DOCSLIB.ORG

Continuous Flow Synthesis of ZSM-5 Zeolite on the Order of Seconds

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
Continuous Flow Synthesis of ZSM-5 Zeolite on the Order of Seconds Continuous flow synthesis of ZSM-5 zeolite on the order of seconds Zhendong Liua, Kotatsu Okabea, Chokkalingam Ananda, Yasuo Yonezawaa, Jie Zhua, Hiroki Yamadaa, Akira Endob, Yutaka Yanabac, Takeshi Yoshikawac, Koji Oharad, Tatsuya Okuboa, and Toru Wakiharaa,1 aDepartment of Chemical System Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656, Japan; bNational Institute of Advanced Industrial Science and Technology, Ibaraki 305-8565, Japan; cInstitute of Industrial Science, The University of Tokyo, 4-6-1 Komaba, Meguro-ku, Tokyo, 153-8505, Japan; and dJapan Synchrotron Radiation Research Institute/SPring-8, Kouto 1-1-1, Sayo-gun, Hyogo 679-5198, Japan Edited by Mark E. Davis, California Institute of Technology, Pasadena, CA, and approved November 8, 2016 (received for review September 23, 2016) The hydrothermal synthesis of zeolites carried out in batch reactors established (11–13). The ultrafast route on the order of minutes takes a time so long (typically, on the order of days) that the not only enabled the continuous flow synthesis but also demon- crystallization of zeolites has long been believed to be very slow strated that the crystallization of zeolites can proceed much faster in nature. We herein present a synthetic process for ZSM-5, an than generally observed. industrially important zeolite, on the order of seconds in a contin- Owing to specific physical and chemical properties, supercritical uous flow reactor using pressurized hot water as a heating medium. water or pressurized water with extremely high temperatures Direct mixing of a well-tuned precursor (90 °C) with the pressurized (usually near or above 300 °C) offers several potential advantages water preheated to extremely high temperature (370 °C) in the mil- for hydrothermal processing (14). Continuous flow hydrothermal limeter-sized continuous flow reactor resulted in immediate heating synthesis of functional nanostructured materials in those mediums to high temperatures (240–300 °C); consequently, the crystallization has been extensively exploited in recent years, and the associated of ZSM-5 in a seed-free system proceeded to completion within tens merits, such as rapid formation of crystalline materials and facile of or even several seconds. These results indicate that the crystalli- tuning of the properties, have been demonstrated (15, 16). The zation of zeolites can complete in a period on the order of seconds. hydrothermal synthesis of zeolites using supercritical water or The subtle design combining a continuous flow reactor with pres- pressurized water with extremely high temperatures, however, surized hot water can greatly facilitate the mass production of zeo- has rarely been reported. The challenge arises from the intrinsic lites in the future. complexity of zeolite formation. Zeolites are formed as a metastable phase compared with their dense-phase counterparts, which implies crystal growth | continuous flow synthesis | zeolites | ultrafast synthesis | that overly high temperatures may only lead to the formation of ZSM-5 nonporous materials (17, 18). Meanwhile, the complicated assembly of inorganic–organic species leading to the formation of zeolites eolites have typically been synthesized via hydrothermal may not be favored under the less hydrophilic conditions of water Ztreatment, a process designed to artificially mimic the geo- with too high temperatures (19). Finally, the organic structure- logical formation conditions of natural zeolites (1, 2). Depending directing agent (OSDA) tends to decompose at high temperatures, on the targeted framework and composition, several hours to days which imposes further restrictions (20). To realize a synthesis in (or even several weeks) are required to complete the synthesis of a such environments, it is of paramount importance that the crystal- crystalline product (3). As a great improvement over the hundreds lization of the target phase should be completed before the for- or thousands of years required for the formation of natural zeolites, mation of a dense phase as well as the complete decomposition artificial synthesis on the