The authors acknowledge National Science Foundation grant CHE- 1214068 for supporting this research project.

GMSの調製<ol><li>受け取った次のプロセスですべての化学物質を使用してください。 </li><li>塩酸（HCl）溶液を2 Mの75ミリリットルを準備します。ポリ（エチレングリコール）を2.0gを秤量 - ブロック - ポリ（プロピレングリコール） - ブロック - ポリ（エチレングリコール）（P123、MW = 5,800）および2MのHCl溶液の調製75ミリリットルに移します。 P123が完全に溶解するまで室温で、350 R /分の速度で溶液を磁気攪拌を適用します。溶液は透明になります。 </li><li>小瓶転送ビスの180μlのテトラエトキシシランの4グラム（TEOS、MW = 208.33）を計量[3-（トリエトキシシリル）プロピル] - テトラスルフィド（TESPTS、MW = 538.94）をバイアルに。ゆっくりと2種類の化学物質を混合するために、バイアルを振ります。別のバイアルでは、塩化金酸38mgの（のHAuCl 4、99.90パーセント）を計量し、脱イオン水1mlに溶解します。 </li><li>熱電対によって制御された温度で油浴中で35℃にP123液の温度を上昇させます。 </li><li> TEOSの混合物のすべてを追加し、TESPTSはP123溶​​液にステップ1.3で調製し、700 R /分の激しい磁気撹拌で溶液を維持します。 2分間攪拌し、溶液を維持し、その後、30秒以内にステップ1.3を滴下で製造したのHAuCl 4溶液のすべてを追加します。 </li><li> 35℃で24時間、700 /分（rpm）で撹拌し、溶液を保管してください。 </li><li> 24時間後、72時間、100℃に設定したオーブンで密封されたボトルとストアにソリューションを転送します。これは、熱水処理と呼ばれています。 </li><li>熱水処理の後、残ったHClを除去するために二度、エタノールを水で3回洗浄し、その後、漏斗の下＃1濾紙負圧で溶液を濾過します。各洗浄工程の間、固体の上に水またはエタノール1cmに追加して、材料が乾燥するのを待ちます。 </li><li> 4時間550℃でセラミック坩堝や焼物に濾過からの沈殿を転送します。 25°Cを550℃に2時間、4、550℃で保つ次のようランププログラムを設定します時間は、その後、温度が40℃を下回るまで、ドアを閉じた状態で試料を炉内に残ることができます。 </li><li>焼成後、プラスチックスパチュラでガラスバイアルに製品を移します。合成された物質は、赤色を有します。 </li></ol> 2.触媒反応、ベンジルアルコールの酸化<ol><li>ベンジルアルコールの酸化は、別々の無溶媒液相反応でベンジルアルコールの尺度5ミリリットル（99.8％）、25 mlの三つ口フラスコにそれを転送するので、次にGMS触媒10mgを秤量し、それがベンジルに追加アルコール。 </li><li>反応温度の正確かつ均一な制御を確実にするために、磁気撹拌しながら、温度制御された油浴を設定します。 </li><li>油浴中にベンジルアルコール及び触媒をフラスコに入れ、次いで100℃に温度を設定し、150 R /分で撹拌。 </li><li>マスフローコントローラにより制御2ml /分でフラスコに99.9％の純度を有する酸素ガスフロー。 </li><li>いつ油浴の温度が100℃に達し、安定化、三口フラスコ内に酸素ガスを導入します。 </li><li>酸素流量と温度を一定に維持し、反応を6時間進行させます。 </li><li>反応後、＃1の濾過紙で製品をフィルタリングします。液相を収集し、ガスクロマトグラフィー（GC）バイアルにアリコートを移します。 GCバイアル中で、一人一人の部分のサンプルについて四つの部分のHPLCグレードの酢酸を混合（例えば、36μlのサンプルと144μlの酢酸を使用しています。）分析のためのガスクロマトグラフのオートサンプラーにバイアルを置きます。 DI水とエタノールでろ紙上に固体沈殿物を洗い流した後、空気中で乾燥させます。リサイクル触媒としてスパチュラで乾燥した固体を収集します。 </li><li>リサイクル触媒と2.7を介してステップ2.3から3回同じ実験手順を繰り返します。各繰り返しにおいて、ステップ2.2に記載の比率と一致するように、ベンジルアルコールの量を調整します。 </li></ol> 3. THER熱安定性の試験のためのGMSの発作治療<ol><li>合成されたGMSの3つの別々の300mgの部分を計量し、ガラスバイアルに保存します。これらは、対照群として、バッチ1、バッチ2及びバッチ3キープバッチ1としてマークされ、熱処理炉にバッチ2及びバッチ3を入れています。 </li><li>プログラム400℃での処理のために次のように炉：、0.5時間で400℃まで25℃から上昇4時間400℃で維持し、ドアが温度低下するまで閉じた状態の試料を炉内に残ることを可能40℃以下。るつぼにバッチ2を入れて、プログラムを起動します。 </li><li> 650℃での処理のために次のように炉プログラム：ドアを閉じた状態で温度を下回るまで、650°Cまで25°Cからランプを0.75時間では、4時間650℃で維持するには、試料を炉中に残存することを可能にします40°C。るつぼにバッチ3を入れ、プログラムを起動します。 </li></ol> 4.特性GMS材料21,22の<ol><li> 60分間の90℃、480分間、次いで350°C：物理吸着装置で、ドガは、以下のプログラムを有する材料をGMS。物理吸着データを取得するために脱気した材料でフル等温線分析を実行します。 </li><li> 200メッシュ穴あき炭素TEMグリッド上にGMS試料を分散し、透過型電子顕微鏡でサンプルを観察します。材料を保護するために44,000X下倍率を制限します。 </li><li> CuKα線（λ= 1.5418オングストローム）を使用して実行XRD。セット45 kVの管電圧、および40ミリアンペアの管電流。 0.008°のステップサイズと各ステップで5秒の測定時間で10°と90°の間の2θ範囲内の強度を収集します。 </li></ol>

