Portions of this study have been previously published in the Journal of Radioanalytical and Nuclear Chemistry.3,13 A patent is pending for this method.

Achtung: Die hier skizzierten Prozess beinhaltet die Verwendung von radioaktivem Material (zB Uran-Hexahydrat) und mehrere ätzende Stoffe. Geeignete Schutzkleidung und Ausrüstung verwendet werden soll (einschließlich eines Laborkittel, Handschuhe, Schutzbrille und einer Abzugshaube) während der Probenvorbereitung. Darüber hinaus sollten Laborbereiche für diese Arbeit verwendet regelmäßig auf radioaktive Kontamination überwacht werden. Anmerkung:. Die chemischen Verbindungen notwendig sind in Tabelle 1 aufgelistet Diese Formulierung wurde von zuvor Prüfung kompositorischen Daten für Trinitit durch Mittelung der Massenanteile für mehrere unterschiedliche Trinitit Proben entwickelt berichteten 10 Die hier ausgewiesenen bestimmt Massenanteile 10 Das &quot;fehlende&quot; Masse.. (die Fraktionen nicht zur Einheit zusammenfassen) vorhanden ist, um eine gewisse Flexibilität beim Hinzufügen von Kraftstoff, Sabotage, und andere Bestandteile zu ermöglichen. Unsere unabhängige Analyse von mehreren Proben Trinitit legt nahe, dass Quarz ist der einzige MineralphaseÜberleben in Trinitit. 5 ist daher der einzige Quarz Mineral in unserer Standard Trinitit Formulierung (STF) enthalten. Obwohl Relikt Körner anderer Mineralien in Trinitit gemeldet, 11 davon sind eher die Ausnahme und nicht die Regel sein. Im Allgemeinen ist die einzige Quarz Mineral im Schmelzglas gefunden. 10,12 Auch ist Quarzsand ein üblicher Bestandteil von Asphalt und Beton, der in der Bildung von städtischen Kernschmelzglas wichtig sein werden. <table fo:keep-together.within-page="1"><tbody><tr height="41"><td colspan="2" height="41" style="height:42px;width:317px;"> Gemittelt Trinitit Daten </td><td colspan="2" style="width:317px;"> Standard Trinitit Formulierung (STF) </td></tr><tr height="22"><td height="22" style="height:22px;width:159px;"> Verbindung </td><td style="width:159px;"> Massenanteil </td><td style="width:159px;"> Verbindung </td><html><td style="width:159px;"> Massenanteil </td></tr><tr height="26"><td height="26" style="height:26px;width:159px;"> SiO 2 </td><td style="width:159px;"> 6.42x10 -1 </td><td style="width:159px;"> SiO 2 </td><td style="width:159px;"> 6.42x10 -1 </td></tr><tr height="26"><td height="26" style="height:26px;width:159px;"> Al 2 O 3 </td><td style="width:159px;"> 1.43x10 -1 </td><td style="width:159px;"> Al 2 O 3 </td><td style="width:159px;"> 1.43x10 -1 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;"> CaO </td><td style="width:159px;"> 9.64x10 -2 </td><td style="width:159px;"> CaO </td><td style="width:159px;"> 9.64x10 -2 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;"> FeO </td><td style="width:159px;"> 1.97x10 -2 </td><html> &quot;&gt; FeO </td><td style="width:159px;"> 1.97x10 -2 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;"> MgO </td><td style="width:159px;"> 1.15x10 -2 </td><td style="width:159px;"> MgO </td><td style="width:159px;"> 1.15x10 -2 </td></tr><tr height="26"><td height="26" style="height:26px;width:159px;"> Na 2 O </td><td style="width:159px;"> 1.25x10 -2 </td><td style="width:159px;"> Na 2 O </td><td style="width:159px;"> 1.25x10 -2 </td></tr><tr height="26"><td height="26" style="height:26px;width:159px;"> K 2 O </td><td style="width:159px;"> 5.13x10 -2 </td><td style="width:159px;"> KOH </td><td style="width:159px;"> 6.12x10 -2 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;"> MnO </td><td style="width:159px;"> 5.05x10 -4 </td><td style="width:159px;"> MnO </td>9px; &quot;&gt; 5.05x10 -4 </td></tr><tr height="26"><td height="26" style="height:26px;width:159px;"> TiO 2 </td><td style="width:159px;"> 4.27x10 -3 </td><td style="width:159px;"> TiO 2 </td><td style="width:159px;"> 4.27x10 -3 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;"> Gesamt </td><td style="width:159px;"> 9.81x10 -1 </td><td style="width:159px;"> Gesamt </td><td style="width:159px;"> 9.91x10 -1 </td></tr></tbody></table> Tabelle 1. Liste der chemischen Verbindungen. 