order of days allows us more opportu- of OSDA. nities to obtain zeolites with tunable properties (4, 5). Nevertheless, the hydrothermal synthesis of zeolites has remained a time-con- Significance suming process. Long periods of hydrothermal treatment, for one thing, cause a burden on both energy efficiency and operational costs. Furthermore, pressure-tight vessels used for the hydrother- Zeolites have greatly contributedtomodernindustries.Con- mal treatment as well as harsh conditions therein make mechanistic sumption of zeolites is expected to increase with the emergence studies using in situ techniques difficult to perform (6, 7). The of newly commercialized applications. Typical synthesis of zeo- complexity of crystallization, in turn, hinders the attempts at short- lites relies on batchwise hydrothermal synthesis, which usually takes tens of hours or even several days to complete. People have ening the synthesis period. This dilemma explains to some extent the thus long believed that the crystallization of zeolites is very slow reason behind the long-held belief that crystallization of zeolites is in nature. We herein demonstrate the continuous flow synthesis extremely slow in nature. of ZSM-5, an industrially important zeolite, on the order of sec- The other major hurdle for the widespread application of zeolites onds. Crystallization from amorphous state to full crystallinity is the difficulty in mass production. Batchwise synthesis using au- could be completed in tens of or even several seconds. The syn- toclaves is convenient for basic laboratory investigations but poses thesis on the order of seconds provides a great potential to fa- several challenges––in terms of economic efficiency, quality control, –– cilitate the mass production as well as to deepen the fundamental and operation flexibility when large-scale manufacturing is con- understanding of zeolite crystallization. sidered (8). In contrast, continuous flow process has proved to be ENGINEERING beneficial in the production of various chemicals (9, 10). Due to the Author contributions: T.W. designed research; Z.L., K. Okabe, C.A., Y. Yonezawa, and J.Z. time-consuming hydrothermal treatment used for the synthesis of performed research; A.E., Y. Yanaba, T.Y., and K. Ohara contributed new reagents/analytic zeolites, however, making a direct switch from batchwise synthesis tools; Z.L., H.Y., T.O., and T.W. analyzed data; and Z.L., T.O., and T.W. wrote the paper. to continuous flow manufacturing is not easy. To realize continuous The authors declare no conflict of interest. flow production, shortening the synthesis period is therefore an This article is a PNAS Direct Submission. issue of the highest priority. Recently, we have developed an Freely available online through the PNAS open access option. ultrafast route to synthesize industrially important zeolitic materials 1To whom correspondence should be addressed. Email: [email protected]. on the order of minutes (e.g., 10 min for aluminosilicate SSZ-13), This article contains supporting information online at www.pnas.org/lookup/suppl/doi:10. based on which the continuous flow synthesis was successfully 1073/pnas.1615872113/-/DCSupplemental. www.pnas.org/cgi/doi/10.1073/pnas.1615872113 PNAS | December 13, 2016 | vol. 113 | no. 50 | 14267–14271 Downloaded by guest on September 29, 2021 detailed explanation of the HEXTS results, see Fig. S3). The Si/Al ratio of the product, analyzed by inductively coupled plasma– atomic emission spectrometer (ICP-AES), was 105, which is sim- ilar to that of the reference ZSM-5 (with a Si/Al ratio of 108). The micropore volumes for both products were also comparable (0.128 and 0.124 cm3/g for the product synthesized in 6 s and the refer- ence ZSM-5, respectively; Fig. 3B). A stable hydrodynamic condition was maintained in the con- tinuous flow synthesis, as indicated by the temperature and pres- sure profiles (Fig. S1). Hydrodynamic failure is one of the main Fig. 1. Flowchart for the continuous flow synthesis of ZSM-5 on the order obstacles for the continuous flow synthesis involving solid reactants of seconds. and/or products. Continuous production having a high solid con- tent is susceptible to hydrodynamic failure caused by constriction, We present herein a continuous flow method for the synthesis bridging, and