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The authors have nothing to disclose.

合成プロトコル内では、界面活性剤濃度、溶液のpH、反応温度への配慮は、GMSの成功形成に重要です。重要なステップは、1.2、1.3、1.4および1.6です。上記のパラメータは、界面活性剤から形成されたミセルの臨界充填パラメータと位相を制御します。ミセルの位相および形態は、GMSのためのフレームワークとして機能するシリカマトリックスの最終状態が決定されます。また、形成プロセス?...

触媒用途において大きな可能性を秘めている新興技術として、ナノスケール材料は、過去数十年間で集中的な研究の関心を受けています。報告されたナノスケールの触媒の中で、例えば、Au、Ag、PdおよびPtのような貴金属触媒は、ワールドワイド1-3注目を集めています。触媒反応を選択したPtとPdを触媒上のAu、ヘック反応、および水分解の一酸化炭素の研究者の酸化が含まれます。有望な触媒の可能性にもかかわらず、ナノスケール金が原因で中毒、コーキング、熱分解、焼結から不活性化への適用に限定されています。それは金、貴金属のための代表として、高い選択性を有することが報告と金属浸出、過酸化、および自己中毒4にくいされています。しかし、金の触媒性能が強く、粒子サイズに依存します。春田らは、触媒性能との関係を報告して行きましたLDクラスター径、粒径2.7nmで5〜に金触媒の最高活性を示します。 貴金属の粒子径は、製造方法6-9により制御することができます。しかし、幅広いアプリケーションへの大きな障害は、凝集および活性の喪失のまま。焼結の問題を解決するために、一般的な方法は、支持体材料上にナノ粒子を固定化することです。様々な担体材料は、ポリマー14、金属酸化物を12〜13を半導体、多孔質シリカ10〜11を含むグラフェン15カーボンナノチューブ16が適用されています。それは、熱的および化学的に安定した比較的不活性な、唯一の弱酸性であり、非常に明確に定義されたメソ/ミクロ多孔度を用いて調製することができるので、使用される材料の中でも、多孔質シリカが支持体として魅力的な材料です。多孔質構造は、金属粒子のための優れたサポートを提供していますが、またのサイズ選択的基質へのアクセスを付与します金属触媒。この選択は、これらの多孔質材料に関連同調性の特に有望です。多くの場合、金粒子は、このように、それが困難なシリカ19に金ナノ粒子を調製すること、シリカの表面17-18上で非常に移動可能であり、容易に高温に曝されたときに、非常に大きな（50+ nm）の非反応性粒子を形成することが見出されています。ムカジーらは、3-アミノプロピルトリメトキシシラン及び3-メルカプトプロピル-トリエトキシシランによりメソポーラスシリカMCM-41上に単分散金ナノ粒子の固定化を報告し、担持された金ナノ粒子を水素化反応に高活性であることが見出され、金のない浸出が認められませんでした反応20で。 メソポーラスシリカの表面改質の報告に続いて、我々は、金を調製するための方法メソポーラスシリカ（GMS）の壁にインターカレートを報告しました。また、メソポーラスシリカ担持アプローチは、スケーラブルなAPを提供しています潜在的に独立して触媒と多孔質環境を変更するローチ。触媒プロセスは、重要な経済的に重要であるので、メリットは広範囲に及ぶ可能性があります。 「グリーン」触媒を開発する能力は、環境に多大なプラスの影響を与える、重要な工業プロセスの経済性とリソース効率を向上させることになります。

