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.

Precaución: El proceso descrito aquí incluye el uso de material radiactivo (por ejemplo, hexahidrato de nitrato de uranio) y varias sustancias corrosivas. Ropa de protección adecuada y el equipo deben ser utilizados (incluyendo una bata de laboratorio, guantes, protección para los ojos, y una campana de humos) durante la preparación de la muestra. Además, las áreas de laboratorio utilizados para este trabajo deben ser controlados regularmente por la contaminación radiactiva. Nota:. Los compuestos químicos necesarios se enumeran en la Tabla 1 Esta formulación se desarrolló mediante el examen previamente reportó datos de composición para trinitita 10 Las fracciones de masa aquí presentados fueron determinados por un promedio de las fracciones de masa de varias muestras trinitita diferentes 10 La masa &quot;desaparecidos&quot;.. (las fracciones que no suman a la unidad) existe para permitir cierta flexibilidad a la hora de agregar combustible, sabotaje, y otros componentes. Nuestro análisis independiente de varias muestras trinitita sugiere que el cuarzo es la única fase mineralsobrevivir en trinitita. 5 Por lo tanto, el cuarzo es el único mineral incluido en nuestra trinitita formulación estándar (STF). Aunque granos reliquia de otros minerales han sido reportados en trinitita, 11 estos tienden a ser la excepción, no la regla. En general, el cuarzo es el único mineral que se encuentra en el vidrio fundido. 10,12 Además, la arena de cuarzo es un componente común de asfalto y hormigón que será importante en la formación de la masa fundida de vidrio nuclear urbana. <table fo:keep-together.within-page="1"><tbody><tr height="41"><td colspan="2" height="41" style="height:42px;width:317px;"> Promedió datos trinitita </td><td colspan="2" style="width:317px;"> Estándar trinitita Formulación (STF) </td></tr><tr height="22"><td height="22" style="height:22px;width:159px;"> Compuesto </td><td style="width:159px;"> Fracción de masa </td><td style="width:159px;"> Compuesto </td><html><td style="width:159px;"> Fracción de masa </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;"> Na2O </td><td style="width:159px;"> 1.25x10 -2 </td><td style="width:159px;"> Na2O </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;"> Total </td><td style="width:159px;"> 9.81x10 -1 </td><td style="width:159px;"> Total </td><td style="width:159px;"> 9.91x10 -1 </td></tr></tbody></table> Tabla 1. Lista de compuestos químicos. 1. Preparación de la STF Nota: El equipo necesario incluye una microbalanza, espátulas de metal, un mortero y una maja de cerámica, una campana de humos químicos, guantes de látex, una bata de laboratorio y protección para los ojos. <ol><li> La mezcla de componentes no radiactivos <ol><li> Adquirir al menos 65 g de arena de cuarzo (SiO2), 15 g de Al 2 O 3 &lt;/ sub&gt; en polvo, 10 g de polvo de CaO, 2 g de polvo de FeO, 2 g de polvo de MgO, 2 g de Na 2 polvo de O, 7 g de gránulos de KOH, 1 g de polvo de MnO y 1 g de TiO 2 en polvo ( compuestos enumerados en la Tabla 1). </li><li> Utilice una microbalanza y pequeña espátula para medir con precisión las fracciones de masa de cada compuesto enumerados en la Tabla 1. Para obtener los mejores resultados preparan 100 g de la matriz de precursor no radiactivo al mismo tiempo. </li><li> Use un mortero para pulverizar (a ~ 10-20 gránulos de tamaño de micras) ya fondo mezclar los compuestos, formando una mezcla en polvo homogénea que contiene 64,2 g de SiO2, 14,2 g de Al 2 O 3, 9.64 g de CaO, 1,97 g de FeO, 1,15 g de MgO, 1,25 g de Na 2 O. 6,12 g de KOH, 0,0505 g de MnO, y 0,427 g de TiO 2. </li><li> Agitar la mezcla, utilizando un mezclador de bola, poco antes de que se tome la siguiente etapa. </li></ol></li><li> La mezcla del STF con uranio nitrato hexahidrato (UNH) <ol><li> Acquire al menos 1 g de UNH. </li><li> Dentro de una campana de humos, pulverizar unos pocos cristales UNH (utilizando un mortero y almirez) para formar un polvo fino de 1-2 micras gránulos. </li><li> Añadir 33.75 g de UNH por gramo de la matriz de precursor no radiactivo (esta relación es apropiado para la simulación de un arma simple con un rendimiento de 1 kilotones). 