Name: generation of zerovalent metal core nanoparticles using n-(2-aminoethyl)-3-aminosilanetriol
Uploaded: 2016-02-11T13:00:00
Description: Watch this Scientific Journal Video about Generation of Zerovalent Metal Core Nanoparticles Using n-2-aminoethyl-3-aminosilanetriol at JoVE.com

Dr. B.P.S. Chauhan would like to gratefully acknowledge William Paterson University for assigned release time (ART) award for part of the research described here and also for the research program in general.

הערה: כל ריאגנטים משמשים הוא מיצרן ללא טיהור נוספת. התגובות היו במעקב במשך עד שבוע באמצעות ספקטרוסקופיית UV-Vis כדי להבטיח הפחתה מלאה. כל תגובות מתבצעים מתחת למכסת מנוע אוורור לבוש בטיחות המתאימה משוחק בכל עת, כולל כפפות, משקפי מגן עיניים, בחלוקי מעבדה. <p class="jove_title" style=...

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מלח דיווח בעיתון זה הוא המלחים רק שנבדקו מתכת זה. כתוצאה מכך, אין הוודאות כי אסטרטגית תגובה זה יעבוד עם כל המלחים של המתכות, בעיקר זהב. המסיסות של מלחים אלה במים עלולה גם להשפיע על התוצאה של התגובה במונחים של זמן תגובה, מורפולוגיה, ותשואות. בכל התגובות, silane התווסף פתרון ...

ככל שהביקוש והיישומים של עליות ננו המעצב, אז לעשות את השיטות השונות של סינתזה. שיטות &quot;מלמעלה למטה&quot;, כגון אבלציה ליזר או תחריט כימי כבר מועסקות controllability המעולה שלהם ויכלו לפתור חומרים באופן מהימן עד לרמה תת-מיקרון. שיטות אלו מבוסס על חומרים בתפזורת מעובדת למרכיבים עדינים, אשר בדרך כלל להגדיל את העלות של ייצור כמו גודל ננו-המבנה הרצוי פוחתות. שיטה חלופית של סינתזה זו הגישה &quot;מלמטה למעלה&quot;, השולטת סינתזה ברמה מולקולרית ובונה עד ננו-המבנה הרצוי. זה מקנה מידה משמעותית של שליטה על הרכבה עצמית, הפונקציונלית רצויה, פסיביות, ויציבות בדור של חומרי nanostructured אלה 1. הודות לשיתוף פעולה מהרמה המולקולרית, nanocomposites היברידית יכול להיווצר לספק את היתרונות של שני החומרים בתוך אותה structuמִחָדָשׁ. כמו ננו מסונתז באמצעות האסטרטגיה מלמטה למעלה, שיטות צריכות להיות מועסק על מנת לשלוט גודל חלקיקים, צורה, מרקם, הידרופוביות, נקבובי, פריצה, ופונקציונלי 2. בסינתזת nanoparticle מתכת ליבה, מלח המתכת הראשוני מצטמצם בתהליך autocatalytic ליצור חלקיקי אפס ערכי, אשר בתורו לכוון את ההתגרענות של חלקיק אחר. זה מוביל clustering ו -3 ייצור ננו-חלקיקים לבסוף. במאמץ לשלוט על הגודל של חלקיקים שנוצרו ולמנוע מהם מזרזים מתוך פתרון, מייצב כגון הליגנדים, פעיל שטח, מטען יוני, ופולימרים גדולים מנוצלים על יכל לחסום חלקיקים מן למסכת נוספת 4-10. חומרים אלו מעכבים את האטרקציה ואן דר ואלס של החלקיקים, בין אם באמצעות הפרעה סטרית בשל נוכחותם של קבוצות מגושמות או דרך Coulombic 3 repulsions. בשנת tעבודתו, סיר קליל, אחד, אסטרטגיה סינטתית עבור דור של חלקיקי ליבת מתכת שונה באמצעות silane, n- (2-aminoethyl) -3-aminosilanetriol (2-AST) מוצגת (איור 1). הליגנדים על המתחם הזה הוא מסוגלים להפחית מבשרי מתכת וייצוב חלקיקי מתכת עם יעילות גבוהה יחסית. השלושה moieties silanol הנוכחי הם גם מסוגלים crosslinking וזה מהווה רשת המקושרים ביניהם של פולימר organosilane ספוג חלקיקים בתוך המטריצה ​​שלה (איור 2). בניגוד לרוב silanes, אשר עוברים הידרוליזה בקלות בנוכחות מים, המתחם הזה הוא התייצב במים, דבר המהווה יתרון למטרות הידרופוביות, יציבות ושליטה.