<table><tbody><tr><td>poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol)</td><td>Aldrich</td><td>435465-250ML</td><td></td></tr><tr><td>tetraethoxysilane</td><td>TCI</td><td>201-083-8</td><td></td></tr><tr><td>bis[3-(triethoxysilyl)propyl]-tetrasulfide</td><td>GELEST</td><td>SIB1825.0-100GM</td><td></td></tr><tr><td>chloroauric acid</td><td>Aldrich</td><td>520918-1G</td><td></td></tr><tr><td>benzyl alcohol</td><td>Sigma-Aldrich</td><td>305197-1L</td><td></td></tr><tr><td>nitrogen physisorption</td><td>Micromeritics</td><td>Tristar II</td><td></td></tr><tr><td>X-ray diffraction</td><td>Philips</td><td>X&#039;Pert Pro</td><td></td></tr><tr><td>transmission electron microscopy</td><td>Philips</td><td>CM200</td><td></td></tr><tr><td>gas chromatography</td><td>Shimadzu</td><td>GC-2010</td><td></td></tr></tbody></table>

synthesis and catalytic performance of gold intercalated in the walls of mesoporous silica

有望な触媒活性ナノリアクターとしては、メソポーラスシリカ（GMS）中に挿入金ナノ粒子を首尾よく合成し、材料の特性を調べました。私たちは、メソポーラスシリカの壁に金ナノ粒子をインターカレートするために、1つのポット、ゾル - ゲル法を使用していました。合成を開始するために、P123は、ミセルを形成するための鋳型として使用しました。その後TESPTS金ナノ粒子をインターカレートする表面改質剤として使用しました。この工程に続いて、TEOSは酸性環境で重合プロセスを行ったシリカ源として添加しました。熱水処理、焼成後、最終生成物を得ました。いくつかの技術が金インターカレーメソポーラスシリカの多孔度、形態および構造を特徴づけるために使用されました。結果は、金のインターカレーション後のメソポーラスシリカの安定した構造を示しました。ベンチマーク反応としてベンジルアルコールを酸化して、GMSの材料は、高いセレクを示しtivityやリサイクル。

この方法は、癌（HCC4017）肺細胞対（HBEC30KT）正常でヘム合成のレベルを比較した。 図2は 、正常肺細胞（HBEC30KT）よりも癌細胞（HCC4017）においてヘム合成のより高いレベルを示しています。ヘム合成のレベルはまた、ミトコンドリアの脱共役カルボニルシアニド3-クロロフェニル（CCCP）の存在下で、正常細胞と癌細胞で測定しました。細胞は、ヘム合成のレベルを測定する前に24...

