我们感谢中国科学技术部国家重点研究 & 开发项目 (2016YFB0600305)、国家自然科学基金 (21573031 和21373038号) 提供的财政支持, 项目为大连市 (2016RD09) 和香港科技高等教育学院优秀人才 (SG1617105 和 SG1617127)。

警告:针对本白皮书所述化学品的正确处理方法、性质和毒性, 请参阅有关材料安全数据表 (MSDS)。使用的一些化学物质是有毒和致癌的, 必须特别注意。纳米材料可能会造成安全隐患和健康影响。应避免吸入和皮肤接触。必须采取安全防范措施, 如在油烟机中进行催化剂合成和用高压釜反应器进行催化剂性能评估。必须佩戴个人防护设备。
1. 制备镍0.97铌0.03O 催化剂, 其中 Nb: (镍 + 铌) 摩尔比率等于0.03
<ol><li>将0.161 克草酸铌 (V) 水合物与2.821 克硝酸镍混合在100毫升的去离子水中, 在250毫升的三颈圆底烧瓶中装有搅拌棒。</li>
	<li>搅拌溶液在 50 rpm 和70°c, 以溶解化合物, 直到沉淀消失, 使用一个加热磁力搅拌器。</li>
	<li>将温度迅速提高到80摄氏度, 速度为2摄氏度/分钟。</li>
	<li>加入混合基本溶液 [氢氧化铵 (50 毫升, 1.0 米) 和氢氧化钠 (50 毫升, 0.2 米)] 到反应混合物滴状直到镍/铌溶液的 pH 值达到9.0。</li>
	<li>搅拌反应混合物时, 将温度提高到120摄氏度, 在2摄氏度/分钟。</li>
	<li>搅拌反应混合物隔夜在 50 rpm 在120°c, 直到完全消失的绿色颜色的解决方案。</li>
	<li>进行电感耦合等离子体-光发射光谱 (ICP) 分析, 以评估溶液中剩余 Ni2 +和铌5 +离子的浓度, 确保剩余镍的完全沉淀硝酸盐.</li>
	<li>用 Büchner 瓶过滤收集固体。在20分钟内重复添加2升去离子水, 以去除残留 Na+阳离子, 以洗涤固体。</li>
	<li>在手表玻璃中收集固体。干燥的固体在110°c 12 小时在干燥的烤箱。</li>
	<li>将合成空气中的固体加热 (20 毫升/分钟2和80毫升/分 N2) 的煅烧, 在450摄氏度为 5 h 在管式炉中。在使用高温反应之前, 检查所有玻璃器皿是否有缺陷。</li>
	<li>煅烧后, 获得1克镍0.97铌0.03O 催化剂。使用适当的防护设备, 如安全眼镜, 手套, 实验室大衣和油烟机, 以执行纳米晶反应, 由于潜在的安全隐患和健康影响的纳米材料。</li>
</ol>2. 制备镍0.92铌0.08O 催化剂, 其中 Nb: (镍 + 铌) 摩尔比率等于0.08
<ol><li>除前两个步骤外, 此过程与1类似:<ol>
<li>将0.43 克草酸铌 (V) 水合物溶解在100毫升的去离子水中。</li>
		<li>分别在100毫升去离子水中溶解2.675 克硝酸镍。</li>
	</ol>
</li>
</ol>3. 制备镍0.85铌0.15O 催化剂, 其中 Nb: (镍 + 铌) 摩尔比率等于0.15
<ol><li>除前两个步骤外, 该过程与1类似:<ol>
<li>将0.807 克草酸铌 (V) 水合物溶解在100毫升的去离子水中。</li>
		<li>分别在100毫升去离子水中溶解2.472 克硝酸镍。</li>
	</ol>
</li>
</ol>4. 制备镍0.80铌0.20O 催化剂, 其中 Nb: (镍 + 铌) 摩尔比率等于0.20
<ol><li>除前两个步骤外, 该过程与1类似:<ol>
<li>将1.076 克草酸铌 (V) 水合物溶解在100毫升的去离子水中。</li>
		<li>分别在100毫升去离子水中溶解2.326 克硝酸镍。</li>
	</ol>
</li>
</ol>5. 使用化学沉淀法制备 Nb2O5