1. Herstellung des STF Hinweis: Benötigte Ausrüstung umfasst eine Mikrowaage, Metallspachtel, einer keramischen Mörser und Stößel, einer chemischen Abzugshaube, Latexhandschuhe, Laborkittel und Schutzbrille. <ol><li> Mischen von nicht-radioaktiven Komponenten <ol><li> Erfassen mindestens 65 g Quarzsand (SiO 2), 15 g Al 2 O 3 &lt;/ sub&gt; Pulver, 10 g CaO-Pulver, 2 g FeO-Pulver, 2 g MgO-Pulver, 2 g Na 2 O-Pulver, 7 g KOH-Pellets wurden 1 g MnO-Pulver und 1 g TiO 2 -Pulver ( in Tabelle 1 aufgeführten Verbindungen). </li><li> Verwenden Sie einen Mikrowaage und kleine Spachtel, um genau die Massenanteile der einzelnen Verbindungen zu messen, wie in Tabelle 1 aufgeführt. Die besten Ergebnisse vorzubereiten 100 g des nicht-radioaktiven Vorstufen-Matrix auf einmal. </li><li> Verwenden Sie einen Mörser und Stößel zu pulverisieren (auf ~ 10-20 um Größe Granulat) und gründlich mischen, die Verbindungen und bilden eine homogene Pulvermischung, die 64,2 g SiO 2, 14,2 g Al 2 O 3, 9,64 g CaO, 1,97 g FeO, 1,15 g MgO, 1,25 g Na 2 O. 6,12 g KOH, 0,0505 g MnO, und 0,427 g TiO2. </li><li> Rühren der Mischung unter Verwendung einer Kugelmischer, kurz bevor der nächste Schritt gemacht wird. </li></ol></li><li> Mischen der STF mit Urannitrat-Hexahydrat (UNH) <ol><li> Acquire mindestens 1 g UNH. </li><li> Innerhalb einer Abzugshaube, pulverisieren einige UNH Kristalle (mit einem Mörser und Stößel) zu einem feinen Pulver von 1-2 um Körnchen zu bilden. </li><li> Hinzuzufügen 33,75 ug UNH pro Gramm des nicht-radioaktiven Vorstufen-Matrix (dieses Verhältnis zur Simulation eines einfachen Waffe mit einer Ausbeute von 1 Kilotonnen angebracht). 13 </li><li> Gründliche Durchmischung der Pulvermischung, einschließlich der UNH, mit einem Mörser und Stößel. Vervollständigen endgültige Mischen kurz vor dem Schmelzschritt. </li></ol></li></ol> 2. Herstellung von 1-Gramm-Melt Glasproben Hinweis: Benötigte Ausrüstung umfasst eine HTF bewertet bei 1600 ° C oder höher, hochreine Graphittiegel, langen Edelstahltiegelzange, hitzebeständige Handschuhe und eine Schutzbrille. Hitzebeständige Handschuhe und Augenschutz sollte bei der Einführung oder Entnahme von Proben aus dem Ofen getragen werden. Getönte Schutzbrille (oder Sonnenbrille) sind nützlich, da sie die Blendung aus dem Ofen zu reduzieren. <ol><li> Herstellung eines nicht-radioaktiven Probe <ol><li> Füllen einer dicken Keramikschale (wie ein Mörtel) mit ~ 100 g reinem Quarzsand und aufrechtzuerhalten bei RT in der Nähe von dem Ort des Ofens, wo die Proben geschmolzen werden. </li><li> Heizen Sie den HTF zu 1.500 ° C. </li><li> Sorgfältig zu messen 1,00 g des nicht-radioaktiven Pulvermischung und legen Sie das Pulver in einem hochreinen Graphittiegel. </li><li> Legen Sie das Tiegel im beheizten HTF (mit einem langen Paar Stahltiegelzange) und Schmelze der Mischung für 30 min. </li><li> Entfernen Sie die Probe (wieder mit Hilfe der Zange) und gießen Sie die geschmolzene Probe in den Mörtel mit Sand gefüllt. </li><li> Lassen Sie die Glasperle für 1-2 Minuten vor dem Umgang mit kühlen. </li><li> Polieren Sie die Wulst zu Rest Sand zu