Watch this Scientific Journal Video about Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica at JoVE.com

Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

Here, we present a protocol with a sol-gel process to synthesize gold intercalated in the walls of mesoporous materials (GMS), which is confirmed to possess a mesoporous matrix with gold intercalated in the walls imparting great stability and recyclability.

合成とメソポーラスシリカの壁に金インターカレーの触媒性能

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties ...

synthesis-catalytic-performance-gold-intercalated-walls-mesoporous

Research

JoVE Journal

Chemistry

10.0K ビュー.  Colorado School of Mines. Here, we present a protocol with a sol-gel process to synthesize gold intercalated in the walls of mesoporous materials (GMS), which is confirmed to possess a mesoporous matrix with gold intercalated in the walls imparting great stability and recyclability.

ビデオ: Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

マイクロ波支援酸 - 触媒反応によりシリカナノ粒子の調製

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

化学

In Situ SIMS and IR Spectroscopy of Well-defined Surfaces Prepared by Soft Landing of Mass-selected Ions

Soft landing of mass-selected ions onto surfaces is a powerful approach for the highly-controlled preparation of materials that are inaccessible using conventional synthesis techniques. Coupling soft landing with in situ characterization using secondary ion mass spectrometry (SIMS) and infrared reflection absorption spectroscopy (IRRAS) enables analysis of well-defined surfaces under clean vacuum conditions. The capabilities of three soft-landing instruments constructed in our laboratory are illustrated for the representative system of surface-bound organometallics prepared by soft landing of mass-selected ruthenium tris(bipyridine) dications, [Ru(bpy)3]2+ (bpy = bipyridine), onto carboxylic acid terminated self-assembled monolayer surfaces on gold (COOH-SAMs). In situ time-of-flight (TOF)-SIMS provides insight into the reactivity of the soft-landed ions. In addition, the kinetics of charge reduction, neutralization and desorption occurring on the COOH-SAM both during and after ion soft landing are studied using in situ Fourier transform ion cyclotron resonance (FT-ICR)-SIMS measurements. In situ IRRAS experiments provide insight into how the structure of organic ligands surrounding metal centers is perturbed through immobilization of organometallic ions on COOH-SAM surfaces by soft landing. Collectively, the three instruments provide complementary information about the chemical composition, reactivity and structure of well-defined species supported on surfaces.

In Situ SIMS and IR Spectroscopy of Well-defined Surfaces Prepared by Soft Landing of Mass-selected Ions

Soft landing of mass-selected ions onto surfaces is a powerful approach for the highly-controlled preparation of novel materials. Coupled with analysis by in situ secondary ion mass spectrometry (SIMS) and infrared reflection absorption spectroscopy (IRRAS), soft landing provides unprecedented insights into the interactions of well-defined species with surfaces.

その場 SIMSおよび質量選択されたイオンのソフトランディングで調製し明確に定義された表面の赤外分光法における

Soft landing of mass-selected ions onto surfaces is a powerful approach for the highly-controlled preparation of materials that are inaccessible using ...

