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.

注意：ここで説明するプロセスは、放射性物質の使用（例えば、ウラン六水和物）と、いくつかの腐食性物質を含んでいます。適切な防護服や機器は、サンプル調製中（白衣、手袋、眼の保護、およびヒュームフードを含む）を使用する必要があります。また、この作業に使用実験室面積は放射能汚染のために定期的に監視する必要があります。 注：必要に応じて化学化合物を 、表1に記載されているこの製剤は、先に検討することによって開発されたトリニタイトための組成データを報告し、ここで報告された10質量分率は、いくつかの異なるトリニタイトサンプルの質量分率を平均することによって決定された10 &quot;欠落&quot;塊。 （画分が1に合計しないように）燃料、タンパーを追加する際にある程度の柔軟性を可能にするために存在し、他の成分。いくつかのトリニタイトサンプルの我々の独立した分析は、石英のみ鉱物相であることを示唆していますトリニタイトで生存する。5そこで、石英は、当社の標準トリニタイト製剤（STF）に含まれる唯一の鉱物です。他の鉱物の遺物粒がトリニタイトで報告されているが、11これらは例外ではなく、ルールになる傾向があります。一般的には、石英、溶融ガラスに見られる唯一の鉱物である。10,12また、石英砂は、都市核溶融ガラスの形成に重要となるアスファルトやコンクリートの一般的な構成要素です。 <table fo:keep-together.within-page="1"><tbody><tr height="41"><td colspan="2" height="41" style="height:42px;width:317px;"> 平均化トリニタイトデータ </td><td colspan="2" style="width:317px;"> 標準トリニタイト製剤（STF） </td></tr><tr height="22"><td height="22" style="height:22px;width:159px;"> 化合物 </td><td style="width:159px;"> 質量分率 </td><td style="width:159px;"> 化合物 </td><html><td style="width:159px;"> 質量分率 </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;のFeO </td><td style="width:159px;"> 1.97x10 -2 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;"> MgOの</td><td style="width:159px;"> 1.15x10 -2 </td><td style="width:159px;"> MgOの</td><td style="width:159px;"> 1.15x10 -2 </td></tr><tr height="26"><td height="26" style="height:26px;width:159px;"> Na 2 Oを</td><td style="width:159px;"> 1.25x10 -2 </td><td style="width:159px;"> Na 2 Oを</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の</td><td style="width:159px;"> 4.27x10 -3 </td><td style="width:159px;"> TiO 2の</td><td style="width:159px;"> 4.27x10 -3 </td></tr><tr height="25"><td height="25" style="height:25px;width:159px;">トータル</td><td style="width:159px;"> 9.81x10 -1 </td><td style="width:159px;">トータル</td><td style="width:159px;"> 9.91x10 -1 </td></tr></tbody></table>化合物の表1。リスト。 STFの調製注意：必要な機器は、マイクロバランス、金属ヘラ、セラミック乳鉢と乳棒、化学ヒュームフード、ゴム手袋、白衣、および眼の保護が含まれています。 <ol><li>非放射性成分の混合<ol><li>石英砂の少なくとも65グラム（SiO 2）ではAl 2 O 3を15gを取得&lt;/サブ&gt;粉末、酸化カルシウム粉末10g、のFeO粉末2g、MgO粉末2gを、Na 2 Oを粉末2g、KOHペレット7gの、酸化マンガン粉末1g及びTiO 2粉末1g（ 表1に列挙した化合物）。 </li><li> 表1に記載されているように正確に、各化合物の質量分率を測定するために、微量天秤と小さなへらを使用してください。最良の結果を一度に非放射性前駆体マトリックスの100グラムを準備するために。 </li><li> （〜10〜20ミクロンのサイズの顆粒に）粉砕する乳鉢と乳棒を使用して、徹底的に化合物を混合し、SiO 2を64.2グラムを含む均質な粉末混合物を形成する、 の Al 2 O 3、CaOを、1.97グラムの9.64グラムの14.2グラムFeO、MgOを1.15グラム、のNa 2 Oを 1.25グラムのKOHの6.12グラム、のMnOの0.0505グラム、及びTiO 2の0.427グラム。 </li><li>次のステップが取られる直前に、ボールミキサーを使用して、混合物を撹拌します。 </li></ol></li><li>ウラン六水和物（UNH）とSTFの混合<ol><li> AcquUNHの少なくとも1gをIRE。 </li><li>ヒュームフードの内側には、1〜2μmで顆粒の微粉末を形成する（乳鉢と乳棒を使用して）いくつかのUNH結晶を粉砕。 </li><li> （この比率は1キロトンの収率で単純な武器をシミュレートするために適切である）非放射性前駆体マトリックスのグラム当たりUNHの33.75μgのを追加します。13 </li><li>乳鉢と乳棒を用いて、UNH含む、粉末混合物を混ぜます。溶融工程の直前に最終混合を完了します。 </li></ol></li></ol> 1グラムメルトガラスサンプルの2生産注意：必要な機器は、1,600℃以上、高純度黒鉛ルツボ、長いステンレス製るつぼトング、耐熱手袋、眼の保護定格HTFが含まれています。炉からサンプルを導入するか、削除する際に耐熱手袋と目の保護を着用してください。彼らは炉からのまぶしさを軽減としてティント安全ゴーグル（または太陽メガネ）が便利です。 <ol><li>非放射性サンプルの製造<ol><li>純粋な石英砂の〜100gで（例えばモルタルなど）の厚さのセラミックの皿を記入し、試料が溶融される炉の場所の近くに、室温で維持します。 </li><li> 1,500℃に予熱HTF。 </li><li>慎重に非放射性粉末混合物の1.00グラムを測定し、高純度の黒鉛坩堝に粉末を配置します。 </li><li>慎重に（鋼るつぼトングの長い対を用いて）加熱HTFでるつぼを配置し、30分間混合物を溶融します。 </li><li> （再びトングを使用して）サンプルを削除し、砂を充填したモルタルへの溶融サンプルを注ぎます。 </li><li>ガラスビーズを取り扱​​う前に1〜2分間冷却してください。 </li><li> （必要な場合）の残留砂を除去するために、ビーズを磨きます。 </li></ol></li><li>放射性試料の作製<ol><li>繰り返しは、上記の2.1.1と2.1.2手順。 </li><li>慎重に（UNH含む）放射性粉末混合物の1.00グラムを測定し、powdを配置<html>相互汚染を避けるために、別個のへらと天秤を用いて高純度黒鉛坩堝におけるER。 </li><li>上記2.1.6 - を繰り返し2.1.4手順。 </li><li>放射能汚染をチェックする（手持ち放射線検出器および/またはスワイプアッセイを用いて）炉の周囲の領域を監視します。 </li></ol></li></ol> 3.サンプルのアクティベーション注：下記の式は、兵器級（濃縮）ウラン金属の使用を想定して誘導しました。 UNHまたは酸化ウランの量は、元素のウランの質量分率と235 U濃縮のレベルに応じてスケーリングする必要があります。 <ol><li>ウラン笛でメルトガラス試料の活性化<ol><li> （mは Uウラン質量分率を表し、Yは、武器の収率を示す）13以下の式を使用して、サンプルに必要なウラン金属の質量分率を計算します。 473 / 53473eq1.jpg &quot;/&gt; </li><li>オプション：以下の式を使用して、タンパ（例えば、天然ウラン、鉛、タングステン）の質量分率を計算します。13 <img alt="式（2）" src="/files/ftp_upload/53473/53473eq2.jpg" /></li><li> M sはグラムでのサンプルの質量を表し、N fは照射の間、サンプルにおいて生成さ核分裂の数を表し、以下の式13を用いて試料中の核分裂の目標数を計算します。 <img alt="式3" src="/files/ftp_upload/53473/53473eq3.jpg" /></li><li> M 235が 235 Uの質量分率（濃縮レベル）を表し、Tの IRRは、秒単位の照射時間である13以下の式を使用して、必要な照射時間を計算します。 <img alt="式（4）" src="/files/ftp_upload/53473/53473eq4.jpg" /></li><li>以下のためのサンプルを照射4.0×10 14 N / cmで2 /秒の熱中性子束にIRR秒のt。例えば、（35の共振比が熱を持つ）HFIRで気送管1（PT-1）で60秒照射はUNHの870μgの410μgのに（等価を含む試料では約1.1×10 11核分裂が生成されます天然ウラン、または235 Uの3.0μgの）。これは、0.1キロトンの収率で武器によって生成溶融ガラスサンプルをシミュレートするように設計された1つ0.433グラムのガラスビーズのために達成されています。この試料を十分にクックらによって分析された。14 </li><li>放射性試料照射後の処理に適用される安全なプロトコルに従ってください。 </li></ol></li><li>プルトニウム燃料（計画要因）とメルトガラス試料の活性化<ol><li> 13 ここで、m プルトニウム represen以下の式を使用して、サンプルに必要なプルトニウム金属の質量分率を計算しますプルトニウム質量分率TS と Y は、武器の収量を表しています。 <img alt="式（5）" src="/files/ftp_upload/53473/53473eq5.jpg" /></li><li>手順を繰り返し上記の3.1.2と3.1.3。 </li><li>溶融ガラス試料中の核分裂の所望の数を得るために必要な照射時間を決定します。この時間は、組成やグ​​レードプルトニウムだけでなく、中性子エネルギースペクトルに依存します。 </li></ol></li></ol>注意：必要とされるプルトニウム、追加の分析を扱うときに細心の注意を払うべきです。この記事の執筆時点では、唯一のウランは、合成溶融ガラス試料UTで生産し、HFIRで照射に使用されています。