<ol><li>煅烧铌酸 (Nb2O5·nH2O) 在合成空气中为 5 h 在450°c 获得纯 Nb2O5粒子。 注: 使用 X 射线粉末衍射 (XRD) 分析确认完成反应, 其中 nb2O5·nH2o 为无定形, nb2o5为晶体。根据分析, 在450摄氏度煅烧5小时足够完成反应。</li>
</ol>6. 合成β O-4 木质素模型化合物, 2-(2-methoxyphenoxy)-1-phenylethan-1-一
<ol><li>将 bromoacetophenone (9.0 克, 45 毫摩尔) 和 2-苯酚 (6.6 克, 53 毫摩尔) 在200毫升的甲基酰胺 (DMF) 中溶解, 用磁力搅拌器将其放在一个多锥瓶中。使用适当的防护设备和通风罩, 使用腐蚀性和致癌性的化学品和试剂进行反应。</li>
	<li>将上述 DMF 溶液与氢氧化钾 (3.0 克, 53 毫摩尔) 混合, 用磁性搅拌器在室温下以 50 rpm 的方式搅拌混合物。</li>
	<li>用分离漏斗提取200毫升的 H2O 和600毫升乙醚 (1:3, v/v) 的混合物溶液。获得溶液的上二乙基醚层。</li>
	<li>添加 MgSO4 (10 克) 以吸收二乙基醚溶液的水分。筛选 MgSO4以使用过滤纸和漏斗获得二乙醚溶液。</li>
	<li>用旋转蒸发器在0.08 兆帕斯卡的减压下除去二乙基醚溶液后, 将残留物溶解在5毫升乙醇中。</li>
	<li>慢慢蒸发乙醇溶剂, 结晶10毫升烧杯中的产品。获得产品 (11.5 克) 为黄粉, 产品产量为 90%, 基于 bromoacetophenone。从1h 核磁共振分析, 1h 核磁共振 (亚砜): δ 3.78 (s, 3H, 秒3), 5.54 (s, 2H, CH2), 6.82-8. 01 (m, 9H, 芳香) ppm。17
</li>
</ol>7. 木质素衍生芳香醚的加氢脱氧
注: 本实验中选用的木素衍生芳烃醚为甲醚, 催化剂为 Ni0.92铌0.08o 使用适当的保护设备和油烟机, 使用致癌试剂进行反应。
<ol><li>用加热器和磁力搅拌器装备一个50毫升不锈钢蒸压釜。</li>
	<li>将在 H2大气中的高压釜反应器中从步骤2获得的 Ni0.92铌0.08O 催化剂 (1 克) 减少400摄氏度, 然后在氩 (2 毫升/分钟) 一夜之间钝化催化剂。</li>
	<li>将甲醚 (1.1712 克, 8 wt%) 分解为 n-decane (20 毫升), 使用 n-烷基 (0.2928 克, 2 wt%) 作为定量气相色谱 (GC) 分析的内部标准。</li>
	<li>迅速将还原催化剂 (0.1 克) 引入高压釜反应器, 以避免长时间接触空气 (< 5 分钟)。</li>
	<li>密封釜式反应器, 用 H2重复清除 (3 次, 3 兆帕压力) 以消除空气, 然后在大气压下反应混合物。</li>
	<li>设置搅拌速度为 700 rpm。</li>
	<li>加热到期望的温度在160-210 °c 在2°c/分钟, 加压釜反应器到 3 MPa 并且设置零时间点 (t = 0)。 注: 本报告适用于160-210 摄氏度的温度范围。</li>
	<li>随后, 将混合物冷却到室温在10摄氏度/分钟, 并分析脱氧产品使用气相色谱与质量选择检测器。17
</li>
	<li>根据以下方程式确定木质素模型化合物的转化: <img alt="Equation 1" src="/files/ftp_upload/56987/56987eq1.jpg">
</li>
	<li>根据以下公式确定产品选择性: <img alt="Equation 2" src="/files/ftp_upload/56987/56987eq2.jpg">
</li>
</ol>