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

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large extinction coefficients which can be tuned across the visible spectrum. Research into the plasmonic enhancement of optical transitions has become popular, due to the possibility of altering and in some cases improving photo-absorption or emission properties of nearby chromophores such as molecular dyes or quantum dots. The electric field of the plasmon can couple with the excitation dipole of a chromophore, perturbing the electronic states involved in the transition and leading to increased absorption and emission rates. These enhancements can also be negated at close distances by energy transfer mechanism, making the spatial arrangement of the two species critical. Ultimately, enhancement of light harvesting efficiency in plasmonic solar cells could lead to thinner and, therefore, lower cost devices. The development of hybrid core/shell particles could offer a solution to this issue. The addition of a dielectric spacer between a gold nanoparticles and a chromophore is the proposed method to control the exciton plasmon coupling strength and thereby balance losses with the plasmonic gains. A detailed procedure for the coating of gold nanoparticles with CdS and ZnS semiconductor shells is presented. The nanoparticles show high uniformity with size control in both the core gold particles and shell species allowing for a more accurate investigation into the plasmonic enhancement of external chromophores.

The synthesis of uniform gold nanoparticles coated with semiconductor shells of CdS or ZnS is performed. The semiconductor coating is conducted by first depositing a silver sulfide shell and exchanging the silver cations for zinc or cadmium cations.

合成、キャラクタリゼーション、およびハイブリッドのAu / CdSのとAu / ZnSのコア/シェルナノ粒子の機能化

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

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

層状チタン酸透明フィルムの層間空間で凝集することなく金ナノ粒子のその場合成で

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

工学

Preparation of Functional Silica Using a Bioinspired Method

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally purify the same by acid elution. By combining sodium silicate with a polyfunctional bioinspired additive, silica is rapidly formed at ambient conditions upon neutralization. 
The effect of neutralization rate and biomolecule addition point on silica yield are investigated, and biomolecule immobilization efficiency is reported for varying addition point. In contrast to other porous silica synthesis methods, it is shown that the mild conditions required for bioinspired silica synthesis are fully compatible with the encapsulation of delicate biomolecules. Additionally, mild conditions are used across all synthesis and modification steps, making bioinspired silica a promising target for the scale-up and commercialization as both a bare material and active support medium.
The synthesis is shown to be highly sensitive to conditions, i.e., the neutralization rate and final synthesis pH, however tight control over these parameters is demonstrated through the use of auto titration methods, leading to high reproducibility in reaction progression pathway and yield. 
Therefore, bioinspired silica is an excellent active material support choice, showing versatility towards many current applications, not limited to those demonstrated here, and potency in future applications.

Here, we present a protocol to synthesize bioinspired silica materials and immobilize enzymes therein. Silica is synthesized by combining sodium silicate and an amine &#39;additive&#39;, which neutralize at a controlled rate. Material properties and function can be altered either by in situ enzyme immobilization or post-synthetic acid elution of encapsulated additives.

バイオインスパイアード法を用いた機能性シリカの作製

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally ...

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various precursor noble metal ions with reducing agents in a 1:1 (v/v) ratio results in the formation of metal gels within seconds to minutes compared to much longer synthesis times for other techniques such as sol-gel. Conducting the reduction step in a microcentrifuge tube or small volume conical tube facilitates a proposed nucleation, growth, densification, fusion, equilibration model for gel formation, with final gel geometry smaller than the initial reaction volume. This method takes advantage of the vigorous hydrogen gas evolution as a by-product of the reduction step, and as a consequence of reagent concentrations. The solvent accessible specific surface area is determined with both electrochemical impedance spectroscopy and cyclic voltammetry. After rinsing and freeze drying, the resulting aerogel structure is examined with scanning electron microscopy, X-ray diffractometry, and nitrogen gas adsorption. The synthesis method and characterization techniques result in a close correspondence of aerogel ligament sizes. This synthesis method for noble metal aerogels demonstrates that high specific surface area monoliths may be achieved with a rapid and direct reduction approach.

A rapid, direct solution-based reduction synthesis method to obtain Au, Pd, and Pt aerogels is presented.

Au、Pd、およびソリューションに基づく還元を介して Pt エアロゲルの迅速合成法

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

合成多孔性カーボンとシリカ マトリックスの表面特性

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

親和性金ナノ粒子の合成と特性化

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

表面有機金属化学の方法論を用いてシリカ支持触媒によるイミンメタセシス

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...