random detachment of solid particles (23). In our of ZSM-5 using pressurized hot water with extremely high tem- case, the solid content in the synthesis mixture was significantly perature (370 °C) as the heating medium. ZSM-5 is an alumi- high even in the presence of pressurized hot water. Despite a high nosilicate zeolite with intensive industrial applications (21, 22), solid content, the compressed-air-driven vibrator, as sketched in yet typically its synthesis consumes tens of hours. In this work, we Fig. 1, proved to be a powerful technique, which can be easily demonstrate that the direct mixing of synthesis precursor and the incorporated, to minimize precipitation or blockage problems. pressurized hot water in a millimeter-sized continuous flow reactor The ultrashort synthesis period required for complete crystalli- could result in immediate heating up to high temperatures (Fig. 1; zation also helped prevent hydrodynamic failure. The yields for for details of the continuous flow reactor see Fig. S1); conse- the continuous flow synthesis are shown in Fig. S4, which dem- quently,
Load more

Recommended publications
  • Conventional and Microwave Hydrothermal Synthesis and Application of Functional Materials: a Review
    materials Review Conventional and Microwave Hydrothermal Synthesis and Application of Functional Materials: A Review Guijun Yang and Soo-Jin Park * Department of Chemistry, Inha University, 100 Inharo, Incheon 402-751, Korea; [email protected] * Correspondence: [email protected]; Tel.: +82-32-876-7234 Received: 5 March 2019; Accepted: 9 April 2019; Published: 11 April 2019 Abstract: With the continuous development and progress of materials science, increasingly more attention has been paid to the new technology of powder synthesis and material preparation. The hydrothermal method is a promising liquid phase preparation technology that has developed rapidly during recent years. It is widely used in many fields, such as the piezoelectric, ferroelectric, ceramic powder, and oxide film fields. The hydrothermal method has resulted in many new methods during the long-term research process, such as adding other force fields to the hydrothermal condition reaction system. These force fields mainly include direct current, electric, magnetic (autoclaves composed of non-ferroelectric materials), and microwave fields. Among them, the microwave hydrothermal method, as an extension of the hydrothermal reaction, cleverly uses the microwave temperature to compensate for the lack of temperature in the hydrothermal method, allowing better practical application. This paper reviews the development of the hydrothermal and microwave hydrothermal methods, introduces their reaction mechanisms, and focuses on the practical application of the two methods. Keywords: hydrothermal method; microwave hydrothermal method; functional materials; application 1. Introduction During the process of continuous development of materials science, the research and development of new processes for material preparation and synthesis has always been an important part. For a long time, researchers have been searching for a material synthesis method with limited pollution, easy operation, excellent product performance, and low production cost [1–3].
    [Show full text]
  • The 3 Hours-Hydrothermal Synthesis of High Surface Area Superparamagnetic Fe3o4 Core-Shell Nanoparticles (Esty Octiana Sari)
    The 3 Hours-Hydrothermal Synthesis of High Surface Area Superparamagnetic Fe3O4 Core-Shell Nanoparticles (Esty Octiana Sari) THE 3 HOURS-HYDROTHERMAL SYNTHESIS OF HIGH SURFACE AREA SUPERPARAMAGNETIC Fe3O4 CORE-SHELL NANOPARTICLES Esty Octiana Sari,Ahmad Fadli andAmunAmri Department of Chemical Engineering Riau University Jl. HR Subrantas KM 12,5 Panam, Pekanbaru 28293, Riau E-mail: [email protected] Received: 2 May 2017 Revised: 27 September 2017 Accepted: 4 October 2017 ABSTRACT THE 3 HOURS-HYDROTHERMAL SYNTHESIS OF HIGH SURFACE AREA SUPERPARAMAGNETIC Fe3O4 CORE-SHELL NANOPARTICLES. The monodisperse core-shell Fe3O4 nanoparticles have been successfully synthesized by short times (3 hours) hydrothermal method at 220 oC from FeCl3, citrate, urea and PEG.The as-synthesized samples have been characterized using X-Ray Diffraction (XRD), Transmission Electron Microscope (TEM), Bruneur-Emmet-Teller (BET) surface area analyzer, and Vibrating Sample Magnetometer (VSM). The XRD result shows the as-synthesized products are pure Fe3O4. The TEM image shows the magnetite nanoparticles have monodisperse core-shell shape. The BET result shows the magnetite nanoparticles have 650.757 m2/g surface area. The hysteresis curve shows the magnetite nanoparticles exhibit super paramagnetic properties. This simple method obtained 60 nm core-shell Fe3O4 particles with super paramagnetic, high surface area as well as hydrophilic properties. Those properties are promising for various biomedical application. The advantages of simple and short times methods with high quality of product make this method very promising to be applied. Keywords: Core-shell, Hydrothermal method, Superparamagnetic, Nanoparticles ABSTRAK 3 JAM-SINTETIS HIDROTERMALNANOPARTIKELCORE-SHELLSUPERPARAMAGNETIK Fe3O4 DENGAN LUAS PERMUKAAN TINGGI. Nanopartikel monodispersi Fe3O4 berbentuk core-shell o telah berhasil disintesis dengan metode hidrothermal waktu singkat (3 jam) pada suhu 220 C dari FeCl3, sitrat, urea dan PEG.
    [Show full text]
  • V.Lelting and Transformation Remperatures of Mineral and \Llied Substances
    v.lelting and Transformation remperatures of Mineral and \llied Substances I F. c. KRACEK ONTRIBUTIONS TO GEOCHEMISTRY EOLOGICAL SURVEY BULLETIN 1144-D HTED STATES GOVERNMENT PRINTING OFFICE, WASHINGTON : 1963 UNITED STATES DEPARTMENT OF THE INTERIOR STEWART L. UDALL, Secretary GEOLOGICAL SURVEY Thomas B. Nolan, Director For sale by the Superintendent of Documents, U.S. Government Printing Office Washington, D.C. 20402 CONTENTS Page Abstract~------------------------------------------------------- 1 General discussion----------------------------------------------- 1 Acknowledgments____________________________________________ 3 General references _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ 3 Elements ------------------------------------------------------- 4 Oxides---------------------------------------------------------- 10 Oxide systems involving A120 3 ------------------------------------ 13 Oxide systems exclusive of Al2o3• B 2o 3, Si02 --------------------- 14 Silicate systems, binary__________________________________________ 17 Silicate systems, ternary _________________________________________ 21 Silicate systems, quaternary and higher ________ ----- _______________ 30 Silicate systems, miscellaneous ___________________________________ 32 Carbonates------------------------------------------------------ 33 Systems, miscellaneous __________________________________________ 36 References------------------------------------------------------ 63 ILLUSTRATIONS Figure 1. The system FeO --------------------------------------
    [Show full text]
  • Transfers Young, Stephanie Lynne, Chalfont St
    The Journal of Gemmology2010 / Volume 32 / Nos. 1–4 The Gemmological Association of Great Britain The Journal of Gemmology / 2009 / Volume 31 / No. 5–8 The Gemmological Association of Great Britain 27 Greville Street, London EC1N 8TN T: +44 (0)20 7404 3334 F: +44 (0)20 7404 8843 E: [email protected] W: www.gem-a.com Registered Charity No. 1109555 Registered office: Palladium House, 1–4 Argyll Street, London W1F 7LD President: Prof. A. H. Rankin Vice-Presidents: N. W. Deeks, R. A. Howie, E. A. Jobbins, M. J. O'Donoghue Honorary Fellows: R. A. Howie Honorary Life Members: H. Bank, D. J. Callaghan, T. M. J. Davidson, J. S. Harris, E. A. Jobbins, J. I. Koivula, M. J. O'Donoghue, C. M. Ou Yang, E. Stern, I. Thomson, V. P. Watson, C. H. Winter Chief Executive Officer: J. M. Ogden Council: J. Riley – Chairman, A. T. Collins, S. Collins, B. Jackson, C. J. E. Oldershaw, L. Palmer, R. M. Slater Members’ Audit Committee: A. J. Allnutt, P. Dwyer-Hickey, J. Greatwood, G. M. Green, J. Kalischer Branch Chairmen: Midlands – P. Phillips, North East – M. Houghton, North West – J. Riley, Scottish – B. Jackson, South East – V. Wetten, South West – R. M. Slater The Journal of Gemmology Editor: Dr R. R. Harding Assistant Editor: M. J. O’Donoghue Associate Editors: Dr A. J. Allnutt (Chislehurst), Dr C. E. S. Arps (Leiden), G. Bosshart (Horgen), Prof. A. T. Collins (London), J. Finlayson (Stoke on Trent), Dr J. W. Harris (Glasgow), Prof. R. A. Howie (Derbyshire), E. A. Jobbins (Caterham), Dr J.