<table border="0" cellpadding="0" cellspacing="0" width="644">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:287px;">n-(2-aminoethyl)-3-aminosilanetriol (2-AST)</td>
			<td style="width:209px;">Gelest</td>
			<td style="width:72px;">SIA0590.0</td>
			<td style="width:76px;">25% in H2O</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Silver nitrate</td>
			<td>Sigma Aldrich</td>
			<td>S6506</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Gold(III) chloride trihydrate</td>
			<td>Sigma Aldrich</td>
			<td align="right">520918</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Palladium(II) Nitrate</td>
			<td>Alfa Aesar</td>
			<td align="right">11035</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Deuterium Dioxide</td>
			<td>Cambridge Isotope Laboratories</td>
			<td>DLM-4-100</td>
			<td></td>
		</tr>
	</tbody>
</table>

generation of zerovalent metal core nanoparticles using n-(2-aminoethyl)-3-aminosilanetriol

In this work, a facile one-pot reaction for the formation of metal nanoparticles in a water solution through the use of n-(2-aminoethyl)-3-aminosilanetriol is presented. This compound can be used to effectively reduce and complex metal salts into metal core nanoparticles coated with the compound. By controlling the concentrations of salt and silane one is able to control reaction rates, particle size, and nanoparticle coating. The effects of these changes were characterized through transmission electron microscopy (TEM), UV-Vis spectrometry (UV-Vis), Nuclear Magnetic Resonance spectroscopy (NMR) and Fourier Transform Infrared spectroscopy (FTIR). A unique aspect to this reaction is that usually silanes hydrolyze and cross-link in water; however, in this system the silane is water-soluble and stable. It is known that silicon and amino moieties can form complexes with metal salts. The silicon is known to extend its coordination sphere to form penta- or hexa-coordinated species. Furthermore, the silanol group can undergo hydrolysis to form a Si-O-Si silica network, thereby transforming the metal nanoparticles into a functionalized nanocomposites.

התגובה היה פיקוח באמצעות ספקטרומטריית UV-Vis כמו היווצרות nanoparticle צריך לייצר פסגות מאפיין לכל הננו-חלקיק מתכת בודדים. בניתוח הסופי של חומרים מסונתזים הושג באמצעות TEM ו- FTIR. ספקטרה FTIR התקבלה אבקת יבשים של דגימות. הניתוח גודל החלקיקים ניתן להשיג על ידי מד?...

Watch this Scientific Journal Video about Generation of Zerovalent Metal Core Nanoparticles Using n-2-aminoethyl-3-aminosilanetriol at JoVE.com

Generation of Zerovalent Metal Core Nanoparticles Using n-2-aminoethyl-3-aminosilanetriol

A novel method for metal core nanoparticle synthesis using a water stable silanol is described.

הדור של Zerovalent מתכת Core חלקיקים שימוש n- (2-aminoethyl) -3-aminosilanetriol

In this work, a facile one-pot reaction for the formation of metal nanoparticles in a water solution through the use of ...

The overall goal of this protocol is to produce water-soluble metal core nanoparticles. This general method uses a silicon-based surfactant as both a reducing and a stabilizing agent. This method helps answer key questions about control of self-assembly functionality, passivity, and the stability of nanostructured materials.The main advantage of this technique is that a water-soluble silicon compound can reduce metal precursors to metal nanoparticles and efficiently stabilize them. It uses green conditions to create silox and metal nanocomposites which have applications in therapeutics drug delivery and heterogeneous catalyses. The implications of this technique are far-reaching because the surfactant can cross-link to form organo-silene gels impregnated with metallic nanoparticles.This method can be applied to create hybrids of most noble metals and can provide mechanistic insights into the formation of nanoparticles. By controlling the concentrations of salt and silene it is possible to control the reaction rates, particle size, and nanoparticle coating. To start the procedure first weigh out 16.9 milligrams of silver nitrate into a 50 milliliter erlenmyer flask equipped with a magnetic stir bar.Add 20 milliliters of 18.2 megaohm ultra-pure water to the flask and stopper it. Place the flask in an oil bath on a hot plate at 60 degrees Celsius and stir the solution. Next slowly add 144 microliters of 2-AST to the flask, using a precision micropipette.Flush the pipette several times with the mixture to ensure that all of the 2-AST is transferred. Every half-hour remove 100 microliters of the mixture using a precision micropipette and place it into a plastic cuvette for UV-Vis spectroscopy analysis. To the plastic cuvettes containing the sample add one milliliter of ultra-pure water and mix the sample in each of the cuvettes thoroughly by repeat pipetting.Transfer the cuvette to a UV-Vis spectrophotometer and record the absorbance spectrum. Discard the sample in an appropriate container when finished. After six hours, remove the flask from the oil bath and transfer the nanoparticle mixture to a 20 milliliter scintillation vial for storage.To begin the sample preparation for electron microscopy place a 200 carbon mesh Formvar coated copper grid onto a clean piece of filter paper. Once the sample has cooled to room temperature cast drop approximately 60 microliters of the nanoparticle mixture directly onto the grid using a one milliliter plastic Pasteur pipette. Allow the grid to dry for 24 hours.Load the grid into a transmission electron microscope and record images using 10 microampere current and 100 kilovolt accelerating voltage. To prepare the NMR sample, first use a precision pipette to transfer 50 microliters of deuterium oxide into a clean NMR tube. Next, slowly pipette 400 microliters of the nanoparticle mixture into the same NMR tube.Cap the tube and shake the top of the tube to force the mixture to the bottom. Mix the sample by shaking and repeatedly inverting the NMR tube. Insert the sample tube into the NMR magnet and record the NMR spectrum.To prepare the FTIR sample first place two milliliters of the nanoparticle mixture into a one dram glass vial. Continue by placing the vial into a vacuum dessicator. Connect the dessicator stopcock to a vacuum pump.Open it and then evacuate the dessicator. Use caution when drying the sample in a vacuum dessicator as rapid reduction of pressure may cause samples to flash boil, expelling some of the material out of the container. Once the vial no longer contains visible liquid, remove it from the dessicator, and scrape out the remaining solid sample using a clean spatula.Finally, place the sample onto an FTIR spectrometer fitted with zinc selenide crystal diode laser and record the FTIR spectrum. The formation of silver nanoparticles was monitored by UV-Vis Spectrometry analysis. The silver nanoparticles have a characteristic peak at 414 nanometers that increases with reaction time.Transmission electron microscopy was used to confirm the presence of silver nanoparticles. Analysis of the images shows that the majority of the nanoparticles were in the 10 nanometer size range. Fourier transform infrared spectroscopy was used to verify the complexation of the nanoparticles with 2-AST.Absorption at around 1000 reciprocal centimeters shows the presence of silicon-oxygen-silicon linkages and peaks at 3000 to 2750 reciprocal centimeters and 1550 to 1650 reciprocal centimeters are attributed to the amino group. Analysis of the NMR spectrum of the nanoparticles shows the coordination to the 2-AST by the shift in and appearance of new peaks between 2.72 to 3.40 parts per million. Once mastered, the reaction process can be set up within an hour.While performing this procedure, it's important to ensure the purity of the water. All experiments were carried out in ultra-pure, 18.2 megaohm water. Following this procedure, scanning electron microscopy or x-ray powder diffraction can be used to further elucidate structural features, such as morphology, size and particle roughness of the hybrid nanocomposites.After watching this video, you should have a good understanding of how to generate and analyze the stabilized metal-core nanoparticles. This method produces large quantities of water-soluble metal nanohybrids which can be capped with ligands for drug delivery applications. Don't forget that working with silver nitrate and other reagents can be hazardous.The use of protective equipment such as gloves, goggles and lab coats is strongly advised while performing this procedure. Thanks for watching, good luck with your experiments.