13 </li><li> Mezclar bien la mezcla de polvo, incluyendo la UNH, utilizando un mortero. Completar mezcla final poco antes de la etapa de fusión. </li></ol></li></ol> 2. La producción de 1 gramo Melt Glass Muestra Nota: El equipo necesario incluye una HTF nominal de 1.600 ° C o superior, crisoles de alta pureza de grafito, acero inoxidable largas pinzas, guantes resistentes al calor y protección para los ojos. Guantes resistentes al calor y protección para los ojos se deben usar al introducir o extraer muestras del horno. Gafas de seguridad tintados (o gafas de sol) son útiles, ya que reducen el resplandor del horno. <ol><li> Producción de una muestra no radiactivo <ol><li> Llenar un plato de cerámica gruesa (tal como un mortero) con ~ 100 g de arena de cuarzo puro y mantener a temperatura ambiente cerca de la ubicación del horno donde se fundieron las muestras. </li><li> Precaliente el HTF a 1500 ° C. </li><li> Mida cuidadosamente 1,00 g de la mezcla de polvo no radiactivo y colocar el polvo en un crisol de grafito de alta pureza. </li><li> Coloque cuidadosamente el crisol en el HTF climatizada (con un largo par de pinzas de crisol de acero) y derretir la mezcla durante 30 min. </li><li> Retire la muestra (de nuevo utilizando las pinzas) y verter la muestra fundida en el mortero lleno de arena. </li><li> Deje que la cuenta de vidrio se enfríe durante 1-2 minutos antes de manipular. </li><li> Pulir el grano para eliminar la arena residual (si es necesario). </li></ol></li><li> Producción de una muestra radiactiva <ol><li> Repita los pasos 2.1.1 y 2.1.2. </li><li> Mida cuidadosamente 1,00 gramo de la mezcla de polvo radiactivo (incluyendo UNH) y colocar el powd<html> er en un crisol de grafito de alta pureza con una espátula y microbalanza separada para evitar la contaminación cruzada. </li><li> Repita los pasos 2.1.4 - 2.1.6 arriba. </li><li> Monitorear el área alrededor del horno (usando un detector de mano de radiación y / o ensayos de banda magnética) para comprobar si hay contaminación radiactiva. </li></ol></li></ol> Activación 3. Muestra Nota: Las ecuaciones que siguen se obtuvieron asumiendo el uso de armas de grado (enriquecido) uranio metálico. Tendrá que ser reducido de acuerdo con la fracción de masa de uranio elemental y el nivel de enriquecimiento de U 235 Las cantidades de UNH u óxido de uranio. <ol><li> La activación de una muestra del derretimiento de vidrio con uranio Fue <ol><li> Calcular la fracción de masa de uranio metálico requerido para la muestra usando la siguiente ecuación 13 (donde m U representa la fracción de masa de uranio y Y representa el rendimiento arma): 473 / 53473eq1.jpg &quot;/&gt; </li><li> Opcional: Se calcula la fracción de masa de manipulación indebida (por ejemplo, el uranio natural, plomo, tungsteno) utilizando la siguiente ecuación: 13 <img alt="Ecuación 2" src="/files/ftp_upload/53473/53473eq2.jpg" /></li><li> Calcular el número objetivo de fisiones en la muestra usando la siguiente ecuación 13 donde M s representa la masa de la muestra en gramos y N f representa el número de fisiones que se producen en la muestra durante la irradiación: <img alt="Ecuación 3" src="/files/ftp_upload/53473/53473eq3.jpg" /></li><li> Calcular el tiempo de irradiación necesario utilizando la siguiente ecuación 13 donde m 235 representa la fracción de masa 235 U (nivel de enriquecimiento) y t TIR es el tiempo de irradiación en segundos: <img alt="Ecuación 4" src="/files/ftp_upload/53473/53473eq4.jpg" /></li><li> Irradiar la muestra paraT segundos IRR a un flujo de neutrones térmicos de 4,0 x 10 14 n / cm 2 / s. Por ejemplo, una irradiación de 60 seg en Pneumatic Tubo 1 (PT-1) en HFIR (con una térmica a la resonancia relación de 35) producirá aproximadamente 1,1 x 10 11 fisiones en una muestra que contiene 870 g de UNH (equivalente a 410 mg de uranio natural, o 3,0 g de 235 U). Esto se ha logrado por una perla de vidrio 0,433 g diseñado para simular una muestra de vidrio de fusión producida por un arma con un rendimiento 0,1 kilotones. Esta muestra se ha analizado a fondo por Cook et al. 14 </li><li> Siga los protocolos de seguridad vigentes para el manejo de la muestra radiactiva después de la irradiación. </li></ol></li><li> La activación de una muestra del derretimiento de cristal con plutonio de combustible (Factores de Planificación) <ol><li> Calcular la fracción de masa de plutonio metal requerido para la muestra usando la siguiente ecuación 13 donde m represen Puts la fracción de masa de plutonio e Y representa el rendimiento arma: <img alt="Ecuación 5" src="/files/ftp_upload/53473/53473eq5.jpg" /></li><li> Repita los pasos 3.1.2 y 3.1.3 anteriores. </li><li> Determinar el tiempo de irradiación necesario para obtener el número deseado de fisiones en la muestra de vidrio fundido. Este tiempo dependerá de la composición y el grado del plutonio, así como el espectro de energía de neutrones. </li></ol></li></ol> Nota: Gran se debe tener cuidado cuando se trata de plutonio y análisis adicional será requerida. Al escribir estas líneas, sólo el uranio se ha utilizado en las muestras de vidrio de fusión sintéticos producidos en UT y irradiados en HFIR.