entfernen (falls erforderlich). </li></ol></li><li> Herstellung eines radioaktiven Probe <ol><li> Wiederholen Sie die Schritte 2.1.1 und 2.1.2. </li><li> Sorgfältig zu messen 1,00 Gramm der radioaktiven Pulvermischung (einschließlich UNH) und legen Sie die powd<html> er in einer hochreinen Graphittiegel mit einem separaten Spachtel und Mikrowaage, um Kreuzkontamination zu vermeiden. </li><li> Wiederholen Sie die Schritte 2.1.4 - 2.1.6 oben. </li><li> Überwachen Sie die Gegend rund um den Ofen (mit einem Handstrahlungsdetektor und / oder Swipe-Assays), die für radioaktive Kontamination zu überprüfen. </li></ol></li></ol> 3. Proben Aktivierung Hinweis: Die folgenden Gleichungen abgeleitet wurden unter der Annahme der Verwendung von Waffen Grad (angereichert) Uranmetall. Die Mengen der UNH oder Uranoxid müssen nach dem Massenanteil an elementarem Uran und der Ebene 235 U Anreicherung skaliert. <ol><li> Aktivierung eines Schmelzglasprobe mit Uranium Fue <ol><li> Berechnen Sie den Massenanteil von Uranmetall für die Probe mit der folgenden Gleichung 13 (wobei m U steht für die Uran-Massenanteil und Y für die Waffe Ausbeute) benötigt: 473 / 53473eq1.jpg &quot;/&gt; </li><li> Optional: Berechnen Sie den Massenanteil von Sabotage (zB natürliches Uran, Blei, Wolfram) unter Verwendung der folgenden Gleichung: 13 <img alt="Gleichung 2" src="/files/ftp_upload/53473/53473eq2.jpg" /></li><li> Berechnung der Sollzahl der Spaltungen in der Probe unter Verwendung der folgenden Gleichung 13 wobei M s die Masse der Probe in Gramm und N f die Zahl der Spaltungen in der Probe während der Bestrahlung erzeugt wird: <img alt="Gleichung 3" src="/files/ftp_upload/53473/53473eq3.jpg" /></li><li> Berechnen Sie die notwendige Belichtungszeit mit Hilfe der folgenden Gleichung 13 wobei m 235 repräsentiert die 235 U-Massenanteil (Anreicherung) und T irr ist die Bestrahlungszeit in Sekunden: <img alt="Gleichung 4" src="/files/ftp_upload/53473/53473eq4.jpg" /></li><li> Bestrahlen die Probe fürt irr Sekunden bei einem thermischen Neutronenfluss von 4,0 x 10 14 n / cm 2 / sec. Zum Beispiel wird eine 60 sec Bestrahlung in Rohrpost 1 (PT-1) HFIR (mit einer thermischen zur Resonanzüberhöhung 35) etwa 1,1 x 10 11 Spaltungen in einer Probe, die 870 ug UNH (äquivalent zu 410 &amp; mgr; g zu erzeugen natürliches Uran oder 3,0 &amp; mgr; g von 235 U). Dies hat für eine 0.433 g Glasperlen entworfen, um eine Schmelzglasprobe von einer Waffe mit einem 0,1 Kilotonnen Ausbeute hergestellt simulieren, erreicht worden. Diese Probe wurde gründlich von Cook et al 14 analysiert. </li><li> Folgen Sie geltenden Sicherheitsprotokolle für die Handhabung der radioaktiven Probe nach der Bestrahlung. </li></ol></li><li> Aktivierung eines Schmelzglasprobe mit Plutonium Fuel (Planungsfaktoren) <ol><li> Berechnen Sie den Massenanteil von Plutoniummetall für die Probe mit der folgenden Gleichung 13 wobei M Pu Vertre erforderlichts Plutonium Massenanteil und Y für die Waffe Ausbeute: <img alt="Gleichung 5" src="/files/ftp_upload/53473/53473eq5.jpg" /></li><li> Wiederholen Sie die Schritte 3.1.2 und 3.1.3 oben. </li><li> Bestimmung der Bestrahlungszeit nötig, um die gewünschte Zahl der Spaltungen in der Schmelzglasprobe erhalten. Diese Zeit hängt von der Zusammensetzung und der Gehalt des Plutoniums sowie Neutronenenergiespektrum abhängen. </li></ol></li></ol> Hinweis: Große Sorgfalt sollte beim Umgang mit Plutonium und zusätzliche Analyse erforderlich sein wird genommen werden. Während ich dies schreibe, hat nur Uran, in dem bei UT hergestellt und HFIR bestrahlt synthetischen Schmelzglasproben verwendet.