    [Show full text]
  • Synthetic Quartz Crystal
    Synthetic Quartz Crystal n Terms and Definitions Synthetic Quartz Crystal: A single crystal grown using the Right-handed and left-handed quartz crystals: Crystals are hydrothermal synthesis method. divided into two types: right-handed and left-handed. A As-Grown Quartz Crystal: A synthetic quartz crystal grown difference in optical rotation creates the 2 types, but their naturally with no processing. physical properties are identical. Therefore, by cutting at the Lumbered Quartz Crystal: A synthetic quartz crystal with the X correct angle, the difference does not affect the characteristics and Z surfaces processed according to specified dimensions of a crystal oscillator. Generally right-handed quartz crystals are and angles using a diamond wheel #80. used in manufacture. Y-bar Synthetic Quartz Crystal: A synthetic quartz crystal grown Zone: A zone with a crystal that has grown from a seed crystal at by using a bar-like seed crystal elongated in the Y-axis direction. its core. There are Z, +X, -X, and S zones. Z-plate Synthetic Quartz Crystal: A synthetic quartz crystal Infrared Absorption Coefficient α: This value measured with an grown by using a plate-like seed crystal with a Y-axis direction infrared spectrophotometer is adopted as the infrared absorption length and X-axis direction width. coefficient α of a synthetic quartz crystal. The value is based on Inclusion: A general term for solid constituents (inclusions) that the absorption characteristic of the OH radical of a synthetic exist in synthetic quartz crystal; they can be observed when light quartz crystal that is around 3,800 to 3,000 cm–1 of the infrared is scattered through a liquid with a refractive index that is close transmittance curve.
    [Show full text]
  • Large-Scale Synthesis Route of Tio2 Nanomaterials with Controlled Morphologies Using Hydrothermal Method and Tio2 Aggregates As Precursor
    nanomaterials Article Large-Scale Synthesis Route of TiO2 Nanomaterials with Controlled Morphologies Using Hydrothermal Method and TiO2 Aggregates as Precursor Wenpo Luo 1 and Abdelhafed Taleb 1,2,* 1 Institut de Recherche de Chimie Paris, PSL Research University Chimie ParisTech—CNRS, 75005 Paris, France; [email protected] 2 Sorbonne Université, 75231 Paris, France * Correspondence: [email protected]; Tel.: +33-1-85-78-41-97 Abstract: TiO2 of controlled morphologies have been successfully prepared hydrothermally using TiO2 aggregates of different sizes. Different techniques were used to characterize the prepared TiO2 powder such as XRD, XPS, FEGSEM, EDS, and HRTEM. It was illustrated that the prepared TiO2 powders are of high crystallinity with different morphologies such as nanobelt, nanourchin, and nanotube depending on the synthesis conditions of temperature, time, and additives. The mechanism behind the formation of prepared morphologies is proposed involving nanosheet intermediate formation. Furthermore, it was found that the nanoparticle properties were governed by those of TiO2 nanoparticles aggregate used as a precursor. For example, the size of prepared nanobelts was proven to be influenced by the aggregates size used as a precursor for the synthesis. Keywords: TiO2 nanoparticles; aggregates; morphologies Citation: Luo, W.; Taleb, A. Large-Scale Synthesis Route of TiO2 Nanomaterials with Controlled Morphologies Using Hydrothermal 1. Introduction Method and TiO2 Aggregates as Recently, tremendous efforts have been devoted to developing innovative strategies Precursor. Nanomaterials 2021, 11, 365. to synthesize nanomaterials with the desired morphologies and properties. Particularly https://doi.org/10.3390/ the one-dimensional (1D) structure of TiO2 nanomaterials exhibits interesting properties nano11020365 compared to other TiO2 nanoparticles: it has lower carrier recombination rate and higher charge carrier mobility, thanks to the grain boundaries and junctions absence.