A Salt-Templated Synthesis Method for Porous Platinum-based Macrobeams and Macrotubes

The synthesis of high surface area porous noble metal nanomaterials generally relies on time consuming coalescence of pre-formed nanoparticles, followed by rinsing and supercritical drying steps, often resulting in mechanically fragile materials. Here, a method to synthesize nanostructured porous platinum-based macrotubes and macrobeams with a square cross section from insoluble salt needle templates is presented. The combination of oppositely charged platinum, palladium, and copper square planar ions results in the rapid formation of insoluble salt needles. Depending on the stoichiometric ratio of metal ions present in the salt-template and the choice of chemical reducing agent, either macrotubes or macrobeams form with a porous nanostructure comprised of either fused nanoparticles or nanofibrils. Elemental composition of the macrotubes and macrobeams, determined with x-ray diffractometry and x-ray photoelectron spectroscopy, is controlled by the stoichiometric ratio of metal ions present in the salt-template. Macrotubes and macrobeams may be pressed into free standing films, and the electrochemically active surface area is determined with electrochemical impedance spectroscopy and cyclic voltammetry. This synthesis method demonstrates a simple, relatively fast approach to achieve high-surface area platinum-based macrotubes and macrobeams with tunable nanostructure and elemental composition that may be pressed into free-standing films with no required binding materials.

A synthesis method to obtain porous platinum-based macrotubes and macrobeams with a square cross section through chemical reduction of insoluble salt-needle templates is presented.

多孔質白金ベースマクロビームおよびマクロチューブの塩鋳合成法

The synthesis of high surface area porous noble metal nanomaterials generally relies on time consuming coalescence of pre-formed nanoparticles, followed ...

合成とメソポーラスシリカの壁に金インターカレーの触媒性能

要約

さらに動画を探す

この動画の章

マイクロ波支援酸 - 触媒反応によりシリカナノ粒子の調製

その場 SIMSおよび質量選択されたイオンのソフトランディングで調製し明確に定義された表面の赤外分光法における

合成、キャラクタリゼーション、およびハイブリッドのAu / CdSのとAu / ZnSのコア/シェルナノ粒子の機能化

層状チタン酸透明フィルムの層間空間で凝集することなく金ナノ粒子のその場合成で

バイオインスパイアード法を用いた機能性シリカの作製

Au、Pd、およびソリューションに基づく還元を介して Pt エアロゲルの迅速合成法

合成多孔性カーボンとシリカマトリックスの表面特性

親和性金ナノ粒子の合成と特性化

表面有機金属化学の方法論を用いてシリカ支持触媒によるイミンメタセシス

多孔質白金ベースマクロビームおよびマクロチューブの塩鋳合成法

合成とメソポーラスシリカの壁に金インターカレーの触媒性能

要約

さらに動画を探す

この動画の章

マイクロ波支援酸 - 触媒反応によりシリカナノ粒子の調製

その場 SIMSおよび質量選択されたイオンのソフトランディングで調製し明確に定義された表面の赤外分光法における

合成、キャラクタリゼーション、およびハイブリッドのAu / CdSのとAu / ZnSのコア/シェルナノ粒子の機能化

層状チタン酸透明フィルムの層間空間で凝集することなく金ナノ粒子のその場合成で

バイオインスパイアード法を用いた機能性シリカの作製

Au、Pd、およびソリューションに基づく還元を介して Pt エアロゲルの迅速合成法

合成多孔性カーボンとシリカ マトリックスの表面特性

親和性金ナノ粒子の合成と特性化

表面有機金属化学の方法論を用いてシリカ支持触媒によるイミンメタセシス

多孔質白金ベースマクロビームおよびマクロチューブの塩鋳合成法

合成多孔性カーボンとシリカマトリックスの表面特性