<ol>
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This work was performed under grant number DE-NA0001983 from the Stewardship Science Academic Alliances (SSAA) Program of the National Nuclear Security Administration (NNSA).

Hinweis in Bezug auf Schritte 1.2.2 und 1.2.3: Die genaue Höhe der UNH wird je nach Szenario unterschiedlich simuliert. Die Planungs Formeln Giminaro et al. Entwickelt wurden, können verwendet werden, um die entsprechende Masse an Uran für eine gegebene Probe 13, wie im Abschnitt &quot;Sample Aktivierung&quot; von diesem Papier zu wählen. Auch kann Uranoxid (UO 2 oder U 3 O 8) anstelle von UNH verwendet werden, wenn verfügbar, und der Massenanteil von 235 U<...

Concerns over the potential malicious use of nuclear weapons by terrorists or rogue nations have highlighted the importance of nuclear forensics analysis for the purpose of attribution.1 Rapid post-detonation analysis techniques are desirable to shorten the attribution timeline as much as possible. The development and validation of such techniques requires realistic nuclear debris samples for testing. Nuclear testing no longer occurs in the United States and nuclear surface debris from the testing era is not readily available (with the exception of trinitite - the melt glass produced by the first nuclear test at the trinity site) and therefore realistic surrogate debris is needed. 
The primary goal of the method described here is the production of realistic surrogate nuclear debris similar to trinitite. Synthetic nuclear melt glass samples which are readily available to the academic community can be used to test existing analysis techniques and to develop new methods such as thermo-chromatography for rapid post-detonation analysis.2 With this goal in mind the current study is focused on producing samples which mimic trinitite but do not contain any sensitive weapon design information. The fuel and tamper components within these samples are completely generic and the comparison to trinitite is based on chemistry, morphology, and physical characteristics. The similarities between trinitite and the synthetic nuclear melt glass produced in this study have been previously discussed.3
The purpose of this article is to outline the details of the production process used at the University of Tennessee (UT). This production process was developed with two key parameters in mind: 1) the composition of material incorporated into nuclear melt glass, and 2) the melting temperature of the material. Methods exist for estimating the melting temperature of glass forming networks4 and these techniques have been employed here, along with additional experimentation to determine the optimal processing temperature for the trinitite matrix.5
Alternative methods for surrogate debris production have been published recently. The use of high power lasers has the advantage of creating sufficiently high temperatures to cause elemental fractionation within the target matrix.6 Porous chromatographic substrates have been used to produce small particles similar to fallout particles using condensed phase methods7. The latter method is most useful for producing particulate debris (nuclear fallout) and has been demonstrated with natural metals. The advantages of the method presented here are 1) simplicity, 2) reproducibility, and 3) scalability (sample sizes can range from tiny beads to large chunks of melt glass). Also, this method is expandable both in terms of production output and variety of explosive scenarios covered, and it has already been demonstrated using radioactive materials. A sample has been successfully activated at the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL). Natural uranium compounds were added to the matrix prior to melting and fission products were produced in situ by neutron irradiation. 
Methods within the glass making industry and those employed for the purpose of radioactive waste immobilization8 have been consulted in the development of the method presented here. The unique effects of radiation in glasses are of inherent interest9 and will constitute an important area of study as this method is further developed. 
The method described below is appropriate for any application where a bulk melt glass sample is desired. These samples most closely resemble the material found near the epicenter of a nuclear explosion. Samples of various sizes can be produced, however, methods employing plasma torches or lasers will be more useful for simulating fine particulate debris. Also, commercial HTFs do not reach temperatures high enough to cause elemental fractionation for a wide range of elements. This method should be employed when physical and morphological characteristics are of primary importance.