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Res. 18 (5), 1-12 (2016).</li><li>Wang, K., Yang, L., Zhao, W., Cao, L., Sun, Z., Zhang, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+facile+synthesis+of+copper+nanoparticles+supported+on+an+ordered+mesoporous+polymer+as+an+efficient+and+stable+catalyst+for+solvent-free+sonogashira+coupling+Reactions.">A facile synthesis of copper nanoparticles supported on an ordered mesoporous polymer as an efficient and stable catalyst for solvent-free sonogashira coupling Reactions.</a> Green Chem. 19, 1949-1957 (2017).</li><li>Song, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-Selectivity+Electrochemical+Conversion+of+CO2+to+Ethanol+using+a+Copper+Nanoparticle/N-Doped+Graphene+Electrode.">High-Selectivity Electrochemical Conversion of CO2 to Ethanol using a Copper Nanoparticle/N-Doped Graphene Electrode.</a> Chemistry Select. 1, 6055-6061 (2016).</li></ol>

我们没有什么可透露的。

制备镍掺杂块状铌氧化物纳米微粒的常用方法之一是旋转蒸发法。9通过在旋转蒸发过程中采用各种压力和温度条件, 将镍铌 O 颗粒的沉淀与溶剂的缓慢去除进行贸易。与旋转蒸发法相比, 本研究报告的化学沉淀法在制备纳米微粒时越来越受到重视, 因此不需要去除溶剂。在典型的化学沉淀法中制备催化剂, 在长期的金属盐溶液中加入碱性溶液是必要的。21在我们?...

纳米复合材料的制备因其在各个领域的重要应用而受到越来越多的关注。为制备镍铌 O 混合氧化物纳米粒子,1,2,3,4,5,6不同的方法已经开发, 如干混合法,7, 8蒸发方法、9、10、11、12、13溶胶凝胶法、14热分解法、15和自动燃烧。16在典型的蒸发方法9中, 含有适当数量的金属前体、硝酸镍六水合物和草酸铌铵的水溶液加热70摄氏度。在溶剂去除和进一步烘干和煅烧后, 得到了混合氧化物。这些氧化物催化剂对乙烷的氧化脱氢 (脱氢) 具有良好的催化活性和选择性, 这与在 NiO 晶格中加入铌阳离子引起的电子和结构重排有关。.11插入 Nb 会大幅减少亲氧的种类, 这是对乙烷12氧化反应的负责。因此, 这种方法的推广已经在制备不同类型的混合镍氧氧化物, 在那里我 = 李, 镁, 铝, Ga, Ti 和 Ta。13发现金属掺杂的变化可以改变 NiO 的 unselective 和亲氧自由基, 从而系统地调节脱氢的活性和对乙烷的选择性。然而, 通常这些氧化物的表面积相对较小 (< 100 米2/克), 这是由于扩展的相隔离和形成大 Nb2O5晶粒, 从而妨碍了它们在其他催化应用程序.
干混法, 又称固态磨削法, 是制备混合氧化物催化剂的另一种常用方法。由于催化材料是以无溶剂的方式获得的, 这种方法为混合氧化物的制备提供了一个有前景的绿色和可持续的替代方案。该方法获得的最高表面积为镍80铌20在煅烧温度为250摄氏度的172米2/克。8然而, 这种固态方法不可靠, 因为反应物在原子尺度上没有很好的混合。因此, 为了更好地控制化学均匀性和特定粒径分布和形貌, 目前仍在寻找其他合适的方法制备镍铌 O 混合氧化物纳米粒子。7
在纳米粒子发展的各种策略中, 化学沉淀是发展催化剂的一种有希望的方法, 因为它允许金属离子的完全沉淀。同时, 用该方法制备较高表面积的纳米粒子。为了提高镍铌纳米粒子的催化性能, 本文报道了化学沉淀法合成高表面积镍铌 o 型混合氧化物催化剂的协议。我们证明, 铌: 镍摩尔比是决定氧化物催化活性的关键因素, 对木质素衍生有机化合物的加氢脱氧。高铌: 镍比0.087 以上, 非活动 NiNb2O6种形成。Ni0.92铌0.08O 具有最大的表面积 (173 米2/克), 它具有折叠状的薄片结构, 并显示了对甲醚到环己烷加氢脱氧的最佳活动和选择性。