<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).

ステップ1.2.2と1.2.3に関する注意：UNHの正確な量は、シミュレートされるシナリオによって異なります。 Giminaro らによって開発された計画の式は、このペーパーの「サンプル活性化」の項で説明したように、与えられたサンプル13のためのウランの適切な量を選択するために使用することができます。また、酸化ウラン（UO 2またはU 3 O 8）が利用可能な?...

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.

本研究で生産非放射性サンプルはトリニタイトに比べて1〜3は、物理的特性および形態が実際に類似していることを示しますされている。 図1は、巨視的レベルで観察された色と質感の類似性を明らかに写真を提供します。 図2は、ミクロンレベルでの類似の特徴を明らかに走査型電子顕微鏡（SEM）二次電子（SE）画像を示します。 SEM分析は?...

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.

合成核メルトガラスの製造

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

ビデオ: 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.

Ex その場その場で調査構造変換の方法: 金属ガラスの結晶化の事例

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

工学

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.

複合金属酸化物ナノ粒子の溶融塩合成

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

化学

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.

ガラスから金属へのシール構造の最適化されたシールプロセスとリアルタイムモニタリング

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.

超伝導ジテルル化ウラン単結晶の合成方法の比較

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

持続性発光ナノ粒子の水熱合成

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.

著者スポットライト:機能性ナノ材料によるバイオイメージングと治療の進歩

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.

リライタブルディスプレイおよび照明アプリケーションのための持続性発光ナノ粒子の合成

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.

オペランド用流体セルラマン分光法 : ケイ酸塩ガラス腐食時の反応・輸送現象の研究

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.

マクロファージの融合を研究するための光学的品質ガラス表面を加工

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

免疫・感染学

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.

ゲルマニウムと有機基との官能の9原子Deltahedral Zintlイオンの合成

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 ...

合成核メルトガラスの製造

要約

さらに動画を探す

Ex その場その場で調査構造変換の方法: 金属ガラスの結晶化の事例

複合金属酸化物ナノ粒子の溶融塩合成

ガラスから金属へのシール構造の最適化されたシールプロセスとリアルタイムモニタリング

超伝導ジテルル化ウラン単結晶の合成方法の比較

リライタブルディスプレイおよび照明アプリケーションのための持続性発光ナノ粒子の合成

リライタブルディスプレイおよび照明アプリケーションのための持続性発光ナノ粒子の合成

リライタブルディスプレイおよび照明アプリケーションのための持続性発光ナノ粒子の合成

オペランド用流体セルラマン分光法 : ケイ酸塩ガラス腐食時の反応・輸送現象の研究

マクロファージの融合を研究するための光学的品質ガラス表面を加工

ゲルマニウムと有機基との官能の9原子Deltahedral Zintlイオンの合成