<table><tbody><tr><td>High Temperature Furnace (HTF)</td><td>Carbolite</td><td>HTF 18</td><td>1,800 &amp;#176;C HTF used to melt samples</td></tr><tr><td>High Temperature Drop Furnace</td><td>CM Inc.</td><td>1706 BL</td><td>1,700 &amp;#176;C Drop Furnace used to melt samples</td></tr><tr><td>Graphite Crucibles</td><td>SCP Science</td><td>040-060-041</td><td>27 ml high purity graphite crucibles (10 pack)</td></tr><tr><td>Crucible Tongs</td><td>Grainger</td><td>5ZPV0</td><td>26 in., stainless steele tongs for handling crucibles</td></tr><tr><td>Heat Resistent Gloves</td><td>Grainger</td><td>8814-09</td><td>Gloves used to protect hands from heat during sample intro/removal</td></tr><tr><td>Mortar &amp;amp; Pestle</td><td>Fisherbrand</td><td>S337631</td><td>300 ml, Ceramic mortar and pestle for powdering and mixing</td></tr><tr><td>Micro Balance</td><td>Grainger</td><td>8NJG2</td><td>220 g Cap, high precision scale for measuring powder mass</td></tr><tr><td>Spatulas</td><td>Fisherbrand</td><td>14374</td><td>Metal spatulas for measure small quantities of powder</td></tr><tr><td>SiO&lt;sub&gt;2&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>274739-5KG</td><td>Quartz Sand&amp;nbsp; CAS Number: 14808-60-7</td></tr><tr><td>Al&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;3&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>11028-1KG</td><td>Aluminum Oxide Powder&amp;nbsp; CAS Number: 1344-28-1</td></tr><tr><td>CaO</td><td>Sigma-Aldrich</td><td>12047-2.5KG</td><td>Calcium Oxide Powder&amp;nbsp; CAS Number: 1305-78-8</td></tr><tr><td>FeO</td><td>Sigma-Aldrich</td><td>400866-25G</td><td>Iron Oxide Powder&amp;nbsp; CAS Number: 1345-25-1</td></tr><tr><td>MgO</td><td>Sigma-Aldrich</td><td>342793-250G</td><td>Magnesium Oxide Powder&amp;nbsp; CAS Number: 1309-48-4</td></tr><tr><td>Na&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>36712-25G</td><td>Sodium Oxide Powder&amp;nbsp; CAS Number: 1313-59-3</td></tr><tr><td>KOH</td><td>Sigma-Aldrich</td><td>278904-250G</td><td>Potasium Hydroxide Pellets&amp;nbsp; CAS Number: 12030-88-5</td></tr><tr><td>MnO</td><td>Sigma-Aldrich</td><td>377201-500G</td><td>Manganese Oxide Powder&amp;nbsp; CAS Number: 1344-43-0</td></tr><tr><td>TiO&lt;sub&gt;2&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>791326-5G</td><td>Titanium Oxide Beads&amp;nbsp; CAS Number: 12188-41-9</td></tr></tbody></table>

production of synthetic nuclear melt glass

Realistic surrogate nuclear debris is needed within the nuclear forensics community to test and validate post-detonation analysis techniques. Here we outline a novel process for producing bulk surface debris using a high temperature furnace. The material developed in this study is physically and chemically similar to trinitite (the melt glass produced by the first nuclear test). This synthetic nuclear melt glass is assumed to be similar to the vitrified material produced near the epicenter (ground zero) of any surface nuclear detonation in a desert environment. The process outlined here can be applied to produce other types of nuclear melt glass including that likely to be formed in an urban environment. This can be accomplished by simply modifying the precursor matrix to which this production process is applied. The melt glass produced in this study has been analyzed and compared to trinitite, revealing a comparable crystalline morphology, physical structure, void fraction, and chemical composition.

Die nicht-radioaktiven Proben in dieser Studie hervorgebracht haben, um Trinitit verglichen worden und Abbildungen 1-3 zeigen, dass die physikalischen Eigenschaften und die Morphologie sind in der Tat ähnlich. Abbildung 1 zeigt Fotografien, die die Ähnlichkeiten in Farbe und Textur, die auf makroskopischer Ebene beobachtet werden, zu offenbaren. Abbildung 2 zeigt Rasterelektronenmikroskop (SEM) Sekundärelektronen (SE) Bilder, die ähnliche Merkmale im Mikrometerberei...

Watch this Scientific Journal Video about Production of Synthetic Nuclear Melt Glass at JoVE.com

Production of Synthetic Nuclear Melt Glass

A protocol for the production of synthetic nuclear melt glass, similar to trinitite, is presented.

Herstellung von synthetischen Kernschmelzglas

Realistic surrogate nuclear debris is needed within the nuclear forensics community to test and validate post-detonation analysis techniques. Here we ...

production-of-synthetic-nuclear-melt-glass

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

9.4K Aufrufe.  United States Military Academy. A protocol for the production of synthetic nuclear melt glass, similar to trinitite, is presented.