<table><tbody><tr><td>Niobium(V) oxalate hydrate, 98%</td><td>Alfa</td><td>L04481902</td><td></td></tr><tr><td>Nickel nitrate hexahydrate, 99%</td><td>Aladdin</td><td>N108891</td><td></td></tr><tr><td>Sodium hydroxide, 98%</td><td>Aladdin</td><td>S111501</td><td></td></tr><tr><td>Ammonium hydroxide, 23-25%</td><td>Aladdin</td><td>A112077</td><td></td></tr><tr><td>Anisole, 99%</td><td>Sinopharm</td><td>81001728</td><td></td></tr><tr><td>Diphenyl ether, 98%</td><td>Aladdin</td><td>D110644</td><td></td></tr><tr><td>Phenol, 98%</td><td>Sinopharm</td><td>100153008</td><td></td></tr><tr><td>2-Methoxyphenol, 98%</td><td>Sinopharm</td><td>30114526</td><td></td></tr><tr><td>Vanillin, 99.5%</td><td>Sinopharm</td><td>69024316</td><td></td></tr><tr><td>Potassium hydroxide, AR</td><td>Aladdin</td><td>P112284</td><td></td></tr><tr><td>N,N-Dimethylformamide, 99.5%</td><td>Sinopharm</td><td>40016462</td><td></td></tr><tr><td>2-Bromoacetophenone,98%</td><td>Aladdin</td><td>B103328</td><td></td></tr><tr><td>Diethyl ether,99.5%</td><td>Sinopharm</td><td>10009318</td><td></td></tr><tr><td>Decane,98%</td><td>Aladdin</td><td>D105231</td><td></td></tr><tr><td>Dodecane,99%</td><td>Aladdin</td><td>D119697</td><td></td></tr><tr><td>Niobic acid</td><td>CBMM</td><td>1313968</td><td></td></tr><tr><td>Heating and Drying Oven</td><td></td><td></td><td>DHG Series (shanghai jinghong laboratory instrument co. ltd)</td></tr><tr><td>Autoclave Reactor</td><td></td><td></td><td>CJF-0.05&amp;mdash;0.1L (Dalian Tongda Equipment Technology Development Co., Ltd)</td></tr><tr><td>Tube&amp;nbsp;furnace</td><td></td><td></td><td>SK2-1-10/12 (Luoyang Huaxulier Electric Stove Co., Ltd)</td></tr><tr><td>Heating magnetic stirrer</td><td></td><td></td><td>DF-101 (Yu Hua Instrument Co. Ltd.)</td></tr><tr><td>Rotary evaporator</td><td></td><td></td><td>RE-3000A (Shanghai Yarong Biochemical Instrument Factory)</td></tr><tr><td>Synthetic air</td><td></td><td></td><td></td></tr><tr><td>Hydrogen gas</td><td></td><td></td><td></td></tr><tr><td>Argon gas</td><td></td><td></td><td></td></tr></tbody></table>

chemical precipitation method for the synthesis of nb2o5 modified bulk nickel catalysts with high specific surface area

我们演示了一种用海绵状和褶皱状纳米结构合成镍x铌1-xO 催化剂的方法。通过改变 Nb: ni 比, 用化学沉淀法制备了一系列不同原子组成 (x = 0.03、0.08、0.15 和 0.20) 的镍x铌1 xO 纳米粒子。这些镍x铌1 xO 催化剂的特点是 x 射线衍射、x 射线光电子能谱和扫描电镜。研究发现镍的0.97铌0.03O 和 ni0.92Nb0.08o 在 NiO 表面上的海绵状和褶皱状外观, 以及这些 Nix铌1 xO 催化剂的较大表面积, 与散装nio.镍0.92铌0.08O 型催化剂可获得173米2/克的最大表面积。此外, 还研究了利用合成的 Ni0.92铌0.08O 催化剂对木质素衍生化合物的催化 hydroconversion。

