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. סינתזה של Titanate ננו-גלוטמט (nMST) <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> הכן 10 מ&quot;ל של תמיסת # 1 על ידי הוספת 0.58 מ&quot;ל של תמיסת 25% WT נתרן methoxide כדי 7.62 מ&quot;ל של isopropanol ואחריו 1.8 מ&quot;ל של isopropoxide טיטניום. </li><li style=";text-align:right;direction:rtl"> הכן 10 מ&quot;ל של תמיסת # 2 על ידי הוספת 0.24 מ&quot;ל מים ultrapure כדי 9.76 מ&quot;ל של isopropanol. </li><li style=";text-align:right;direction:rtl"> להוסיף 280 מ&quot;ל של isopropanol בבקבוק תחתית עגולה 3-צוואר 500 מ&quot;ל, ואחריו 0.44 מ&quot;ל של טריטון X-100 (MW הממוצע: 625 ג &#39;/ mol). מערבבים את הפתרון גם עם בר ומערבבים מגנטי. </li><li style=";text-align:right;direction:rtl"> הכן משאבת מזרק ערוץ כפול כדי לספק פתרונות # 1 ו # 2 בשיעור של 0.333 מ&quot;ל / דקה. </li><li style=";text-align:right;direction:rtl"> פתרונות טענו # 1 ו # 2 לשתי מזרקים נפרדים של 10 מיליליטר מצויד עם אורך של צינורות שייאפשרו אספקת הפתרון מן מזרק המשאבה אל מתחת לרמת הפתרון בבקבוק התחתי העגול 500 המ&quot;ל. </li><li style=";text-align:right;direction:rtl"> תוך ערבוב, להוסיף את כל הפתרונות # 1 ו # 2 (10 מ&quot;ל כל אחד) על התגובה באמצעות משאבת מזרק מתוכנת בשלב 1.4. </li> &lt;li&gt; לאחר תוספת הושלמה, מכסה את הבקבוק את האש וממשיכים לטגן למשך 24 שעות ב RT. </li><li style=";text-align:right;direction:rtl"> מסיר את הפקק מעל הבקבוק ולחמם את תערובת התגובה ~ 82 ° C (isopropanol refluxing) עבור 45-90 דקות, ואחריו טיהור עם חנקן תוך שמירת חימום. כפי isopropanol הוא התאדה, מוסיפים מים ultrapure לסירוגין להחליף את isopropanol התאדו. </li><li style=";text-align:right;direction:rtl"> לאחר שרוב isopropanol התאדו ואת נפח המים הוסיף הוא כ 50 מ&quot;ל, להסיר את החום ולאפשר לתערובת התגובה להתקרר. </li><li style=";text-align:right;direction:rtl"> אסוף את המוצר על ידי סינון דרך נייר סינון ניילון 0.1 מיקרומטר, ולשטוף מספר פעמים עם מים כדי להסיר את פעילי שטח וכל isopropanol שיורית. אל תסנן ליובש. לאחר השטיפה הושלמה, להעביר את התערובת דלילה ממסנן לתוך בקבוק טרום שקל או בקבוקון, ולאחסן כמו slurry מימי. </li><li style=";text-align:right;direction:rtl"> קבע את התשואה על ידי קביעת מוצקי אחוז המשקל של התרחיף. ניתן לעשות זאת על ידי מדידת המשקל של aliquot שלאת התערובת דלילה לפני ואחרי הייבוש. </li></ol> 2. Au (III) יון Exchange <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> העבר 6.50 גרם של 4.23% WT סלארי nMST לצינור צנטריפוגות 50 מ&quot;ל. סכום זה עשוי להשתנות בהתאם על אחוזי המשקל בפועל של תרחיף nMST מיוצר צעד 1.10 לעיל, וקובע בשלב 1.11. </li><li style=";text-align:right;direction:rtl"> תשקול 0.0659 גרם של HAuCl 4 · 3H 2 O לתוך בקבוקון זכוכית 1-DRAM. היעד Ti: יחס מסת Au הוא 4: 1. </li><li style=";text-align:right;direction:rtl"> ממיסים את HAuCl 4 · 3H 2 O ב ~ 1 מ&quot;ל של מים, ולאחר מכן להעביר את צינור צנטריפוגות המכיל את nMST. יש לשטוף את פי בקבוקון כמה עם מים נוספים כדי להבטיח את כל 3H HAuCl 4 · 2 O מועבר בצינור צנטריפוגות המכיל את nMST. </li><li style=";text-align:right;direction:rtl"> לדלל את ההשעיה עם מים נוספים, לפי הצורך, כדי להביא את הנפח הכולל עד 11 מ&quot;ל. מקד ריכוז Au (III) סופי של כ 15 מ&quot;מ. </li><li style=";text-align:right;direction:rtl"> לעטוף את צינור צנטריפוגות בנייר לשמור על ההשעיה בחושך, גידולאז D נפילת ההשעיה על אסכלה שייקר למשך תקופה מינימאלית של 4 ימים. </li><li style=";text-align:right;direction:rtl"> אסוף את המוצר על ידי צנטריפוגה ב 3000 XG במשך 15 דקות על מנת לבודד את המוצקים. שטפו את מוצקים שלוש פעמים במים מזוקקים על ידי redispersing במים reisolate ידי צנטריפוגה ב 3000 XG במשך 15 דקות כדי להסיר כל Au unexchanged (III). </li><li style=";text-align:right;direction:rtl"> אחסן את המוצר הסופי או כקובץ השעיה מימייה ידי redispersing במים, או כמו לחות מוצקה באמצעות אחסון מהמים לשטוף הסופיים וסגירת הצינור. אחסן את המוצר בחושך. </li></ol> 3. הכנה של Peroxotitanate <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> העבר 5 גרם של תערובת נוזלית 9.8% WT של nMST בבקבוק קטן. </li><li style=";text-align:right;direction:rtl"> תשקול 0.154 גרם של 30% WT H 2 O 2 פתרון. היעד H 2 O 2: יחס טוחנת Ti הוא 0.25: 1. </li><li style=";text-align:right;direction:rtl"> תוך ערבוב ההשעיה nMST גם להוסיף את 0.154 גרם של H 2 O 2 פתרון טיפה חכם. עם H 2 O בנוסף 2, ההשעיה של WHIמוצקי te מייד הופכים צהובים. </li><li style=";text-align:right;direction:rtl"> לאחר התוספת השלימה לעורר את התגובה בטמפרטורת סביבה למשך 24 שעות. </li><li style=";text-align:right;direction:rtl"> אסוף את המוצר על ידי סינון דרך מסנן ניילון 0.1 מיקרומטר, ולשטוף מספר פעמים עם מים כדי להסיר כל H unreacted 2 O 2. אל תסנן ליובש. לאחר השטיפה הושלמה, להעביר את התערובת דלילה ממסנן לתוך בקבוק טרום שקל או בקבוקון, ולאחסן כמו slurry מימי. </li></ol>