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</ol>

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

Nota respecto a los pasos 1.2.2 y 1.2.3: La cantidad exacta de UNH variará dependiendo del escenario que se está simulando. Las fórmulas de planificación desarrollados por Giminaro et al. Se pueden utilizar para elegir la masa adecuada de uranio para una muestra dada 13 como se explica en la sección &quot;Activación de ejemplo&quot; de este artículo. También, óxido de uranio (UO 2 o U 3 O 8) se puede utilizar en lugar de UNH, si está disponible, y la fracci?...

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.

Las muestras no radiactivos producidos en este estudio han sido comparados con trinitita y las Figuras 1-3 muestran que las propiedades físicas y la morfología son, en efecto similar. La Figura 1 proporciona fotografías que revelan las similitudes en color y textura que se observan a nivel macroscópico. La figura 2 muestra microscopio electrónico de barrido (SEM) Imágenes secundarias Electron (SE) que revelan características similares a nivel mic...

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.

Producción de masa fundida de vidrio sintético Nuclear

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

Research

JoVE Journal

Engineering

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

Video: 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.

Métodos Ex Situ e In Situ las investigaciones de las transformaciones estructurales: el caso de la cristalización de vidrios metálicos

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

Investigación

Ingeniería

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.

Sales fundidas síntesis de nanopartículas de óxidos metálicos complejos

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

Química

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.

Proceso de sellado optimizado y monitoreo en tiempo real de estructuras de sello de vidrio a metal

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.

Comparación de dos métodos de síntesis diferentes de cristales individuales de diteluro de uranio superconductor

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

Síntesis hidrotermal de nanopartículas luminiscentes persistentes

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 destacado: Avance de la bioimagen y la terapia con nanomateriales funcionales

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.

Síntesis de nanopartículas luminiscentes persistentes para pantallas regrabables y aplicaciones de iluminación

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.

Espectroscopía Raman de celda fluida para estudios de fenómenos de reacción y transporte durante la corrosión por vidrio de silicato

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.

Fabricación de superficies de cristal de calidad óptica para estudiar la fusión de macrófagos

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

Inmunología e Infección

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.

Síntesis de Deltahedral de nueve átomos de germanio Zintl iones y su funcionalización con grupos orgánicos

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 ...

Producción de masa fundida de vidrio sintético Nuclear

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