x 射线衍射 (XRD) 模式 (图 1和图 2), 下注表面积, 用氢 (H2-TPR) 的温度编程还原氢, 扫描电子显微镜 (SEM) 配有能量色散 X 射线 (EDX) 分析仪、X 射线光电子能谱 (XPS) 是为纳米 NiO、镍铌 O 和 Nb2O5氧化物17 (图 3和图 4) 收集的。采用 XRD、SEM 和 XPS 等方...

Watch this Scientific Journal Video about Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area at JoVE.com

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

本文介绍了化学沉淀法合成海绵状和褶皱状镍1-x铌xO 纳米粒子的一种协议。

化学沉淀法合成铌2O5改性高比表面积镍催化剂

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

chemical-precipitation-method-for-synthesis-nb2o5-modified-bulk

Research

JoVE Journal

Chemistry

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

11.8K 次观看.  Dalian University of Technology. 本文介绍了化学沉淀法合成海绵状和褶皱状镍1-x铌xO 纳米粒子的一种协议。

视频: Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

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

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

单金属和双金属前过渡金属碳化物和氮化物纳米粒子的反相微乳液介导的合成

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

科研

化学

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

高炉矿渣的双向稳定物价:沉淀碳酸钙和沸石重金属吸附剂的合成

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

工程学

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), M&#246;ssbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

A facile preparation method of electrodes using the bulk material Fe4.5Ni4.5S8 is presented. This method provides an alternative technique to conventional electrode fabrication and describes prerequisites for unconventional electrode materials including a straightforward electrocatalytic testing method.

用于制备用于电催化应用的非贵金属体电极的简单方法

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

铂镍纳米线的合成及减氧性能优化

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

电化学 CO2还原的过渡金属单原子催化剂的合成及性能表征

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

A Continuous-flow Photocatalytic Reactor for the Precisely Controlled Deposition of Metallic Nanoparticles

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic nanoparticles is developed. Guidelines for the replication of the reactor and its operation are provided in detail. Three different composite systems (Pt/graphene, Pt/TiO2, and Au/TiO2) with monodisperse and uniformly distributed particles are produced by this reactor, and the photodeposition mechanism, as well as the synthesis optimization strategy, are discussed. The synthesis methods and their technical aspects are described comprehensively. The role of the ultraviolet (UV) dose (in each excitation pulse) on the photodeposition process is investigated and the optimum values for each composite system are provided.

For a continuous and scalable synthesis of noble-metal-based nanocomposites, a novel photocatalytic reactor is developed and its structure, operation principles, and product quality optimization strategies are described.

一种用于金属纳米粒子精确控制沉积的连续流动光催化反应器

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

调整二苯醚氢氧化的Pt/CNT催化剂的酸度

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...

Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular transformations. This opens possibilities for the use of visible or near-IR light as a sustainable input to drive and control reactions when plasmonic nanoparticles supporting LSPR excitation in these ranges are employed as catalysts. Unfortunately, this is not the case for several catalytic metals such as palladium (Pd). One strategy to overcome this limitation is to employ bimetallic NPs containing plasmonic and catalytic metals. In this case, the LSPR excitation in the plasmonic metal can contribute to accelerate and control transformations driven by the catalytic component. The method reported herein focuses on the synthesis of bimetallic silver-palladium (Ag-Pd) NPs supported on ZrO2 (Ag-Pd/ZrO2) that acts as a plasmonic-catalytic system. The NPs were prepared by co-impregnation of corresponding metal precursors on the ZrO2 support followed by simultaneous reduction leading to the formation of bimetallic NPs directly on the ZrO2 support. The Ag-Pd/ZrO2 NPs were then used as plasmonic catalysts for the reduction of nitrobenzene under 425 nm illumination by LED lamps. Using gas chromatography (GC), the conversion and selectivity of the reduction reaction under the dark and light irradiation conditions can be monitored, demonstrating the enhanced catalytic performance and control over selectivity under LSPR excitation after alloying non-plasmonic Pd with plasmonic metal Ag. This technique can be adapted to a wide range of molecular transformations and NPs compositions, making it useful for the characterization of the plasmonic catalytic activity of different types of catalysis in terms of conversion and selectivity.