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The authors have nothing to disclose.

הנוכחות של מים זרים, למשל מ ריאגנטים טמאים, יכולה לשנות את התוצאה של התגובה, מה שמוביל חלקיקי polydisperse גדולים או יותר. לכן, יש לנקוט זהירות כדי להבטיח מגיבים יבשים משמשים. טיטניום isopropoxide ונתרן methoxide צריך להיות מאוחסן בתוך תא ייבוש כאשר אינו בשימוש. isopropanol הטוהר הגבוה צריך...

Titanates תחמוצת טיטניום מתכת אלקלית נמצא בשימוש נרחב במגוון הרחב של יישומים כגון פיגמנטים של צבעים וחומרי טיפוח עור וכתוצאת photocatalysts בגיור וניצול אנרגיה. 1-3 titanates נתרן הוכח להיות חומרים יעילים להסרת מגוון של קטיונים על פני טווח רחב של מצבי pH באמצעות תגובות קטיוני. 4-7 בנוסף היישומים פשוט תאר, מיקרון בגודל titanates נתרן peroxotitanates נתרן לאחרונה הוכח גם לשמש פלטפורמת משלוח המתכת טיפולית. ביישום זה, יונים של מתכות טיפוליות כגון Au (III), Au (I), ו Pt (II) הם החליפו עבור יוני נתרן של titanate גלוטמט (MST). בדיקות במבחנה עם titanates מתכת-החליפו אצילי מצביעים דיכוי הצמיחה של תאים סרטניים או חיידקים ידי המנגנון ידוע. 8,9 מבחינה היסטורית, titanates נתרן יש להיותen מיוצר באמצעות טכניקות סינטטיות סול ג&#39;ל הידרותרמיות הן וכתוצאה מכך אבקות בסדר עם גדלים של חלקיקים הנעים בין כמה לכמה מאה מיקרונים. 4,5,10,11 לאחרונה, שיטות סינטטיות דווחו שייצרה תחמוצת טיטניום nanosize, חלקי מתכת תחמוצות טיטניום מסוממים, וכן מגוון של titanates מתכת האחרת. דוגמאות כולל צינורות תחמוצת טיטניום נתרן (NaTONT) או nanowires מתגובה של תחמוצת טיטניום ב סודיום הידרוקסיד עודף בטמפרטורה ולחץ גבוהים, 12-14 nanofibers titanate נתרן מתגובה של חומצת peroxotitanic עם סודיום הידרוקסיד עודף בטמפרטורה ולחץ גבוהים, 15 ונתרן ו nanofibers titanate צזיום ידי delamination של titanates חומצה החליפו מיקרון בגודל. 16 הסינתזה של titanates נתרן nanosize ונתרן peroxotitanates הוא עניין לשפר קינטיקה חילוף יונים, אשר נשלטים בדרך כלל על ידי דיפוזיה הסרט או diffu intraparticleשיאון. מנגנונים אלה נשלטים במידה רבה על ידי גודל החלקיקים של מחליפי יונים. בנוסף, כפלטפורמת משלוח המתכת טיפולית, גודל חלקיקים של חומר titanate יהיה צפוי להשפיע על אופי משמעותי של האינטראקציה בין titanate-החליף מתכת סרטן תאים חיידקיים. לדוגמא, תאים חיידקיים, שהן בדרך כלל בסדר גודל של 0.5 - 2 מיקרומטר, עלולים להביא אינטראקציות שונות עם חלקיקים בגודל מיקרון לעומת חלקיקי nanosized. בנוסף, תאי איקריוטיים הלא phagocytic הוכחו להפנים חלקיקים רק עם גודל של פחות מ 1 מיקרון. 17 לפיכך, הסינתזה של titanates נתרן nanosize היא גם עניין להקל משלוח מתכת ספיגה הסלולר מפלטפורמת משלוח titanate. הקטנת נתרן titanates ו peroxotitanates יהיה גם להגדיל את הקיבולת היעילה פרדות מתכת יונים לשפר תכונות פוטו של חומר. 16,18 &lt;/ sup&gt; מאמר זה מתאר פרוטוקול שפותח לסנתז titanate גלוטמט nanosize (nMST) בתנאים סול-ג&#39;ל עדין 19 הכנת מי המקביל שונה nMST.; יחד עם תגובת יון-חילופי לטעון את nMST עם Au (III) מתוארים גם.