Serie: Production of Synthetic Nuclear Melt Glass

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

Methoden der Ex-Situ und In Situ Untersuchungen zu strukturellen Veränderungen: der Fall der Kristallisation von metallischen Gläsern

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

Forschung

Ingenieurwesen

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. Here, we introduce the molten-salt synthesis (MSS) method for making metal oxide nanomaterials. Advantages over other methods include its simplicity, greenness, reliability, scalability, and generalizability. Using pyrochlore lanthanum hafnium oxide (La2Hf2O7) as a representative, we describe the MSS protocol for the successful synthesis of complex metal oxide nanoparticles (NPs). Furthermore, this method has the unique ability to produce NPs with different material features by changing various synthesis parameters such as pH, temperature, duration, and post-annealing. By fine-tuning these parameters, we are able to synthesize highly uniform, non-agglomerated, and highly crystalline NPs. As a specific example, we vary the particle size of the La2Hf2O7&#160;NPs by changing the concentration of the ammonium hydroxide solution used in the MSS process, which allows us to further explore the effect of particle size on various properties. It is expected that the MSS method will become a more popular synthesis method for nanomaterials and more widely employed in the nanoscience and nanotechnology community in the upcoming years.

Here, we demonstrate a unique, relatively low-temperature, molten-salt synthesis method for preparing uniform complex metal oxide lanthanum hafnate nanoparticles.

Salzschmelze Synthese von komplexen Metall-Oxid-Nanopartikel

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

Chemie

Optimized Sealing Process and Real-Time Monitoring of Glass-to-Metal Seal Structures

Residual stress is an essential factor to keeping the hermeticity and robustness of a glass-to-metal seal structure. The purpose of this report is to demonstrate a novel protocol to characterize and measure residual stress in a glass-to-metal seal structure without destroying the insulation and hermeticity of sealing materials. In this research, a femto-laser inscribed fiber Bragg grating sensor is used. The glass-to-metal seal structure that is measured consists of a metal shell, sealing glass, and Kovar conductor. To make the measurements worthwhile, the specific heat treatment of metal-to-glass seal (MTGS) structure is explored to obtain the model with best hermeticity. Then, the FBG sensor is embedded into the path of sealing glass and becomes well-fused with the glass as the temperature cools to RT. The Bragg wavelength of FBG shifts with the residual stress generated in sealing the glass. To calculate the residual stress, the relationship between Bragg wavelength shift and strain is applied, and the finite element method is also used to make the results reliable. The online monitoring experiments of residual stress in sealing glass are carried out at different loads, such as high temperature and high pressure, to broaden functions of this protocol in harsh environments.

Key procedures to optimize the sealing process and achieve real-time monitoring of the metal-to-glass seal (MTGS) structure are described in detail. The embedded fiber Bragg grating (FBG) sensor is designed to achieve online monitoring of temperature and high-level residual stress in the MTGS with simultaneous environmental pressure monitoring.

Optimierter Versiegelungsprozess und Echtzeitüberwachung von Glas-Metall-Dichtungsstrukturen

Residual stress is an essential factor to keeping the hermeticity and robustness of a glass-to-metal seal structure. The purpose of this report is to ...

Comparison of Two Different Synthesis Methods of Single Crystals of Superconducting Uranium Ditelluride

Single crystal specimens of the actinide compound uranium ditelluride, UTe2, are of great importance to the study and characterization of its dramatic unconventional superconductivity, believed to entail spin-triplet electron pairing. A variety in the superconducting properties of UTe2 reported in the literature indicates that discrepancies between synthesis methods yield crystals with different superconducting properties, including the absence of superconductivity entirely. This protocol describes a process to synthesize crystals that exhibit superconductivity via chemical vapor transport, which has consistently exhibited a superconducting critical temperature of 1.6 K and a double transition indicative of a multi-component order parameter. This is compared to a second protocol that is used to synthesize crystals via the molten metal flux growth technique, which produces samples that are not bulk superconductors. Differences in the crystal properties are revealed through a comparison of structural, chemical, and electronic property measurements, showing that the most dramatic disparity occurs in the low-temperature electrical resistance of the samples.

Here, we present a protocol to synthesize two types of UTe2 crystals: those exhibiting robust superconductivity, via chemical vapor transport synthesis, and those lacking superconductivity, via molten metal flux synthesis.