Presented here is a protocol for the synthesis of silver-palladium (Ag-Pd) alloy nanoparticles (NPs) supported on ZrO2 (Ag-Pd/ZrO2). This system allows for harvesting energy from visible light irradiation to accelerate and control molecular transformations. This is illustrated by nitrobenzene reduction under light irradiation catalyzed by Ag-Pd/ZrO2 NPs.

在可见光照射下为质子催化准备银-铂合金纳米粒子

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular ...

Synthesis of Metal Nanoparticles Supported on Carbon Nanotube with Doped Co and N Atoms and its Catalytic Applications in Hydrogen Production

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented herein. The novel strategy is based on a facile one-pot pyrolysis treatment of cobalt (II) acetylacetonate and nitrogen-rich organic precursors under Ar atmosphere at 800 &#176;C, resulting in the formation of Co- and N- co-doped carbon nanotube with earthworm-like morphology. The obtained catalyst was found to have a high density of defect sites, as confirmed by Raman spectroscopy. Here, cobalt (II) nanoparticles were stabilized on the atomically dispersed cobalt- and nitrogen-doped carbon nanotubes. The catalyst was confirmed to be effective in the catalytic hydrolysis of ammonia borane, in which the turnover frequency was 5.87 mol H2&#183;molCo-1&#183;min-1, and the specific hydrogen generation rate was determined to be 2447 mL H2&#183;gCo-1&#183;min-1. A synergistic function between the Co nanoparticle and the doped carbon nanotubes was proposed for the first time in the catalytic hydrolysis of ammonia borane reaction under a mild condition. The resulting hydrogen production with its high energy density and minimal refueling time could be suitable for future development as energy sources for mobile and stationary applications such as road trucks and forklifts in transport and logistics.

Here, we present a protocol to synthesize Co nanoparticles supported on carbon nanotubes with Co- and N- dopants for hydrogen productions.

碳纳米管负载掺杂Co和N原子金属纳米粒子的合成及其在制氢中的催化应用

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented ...

氢氧化镍纳米片的微波合成与表征

Effect of Microwave Synthesis Conditions on the Structure of Nickel Hydroxide Nanosheets

A protocol for rapid, microwave-assisted hydrothermal synthesis of nickel hydroxide nanosheets under mildly acidic conditions is presented, and the effect of reaction temperature and time on the material&#39;s structure is examined. All reaction conditions studied result in aggregates of layered &#945;-Ni(OH)2 nanosheets. The reaction temperature and time strongly influence the structure of the material and product yield. Synthesizing &#945;-Ni(OH)2 at higher temperatures increases the reaction yield, lowers the interlayer spacing, increases crystalline domain size, shifts the frequencies of interlayer anion vibrational modes, and lowers the pore diameter. Longer reaction times increase reaction yields and result in similar crystalline domain sizes. Monitoring the reaction pressure in situ shows that higher pressures are obtained at higher reaction temperatures. This microwave-assisted synthesis route provides a rapid, high-throughput, scalable process that can be applied to the synthesis and production of a variety of transition metal hydroxides used for numerous energy storage, catalysis, sensor, and other applications.

作者聚焦:氢氧化镍纳米片的快速微波辅助水热合成 

Nickel hydroxide nanosheets are synthesized by a microwave-assisted hydrothermal reaction. This protocol demonstrates that the reaction temperature and time used for microwave synthesis affects the reaction yield, crystal structure, and local coordination environment.

微波合成条件对氢氧化镍纳米片结构的影响

A protocol for rapid, microwave-assisted hydrothermal synthesis of nickel hydroxide nanosheets under mildly acidic conditions is presented, and the effect ...

化学沉淀法合成铌₂O₅改性高比表面积镍催化剂

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