<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

מאמר זה מתאר את הסינתיזה-שינוי חמצן של titanate גלוטמט nanosize (nMST), יחד עם תגובת יון-חילופי לטעון את החומר עם Au יונים (III). שיטת הסינתזה נגזרה תהליך סול ג&#39;ל המשמש לייצור titanate גלוטמט מיקרון בגודל (MST), עם כמה שינויים מרכזיים, ובם שינוי ריכוזים מגיבים, השמטת צעד זרע חלקיקים, החדרה פעילה שטח בלתי יוני כדי להקל את השליטה היווצרות וצמיחת חלקיקים. חומר nMST כתוצאת מפגין מורפולוגיה חלקיקים כדורית בצורה עם חלוקת monodisperse בקטרי חלקיקים נעו בין 100 ל 150 ננומטר. חומר nMST נמצא שטח פן Brunauer-אמט-טלר (BET) של 285 מ &#39;2 g -1, וזה יותר ממה בסדר גודל גבוה יותר מאשר MST בגודל מיקרון. הנקודה איזואלקטרית של nMST נמדד 3.34 יחידות pH, שהיא יחידה pH נמוך מזה שנמדד עבור בגודל מיקרון MST. Tהוא nMST החומר נמצא לשמש מחליף יונים יעיל בתנאים חומצי חלש עבור הכנת nanotitanate Au (III) -exchange. בנוסף, היווצרות של peroxotitanate המקביל הודגם על ידי תגובה של nMST עם מי חמצן.

MST הוא מסונתז באמצעות שיטת סול ג &#39;שבו tetraisopropoxytitanium (IV) (TIPT), נתרן methoxide, ומים משולבים והגיב ב isopropanol כדי ליצור חלקיקים זרע MST. 4 חלקיקים מיקרון בגודל אז מגדלים נשלט תוספת של נוספים כמויות של חומרים כימיים. החלקיקים כתוצאה כוללים ליבת אמורפי אזור סיבי חיצוני שיש ממד?...

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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.

כימית סינתזת תגובה של nanosize מונוסודיום Titanate

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

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8.6K Views.  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.

Video: 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.

הכנה של חלקיקי סיליקה באמצעות חומצה קטליזה בסיוע מיקרוגל

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

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.

המצאה של תחמוצות מורכבות מוקפות מרחבית

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

Engineering

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.

תבניות מוגדרות אטומי לEpitaxial צמיחה של תחמוצת המורכבת Thin Films

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.

אופן ההכנה ושימוש בPhotocatalytically פעיל מקוטע Ag | ZnO וקואקסיאלי טיו<sub&gt; 2</sub&gt;-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 ...

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.

סינתזה בתיווך Microemulsion הפוכה של monometallic ובי-המתכתי המוקדם מעבר מתכת קרביד ניטריד חלקיקים

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.

סינתזה ואפיון של Fe-מסומם aluminosilicate צינורות עם מאפייני מוליכות אלקטרונים משופרים

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.

באתרו הסינתזה של זהב חלקיקים ללא צבירה במרחב Interlayer של סרטים שקופים Titanate Layered

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.

ההשפעה של מליטה כימית interfacial ב TiO<sub&gt; 2</sub&gt; -SiO<sub&gt; 2</sub&gt; מרוכבים על הביצועים שלהם NOX photatalyalytic הפחתה

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.

סינתזה של נקבובי בריום חומצה טיטנית סרט דק וייצוב תרמי של שלב Ferroelectric על ידי זן נקבוביות-Induced

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.

סינתזה ננו-חלקיקים תחמוצת מנגן על ידי ריקבון תרמי של מנגן(II) אצטילאצט

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

כימית סינתזת תגובה של nanosize מונוסודיום Titanate

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