Vergleich zweier verschiedener Synthesemethoden von Einkristallen supraleitender Uranditelluride

Single crystal specimens of the actinide compound uranium ditelluride, UTe2, are of great importance to the study and characterization of its dramatic ...

Hydrothermale Synthese von persistenten lumineszierenden Nanopartikeln

Synthesis of Persistent Luminescent Nanoparticles for Rewritable Displays and Illumination Applications

Persistent luminescent nanoparticles (PLNPs) possess the capabilities to maintain extended longevity and robust emission even after the excitation has ceased. PLNPs have been widely used across various domains, including information displays, data encryption, biological imaging, and artistic decoration with sustained and vivid luminosity, providing boundless possibilities for a variety of innovative technology and artistic projects. This protocol focuses on an experimental procedure for the hydrothermal synthesis of PLNPs. The successful synthesis of enduring luminescent nanomaterials with Mn2+ or Cr3+ serving as a luminescent center in Zn2GeO4: Mn (ZGO: Mn) or ZnGa2O4: Cr highlights the universality of this synthetic method. On the other hand, the optical properties of ZGO: Mn can be changed by adjusting the pH of precursor solutions, demonstrating the tunability of the protocol. When charged with ultraviolet (UV) at a wavelength of 365 nm for 3 min and then stopped, PLNPs exhibit the remarkable capacity to generate afterglow efficiently and consistently, which makes them ideal for making two-dimensional rewritable displays and three-dimensional transparent, luminous artworks. This protocol outlined in this paper provides a feasible method for the synthesis of persistent luminescent nanoparticles for further illumination and imaging applications, opening up novel prospects for the fields of science and art.

Autor im Rampenlicht: Weiterentwicklung von Bioimaging und Therapie mit funktionellen Nanomaterialien

A protocol is presented for the synthesis of persistent luminescent nanomaterials (PLNPs) and their potential applications in rewritable displays and artistic processing utilizing the afterglow effect under ultraviolet light (365 nm) irradiation.

Synthese von persistenten lumineszierenden Nanopartikeln für wiederbeschreibbare Displays und Beleuchtungsanwendungen

Persistent luminescent nanoparticles (PLNPs) possess the capabilities to maintain extended longevity and robust emission even after the excitation has ...

Fluid-cell Raman Spectroscopy for operando Studies of Reaction and Transport Phenomena during Silicate Glass Corrosion

Fluid-cell Raman Spectroscopy (FCRS) enables the real-time and space-resolved (operando) study of reaction mechanisms, kinetics, and their mutual interactions with transport processes during silicate glass corrosion at the micrometer scale and at elevated temperatures. This manuscript provides a detailed protocol for setting up an FCRS experiment, exemplified by a corrosion experiment with a ternary Na borosilicate glass and a 0.5 M NaHCO3 solution at a temperature of 86 &#177; 1 &#176;C. The protocol involves (i) sample preparation, (ii) assembly of the fluid cell, and (iii) setting of Raman measurement parameters for collecting Raman spectra across the sample/solution interface in regular time intervals. The results from the experiment show the formation of a water-rich zone between a silica-based surface alteration layer (SAL) and the pristine glass, which is an intrinsic feature of an interface-coupled dissolution-precipitation model for the formation of a SAL during silicate glass corrosion. The ability to track the reaction and transport processes during the corrosion of silicate glasses and potentially of other transparent materials, spatially resolved and in real-time, represents a unique strength of this technique, overcoming the disadvantages of conventional analysis of multi-step quenching experiments. The corrosion of the top side of the glass sample represents a current issue, reducing spatial resolution at depth due to precipitation within the laser pathway. This is caused by a solution-filled gap between the sapphire window of the fluid cell lid and the top side of the monolith, which is difficult to avoid during the experimental setup. This must be taken into account when choosing the depth at which the measurement should be made. In a few cases, the formation of air bubbles was observed, which disrupted or even led to the termination of the experiment. However, this can be avoided by carefully setting up the experiment, which requires little practice.

Fluid-cell Raman Spectroscopy (FCRS) enables in operando observations of reaction and transport phenomena during the aqueous corrosion of silicate glasses at a microscopic level, at elevated temperatures, and in real-time. Without interrupting ongoing processes, FCRS provides information about reaction mechanisms, kinetics, and transport processes.