Research

JoVE Journal

Chemistry

Generation of Zerovalent Metal Core Nanoparticles Using n-(2-aminoethyl)-3-aminosilanetriol

Using Polystyrene-block-poly(acrylic acid)-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

Using Polystyrene-block-polyacrylic acid-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

באמצעות Polystyrene-<em&gt; בלוק</em&gt; -poly (חומצה אקרילית) -coated מתכת חלקיקים כמו מונומרים להומו- ושיתוף פילמור

We present a template-free method for &#8220;polymerizing&#8221; nanoparticles into long chains without side branches. A variety of nanoparticles are ...

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

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, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

סינתזה, אפיון, ואת Functionalization של תקליטורים היברידי Au / ו Au / ZnS Core / Shell חלקיקים

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

Sediment Core Extrusion Method at Millimeter Resolution Using a Calibrated, Threaded-rod

משקעי Core שחול שיטה ברזולוצית המילימטר בעזרת מכויל, הברגה-מוט

Aquatic sediment core subsampling is commonly performed at cm or half-cm resolution. Depending on the sedimentation rate and depositional environment, ...

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis

בחיי עיר זיהוי, כימות תא בודד של תחמוצת מתכת חלקיקים באמצעות ניתוח Microprobe גרעיני

Micro-analytical techniques based on chemical element imaging enable the localization and quantification of chemical composition at the cellular level. ...

Synthesis of Core-shell Lanthanide-doped Upconversion Nanocrystals for Cellular Applications

סינתזה של ליבה-קליפה מסטול לנתניד Upconversion Nanocrystals עבור אפליקציות לסלולר

Lanthanide-doped upconversion nanocrystals (UCNs) have attracted much attention in recent years based on their promising and controllable optical ...

Ligand-Mediated Nucleation and Growth of Palladium Metal Nanoparticles

התגרענות בתיווך ליגנד והצמיחה של חלקיקי מתכת פלדיום

The size, size distribution and stability of colloidal nanoparticles are greatly affected by the presence of capping ligands. Despite the key contribution ...

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

מלח מותכת סינתזה של חלקיקי תחמוצת מתכת מורכבים

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. ...

Imaging Corrosion at the Metal-Paint Interface Using Time-of-Flight Secondary Ion Mass Spectrometry

הדמיה קורוזיה בממשק צבע מתכת באמצעות המסה של זמן טיסה משני המוני ספקטרומטריה

Corrosion developed at the paint and aluminum (Al) metal-paint interface of an aluminum alloy is analyzed using time-of-flight secondary ion mass ...

A Microwave-Assisted Direct Heteroarylation of Ketones Using Transition Metal Catalysis

מיקרוגל בסיוע ישיר הטרולציה של Ketones באמצעות מתכת מעבר זרז

Heteroarylation introduces heteroaryl fragments to organic molecules. Despite the numerous available reactions reported for arylation via transition metal ...