparation method and the nitrate selectivity is adversely affected by Ti-O-Si bonding.

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The focus of the present work is to establish means to generate and quantify levels of Ti-O-Si linkages and to correlate these with the photocatalytic properties of the supported TiO2.

O efeito da Ligação Química Interfacial em Compósitos de TiO2-SiO2 em seu Desempenho Fotocatalítico de Redução de NOx

The chemical bonding of particulate photocatalysts to supporting material surfaces is of great importance in engineering more efficient and practical ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its well-balanced ferroelectricity, piezoelectricity, and dielectric constant. In addition, BT does not contain any toxic elements. Therefore, it is considered to be an eco-friendly material, which has attracted considerable interest as a replacement for lead zirconate titanate (PZT). However, bulk BT loses its ferroelectricity at approximately 130 &#176;C, thus, it cannot be used at high temperatures. Because of the growing demand for high-temperature ferroelectric materials, it is important to enhance the thermal stability of ferroelectricity in BT. In previous studies, strain originating from the lattice mismatch at hetero-interfaces has been used. However, the sample preparation in this approach requires complicated and expensive physical processes, which are undesirable for practical applications.
In this study, we propose a chemical synthesis of a porous material as an alternative means of introducing strain. We synthesized a porous BT thin film using a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles were used as an organic template. Through a series of studies, we clarified that the introduction of pores had a similar effect on distorting the BT crystal lattice, to that of a hetero-interface, leading to the enhancement and stabilization of ferroelectricity. Owing to its simplicity and cost effectiveness, this fabrication process has considerable advantages over conventional methods.

Here, we present a protocol for the synthesis of porous barium titanate (BaTiO3) thin film by a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles are used as an organic template.

Síntese química de película fina de titanato de bário porosa e estabilização térmica da fase ferroelétrica pela tensão induzida pela porosidade

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of Manganese(II) Acetylacetonate

For biomedical applications, metal oxide nanoparticles such as iron oxide and manganese oxide (MnO), have been used as biosensors and contrast agents in magnetic resonance imaging (MRI). While iron oxide nanoparticles provide constant negative contrast on MRI over typical experimental timeframes, MnO generates switchable positive contrast on MRI through dissolution of MnO to Mn2+ at low pH within cell endosomes to &#8216;turn ON&#8217; MRI contrast. This protocol describes a one-pot synthesis of MnO nanoparticles formed by thermal decomposition of manganese(II) acetylacetonate in oleylamine and dibenzyl ether. Although running the synthesis of MnO nanoparticles is simple, the initial experimental setup can be difficult to reproduce if detailed instructions are not provided. Thus, the glassware and tubing assembly is first thoroughly described to allow other investigators to easily reproduce the setup. The synthesis method incorporates a temperature controller to achieve automated and precise manipulation of the desired temperature profile, which will impact resulting nanoparticle size and chemistry. The thermal decomposition protocol can be readily adapted to generate other metal oxide nanoparticles (e.g., iron oxide) and to include alternative organic solvents and stabilizers (e.g., oleic acid). In addition, the ratio of organic solvent to stabilizer can be changed to further impact nanoparticle properties, which is shown herein. Synthesized MnO nanoparticles are characterized for morphology, size, bulk composition, and surface composition through transmission electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy, respectively. The MnO nanoparticles synthesized by this method will be hydrophobic and must be further manipulated through ligand exchange, polymeric encapsulation, or lipid capping to incorporate hydrophilic groups for interaction with biological fluids and tissues.

Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of ManganeseII Acetylacetonate

This protocol details a facile, one-pot synthesis of manganese oxide (MnO) nanoparticles by thermal decomposition of manganese(II) acetylacetonate in the presence of oleylamine and dibenzyl ether. MnO nanoparticles have been utilized in diverse applications including magnetic resonance imaging, biosensing, catalysis, batteries, and waste water treatment.

Síntese de Nanopartículas de Óxido de Manganês por Decomposição Térmica de Acetilado de Manganês(II) Acetillacetonato

For biomedical applications, metal oxide nanoparticles such as iron oxide and manganese oxide (MnO), have been used as biosensors and contrast agents in ...