    [Show full text]
  • Module 8 Unit-3 NSNT Hydrothermal Synthesis Hydrothermal
    Module 8_Unit-3_NSNT Hydrothermal Synthesis Hydrothermal processing has gained much interest for synthesizing advanced nanomaterials as well as composites exhibiting tailored properties. This technique has been used to produce nanostructured materials for a broad range of applications which include electronics and optoelectronic devices, catalysis, biomedicine, biophotonics, etc. The word ‘hydrothermal’ has its origin in geology and Sir Roderick Murchison, a British geologist, was the first to use it. He attributed the variations in earth’s crust and the subsequent forming rocks as well as minerals to hydrothermal action of water at very high temperatures and pressures. Incidentally, the largest naturally occurring single crystal (beryl crystal, more than 1kg), as well as the largest man-made single crystal (quartz crystal, of several kgs), both have originated via hydrothermal process [1-2]. Hydrothermal synthesis belongs to a group of syntheses techniques in which substances in high- temperature and high pressure aqueous solution are crystallized. This is also called as the “hydrothermal method” [1]. According to Byrappa [3], hydrothermal processing is “any heterogeneous chemical reaction in the presence of a solvent (aqueous or non-aqueous) above room temperature and at pressures > 1 atm in a closed system” [2]. Hydrothermal processing includes techniques such as hydrothermal synthesis, hydrothermal crystal growth, hydrothermal transformation, hydrothermal sintering, etc. Hydrothermal processing of nanomaterials yields highly pure, homogenous, symmetrical crystal structures having novel properties. It also allows greater size control, low temperature synthesis, more control over composition of the end product, dense compounds, and can be used to produce compounds in relatively short time durations. Hydrothermal is a solution processing technique which involves processing of super heated aqueous solutions.
    [Show full text]
  • Hydrothermal Synthesis and Characterization of Cucro2 Laminar
    ARTICLE IN PRESS Journal of Crystal Growth 310 (2008) 5375–5379 Contents lists available at ScienceDirect Journal of Crystal Growth journal homepage: www.elsevier.com/locate/jcrysgro Hydrothermal synthesis and characterization of CuCrO2 laminar nanocrystals Shu Zhou a, Xiaodong Fang a,Ã, Zanhong Deng a,DaLia, Weiwei Dong a, Ruhua Tao a, Gang Meng a, Tao Wang a, Xuebin Zhu b a Anhui Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Hefei 230031, People’s Republic of China b Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, Hefei 230031, People’s Republic of China article info abstract Article history: CuCrO2 laminar nanocrystals were successfully synthesized by a simple hydrothermal technique. The Received 15 July 2008 nanocrystals have a quasi-hexagonal shape with a wide range of size distribution varying from about 10 Received in revised form to 80 nm and thickness less than 10 nm. The results of selected-area electron diffraction (SAED) data and 19 September 2008 high-resolution transmission electron microscopy (HRTEM) indicate the formation of well-formulated, Accepted 24 September 2008 single-crystal CuCrO . The dominant growth of nuclei is driven along the faces of {0 1 2}, and the growth Communicated by H. Fujioka 2 Available online 14 October 2008 along the c-axis is very slow, which directly results in the formation of CuCrO2 laminar nanocrystals. Optical properties of CuCrO2 laminar nanocrystals were investigated by UV–vis–Nis absorption PACS: spectrum, and direct bandgap was estimated to be 2.95 eV. 61.46.Df & 2008 Elsevier B.V.