Fluid-Cell-Raman-Spektroskopie für operando Untersuchungen von Reaktions- und Transportphänomenen bei Silikatglaskorrosion

Fluid-cell Raman Spectroscopy (FCRS) enables the real-time and space-resolved (operando) study of reaction mechanisms, kinetics, and their mutual ...

Fabricating Optical-quality Glass Surfaces to Study Macrophage Fusion

Visualizing the formation of multinucleated giant cells (MGCs) from living specimens has been challenging due to the fact that most live imaging techniques require propagation of light through glass, but on glass macrophage fusion is a rare event. This protocol presents the fabrication of several optical-quality glass surfaces where adsorption of compounds containing long-chain hydrocarbons transforms glass into a fusogenic surface. First, preparation of clean glass surfaces as starting material for surface modification is described. Second, a method is provided for the adsorption of compounds containing long-chain hydrocarbons to convert non-fusogenic glass into a fusogenic substrate. Third, this protocol describes fabrication of surface micropatterns that promote a high degree of spatiotemporal control over MGC formation. Finally, fabricating glass bottom dishes is described. Examples of use of this in vitro cell system as a model to study macrophage fusion and MGC formation are shown.

This protocol describes the fabrication of optical-quality glass surfaces adsorbed with compounds containing long-chain hydrocarbons that can be used to monitor macrophage fusion of living specimens and enables super-resolution microscopy of fixed specimens.

Herstellung optischer Qualität Glasflächen, Makrophagen Fusion zu studieren

Visualizing the formation of multinucleated giant cells (MGCs) from living specimens has been challenging due to the fact that most live imaging ...

Immunologie und Infektion

Synthesis of Nine-atom Deltahedral Zintl Ions of Germanium and their Functionalization with Organic Groups

Although the first studies of Zintl ions date between the late 1890's and early 1930's they were not structurally characterized until many years later.1,2 Their redox chemistry is even younger, just about ten years old, but despite this short history these deltahedral clusters ions E9n- (E = Si, Ge, Sn, Pb; n = 2, 3, 4) have already shown interesting and diverse reactivity and have been at the forefront of rapidly developing and exciting new chemistry.3-6 Notable milestones are the oxidative coupling of Ge94- clusters to oligomers and infinite chains,7-19 their metallation,14-16,20-25 capping by transition-metal organometallic fragments,26-34 insertion of a transition-metal atom at the center of the cluster which is sometimes combined with capping and oligomerization,35-47 addition of main-group organometallic fragments as exo-bonded substituents,48-50 and functionalization with various organic residues by reactions with organic halides and alkynes.51-58 
This latter development of attaching organic fragments directly to the clusters has opened up a new field, namely organo-Zintl chemistry, that is potentially fertile for further synthetic explorations, and it is the step-by-step procedure for the synthesis of germanium-divinyl clusters described herein. The initial steps outline the synthesis of an intermetallic precursor of K4Ge9 from which the Ge94- clusters are extracted later in solution. This involves fused-silica glass blowing, arc-welding of niobium containers, and handling of highly air-sensitive materials in a glove box. The air-sensitive K4Ge9 is then dissolved in ethylenediamine in the box and then alkenylated by a reaction with Me3SiC&equiv;CSiMe3. The reaction is followed by electrospray mass spectrometry while the resulting solution is used for obtaining single crystals containing the functionalized clusters [H2C=CH-Ge9-CH=CH2]2-. For this purpose the solution is centrifuged, filtered, and carefully layered with a toluene solution of 18-crown-6. Left undisturbed for a few days, the so-layered solutions produced orange crystalline blocks of [K(18-crown-6)]2[Ge9(HCCH2)2]&bull;en which were characterized by single-crystal X-ray diffraction. 
The process highlights standard reaction techniques, work-up, and analysis towards functionalized deltahedral Zintl clusters. It is hoped that it will help towards further development and understanding of these compounds in the community at large.

We present the high-temperature synthesis of intermetallic precursors K4Ge9, their dissolution in ethylenediamine to form Ge94- deltahedral Zintl ions, and the reaction of the clusters with alkynes to form organo-Zintl ions. The latter are characterized by electrospray mass spectrometry in solutions and by single-crystal X-ray diffraction in the solid state.

Synthese von neunatomige deltaedrischen Zintl-Ionen von Germanium und deren Funktionalisierung mit organischen Gruppen

Although the first studies of Zintl ions date between the late 1890's and early 1930's they were not structurally characterized until many years later.1,2 ...

Herstellung von synthetischen Kernschmelzglas

Zusammenfassung

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