    [Show full text]
  • Compilation of Crystal Growers and Crystal Growth Projects Research Materials Information Center
    ' iW it( 1 ' ; cfrv-'V-'T-'X;^ » I V' 1l1 II V/ f ,! T-'* «( V'^/ l "3 ' lyJ I »t ; I« H1 V't fl"j I» I r^fS' ^SllMS^W'/r V '^Wl/ '/-D I'ril £! ^ - ' lU.S„AT(yMIC-ENERGY COMMISSION , : * W ! . 1 I i ! / " n \ V •i" "4! ) U vl'i < > •^ni,' 4 Uo I 1 \ , J* > ' . , ' ^ * >- ' y. V * / 1 \ ' ' i S •>« \ % 3"*V A, 'M . •. X * ^ «W \ 4 N / . I < - Vl * b >, 4 f » ' ->" ' , \ .. _../.. ~... / -" ' - • «.'_ " . Ife .. -' < p / Jd <2- ORNL-RMIC-12 THIS DOCUMENT CONFIRMED AS UNCLASSIFIED DIVISION OF CLASSIFICATION COMPILATION OF CRYSTAL GROWERS AND CRYSTAL GROWTH PROJECTS RESEARCH MATERIALS INFORMATION CENTER \i J>*\,skJ if Printed in the United States of America. Available from National Technical Information Service U.S. Department of Commerce 5285 Port Royal Road, Springfield, Virginia 22t51 Price: Printed Copy $3.00; Microfiche $0.95 This report was prepared as an account of work sponsored by the United States Government. Neither the United States nor the United States Atomic Energy Commission, nor any of their employees, nor any of their contractors, subcontractors, or their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness or usefulness of any information, apparatus, product or process disclosed, or represents that its use would not infringe privately owned rights. ORNL-RMIC-12 UC-25 - Metals, Ceramics, and Materials Contract No. W-7405-eng-26 COMPILATION OF CRYSTAL GROWERS AND CRYSTAL GROWTH PROJECTS T. F. Connolly Research Materials Information Center Solid State Division NOTICE This report was prepared as an account of work sponsored by the Unitsd States Government.
    [Show full text]
  • Hydrothermal Synthesis Study
    Advances in Science and Technology Vol. 45 (2006) pp. 184-193 online at http://www.scientific.net © (2006) Trans Tech Publications, Switzerland Hydrothermal Synthesis of Advanced Ceramic Powders Wojciech L. Suchanek1, a and Richard E. Riman2, b 1Sawyer Technical Materials, LLC, 35400 Lakeland Boulevard, Eastlake, OH 44095, USA 2Rutgers University, Department of Materials Science and Engineering, 607 Taylor Road, Piscataway, NJ 08855, USA [email protected], [email protected] Keywords: Hydrothermal synthesis, review powder synthesis, morphology control, hydroxyapatite, PZT, alumina, zinc oxide, carbon nanotubes. Abstract. This paper briefly reviews hydrothermal synthesis of ceramic powders and shows how understanding the underlying physico-chemical processes occurring in the aqueous solution can be used for engineering hydrothermal crystallization processes. Our overview covers the current status of hydrothermal technology for inorganic powders with respect to types of materials prepared, ability to control the process, and use in commercial manufacturing. General discussion is supported with specific examples derived from our own research (hydroxyapatite, PZT, Į-Al2O3, ZnO, carbon nanotubes). Hydrothermal crystallization processes afford excellent control of morphology (e.g., spherical, cubic, fibrous, and plate-like) size (from a couple of nanometers to tens of microns), and degree of agglomeration. These characteristics can be controlled in wide ranges using thermodynamic variables, such as reaction temperature, types and concentrations of the reactants, in addition to non-thermodynamic (kinetic) variables, such as stirring speed. Moreover, the chemical composition of the powders can be easily controlled from the perspective of stoichiometry and formation of solid solutions. Finally, hydrothermal technology affords the ability to achieve cost effective scale-up and commercial production.
    [Show full text]
  • Fast Crystallization of SUZ-4 Zeolite with Hydrothermal Synthesis: Part I Temperature and Time Effect
    AvailableAvailable online online at www.sciencedirect.com at www.sciencedirect.com Procedia Engineering ProcediaProcedia Engineering Engineering 00 (2012) 32 (2012)000–000 198 – 204 www.elsevier.com/locate/procedia I-SEEC2011 Fast Crystallization of SUZ-4 Zeolite with Hydrothermal Synthesis: Part I Temperature and Time Effect P. Vongvoradit and P. Worathanakul∗ Department of Chemical engineering, Faculty of Engineering, King Mongkut’s University of Technology North Bangkok, Bangkok, 10800, Thailand Elsevier use only: Received 30 September 2011; Revised 10 November 2011; Accepted 25 November 2011. Abstract SUZ-4 zeolites were synthesized by hydrothermal technique under autogenous pressure with SiO2:Al2O3 ratio of 21.22 using silica-sol and tetraethlyammonium hydroxide as a silica source and a template, respectively. Effect of temperature with 150, 165, and 180°C and crystallization time with 24, 18, and 12 h were studied to obtain the suitable conditions at crystallization. SUZ-4 zeolite synthesis using short time compared to the conventional method was successful synthesized. The synthesized SUZ-4 zeolites were characterized using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), BET-N2 adsorption, and X-ray fluorescence (XRF). The results show that SUZ-4 zeolite was obtained from rapid crystallization having a narrow pore size distribution and needle-shaped crystals. Highly crystallined SUZ-4 depended on enhanced temperature and time of crystallization conditions. © 2010 Published by Elsevier Ltd. Selection and/or peer-review under responsibility of I-SEEC2011 Keywords: SUZ-4 zeolite; hydrothermal synthesis; needle-shaped; fast crystallization 1. Introduction Zeolite is a crystalline aluminosilicate with a three-dimensional framework structure that forms uniformly sized pores of molecular dimensions.
    [Show full text]
  • And One-Dimensional Titanium Oxide-Based Nano-Photocatalysts Dimitrios Giannakoudakis, Gregory Chatel, Juan Carlos Colmenares
    Mechanochemical Forces as a Synthetic Tool for Zero- and One-Dimensional Titanium Oxide-Based Nano-photocatalysts Dimitrios Giannakoudakis, Gregory Chatel, Juan Carlos Colmenares To cite this version: Dimitrios Giannakoudakis, Gregory Chatel, Juan Carlos Colmenares. Mechanochemical Forces as a Synthetic Tool for Zero- and One-Dimensional Titanium Oxide-Based Nano-photocatalysts. Topics in current chemistry, Springer, 2020, 378 (1), 10.1007/s41061-019-0262-3. hal-02378286 HAL Id: hal-02378286 https://hal.archives-ouvertes.fr/hal-02378286 Submitted on 25 Nov 2019 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Topics in Current Chemistry (2020) 378:2 https://doi.org/10.1007/s41061-019-0262-3 REVIEW Mechanochemical Forces as a Synthetic Tool for Zero‑ and One‑Dimensional Titanium Oxide‑Based Nano‑photocatalysts Dimitrios A. Giannakoudakis1 · Gregory Chatel2 · Juan Carlos Colmenares1 Received: 30 July 2019 / Accepted: 22 October 2019 © The Author(s) 2019 Abstract A new feld where the utilization of mechanochemistry can create new opportunities is materials chemistry, and, more interestingly, the synthesis of novel nanomateri- als. Ball-milling procedures and ultrasonic techniques can be regarded as the most important mechanochemical synthetic tools, since they can act as attractive alterna- tives to the conventional methods.
    [Show full text]