CN106975754A - 一种钯纳米线的制备方法 - Google Patents
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000005684 electric field Effects 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 230000033001 locomotion Effects 0.000 claims abstract description 10
- 230000009471 action Effects 0.000 claims abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 13
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims description 3
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 2
- 230000001808 coupling effect Effects 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims 1
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000012696 Pd precursors Substances 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 lauryl dimethyl benzyl Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
本发明公开了一种钯纳米线的制备方法，首先通过制备钯前驱体溶液，并加入表面活性剂，在电场作用下使钯离子在玻璃基板模板上富集，并加入还原剂还原，得到纳米粒子，随后重新加入前驱体溶液，施加垂直方向的电场并加入还原剂，使钯离子定向运动并生长，作用下加入还原剂，得到高长径比且取向规则的钯纳米线。
Description
技术领域
本发明涉及一种钯纳米线的制备方法。
背景技术
金属于贵金属，由于表现出良好的选择催化活性和导电性，钯的纳米材料目前在催化转换器，燃料电池，石油裂化等很多工业技术领域中具有很好的应用前景。而近研究发现，钯纳米材料的某些良好的物理特性，与纳米材料的形状和尺寸具有密切的关系，有效控制钯纳米材料的形貌和尺寸有望显著改善钯纳米材料的物理化学特性，钯纳米材料的一维结构和零维结构相比，表现出较高的长径比、较少的晶格缺陷、更小的晶格间距以及很高的表面原子数等优点。此外由于结构上的各向异性，一维钯纳米线将会显著提高电子传输效率。由于金属于贵金属，价格昂贵，如何在同样的用量前提下保证最大程度发挥其特性是目前研究的热点，但目前所进行的研究当中，均在一定程度上存在着制备方法工艺复杂，合成的钯纳米线长径比不高的问题，妨碍了钯纳米线的应用。
发明内容
为解决上述技术问题，本发明提供了一种钯纳米线的制备方法，采用玻璃基板作为模板，电场驱动富集的方法，获得了大尺寸钯纳米线。
本发明完整的技术方案包括：
一种钯纳米线的制备方法，其特征在于，包括如下步骤：
(1)将PdCl2加入去离子水，制备0.05mol/L的PdCl2水溶液，加于反应容器内，反应容器一侧设有玻璃基板，随后加入表面活性剂，表面活性剂组成为月桂基二甲基苄基氯化铵：C15三甲基溴化铵＝1：1的混合物，以上为体积比，搅拌5min后静置3h，随后对反应容器两端施加200N/C的电场，在室温下使钯离子在电场作用下定向运动并富集到玻璃基板表面，在超声振动搅拌和电场耦合作用下加入6mmol/L的葡萄糖水溶液，其中PdCl2、表面活性剂和葡萄糖的摩尔比为1:4.5:60，静置3h制得富集在玻璃基板表面的钯纳米粒子。
(2)将浓度为0.2mol/L的PdCl2水溶液再次加入步骤(1)所得溶液，随后加入0.02mol/L的水合肼溶液，加热温度到45-50℃，再次对反应容器两端施加400N/C电场，此次施加电场的方向与步骤(1)施加电场的方向垂直，使钯离子在电场作用下定向运动并沿着与步骤(1)施加电场垂直的方向运动并还原剂作用下析出生长，得到尺寸为800-900纳米的钯纳米线。
步骤(1)所得到钯纳米粒子、步骤(2)所加PdCl2以及水合肼的摩尔比为1:50:30。
步骤(1)所用表面活性剂浓度为0.03mol/L。
本发明相对于现有技术的优点在于：通过采用玻璃基板作为模板，在电场作用下形成钯纳米粒子的富集，还原得到预制颗粒，随后采用垂直电场作用使离子重新富集并进行还原，使纳米线沿电场方向运动并生长，得到高长径比且取向规则的钯纳米线。
具体实施方式
下面结合具体实施方式对本发明做进一步说明。
(1)将PdCl2加入去离子水，制备0.05mol/LPdCl2水溶液，加于反应容器内，反应容器一侧设有玻璃基板，随后加入体积比为月桂基二甲基苄基氯化铵：C15三甲基溴化铵＝1：1的混合物作为表面活性剂，搅拌5min后静置3h，随后对反应容器两端施加200N/C的电场，在室温下使钯离子在电场作用下定向运动并富集到玻璃基板表面，在超声振动搅拌和电场耦合作用下加入6mmol/L的葡萄糖水溶液，其中PdCl2、表面活性剂和葡萄糖的摩尔比为1:4.5:60，静置3h制得富集在玻璃基板表面的钯纳米粒子。
(2)将浓度为0.2mol/L的PdCl2水溶液再次加入步骤(1)所得溶液，随后加入0.02mol/L的水合肼溶液，加热温度到45-50℃，再次对反应容器两端施加400N/C电场，此次施加电场的方向与步骤(1)施加电场的方向垂直，使钯离子在电场作用下定向运动并沿着与步骤(1)施加电场垂直的方向运动并还原剂作用下析出生长，得到尺寸为800-900纳米的钯纳米线，其中，步骤(1)所得到钯纳米粒子、步骤(2)所加PdCl2以及水合肼的摩尔比为1:50:30。
以上所述，仅是本发明的较佳实施例，并非对本发明作任何限制，凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效结构变化，均仍属于本发明技术方案的保护范围内。
Claims (3)
1.一种钯纳米线的制备方法，其特征在于，包括如下步骤：
(1)将PdCl2加入去离子水，制备0.05mol/L的PdCl2水溶液，加于反应容器内，反应容器一侧设有玻璃基板，随后加入表面活性剂，表面活性剂组成为月桂基二甲基苄基氯化铵：C15三甲基溴化铵＝1：1的混合物，以上为体积比，搅拌5min后静置3h，随后对反应容器两端施加200N/C的电场，在室温下使钯离子在电场作用下定向运动并富集到玻璃基板表面，在超声振动搅拌和电场耦合作用下加入6mmol/L的葡萄糖水溶液，其中PdCl2、表面活性剂和葡萄糖的摩尔比为1:4.5:60，静置3h制得富集在玻璃基板表面的钯纳米粒子。
(2)将浓度为0.2mol/L的PdCl2水溶液再次加入步骤(1)所得溶液，随后加入0.02mol/L的水合肼溶液，加热温度到45-50℃，再次对反应容器两端施加400N/C电场，此次施加电场的方向与步骤(1)施加电场的方向垂直，使钯离子在电场作用下定向运动并沿着与步骤(1)施加电场垂直的方向运动并还原剂作用下析出生长，得到尺寸为800-900纳米的钯纳米线。
2.权利要求1所述的方法，其特征在于，其中，步骤(1)所得到钯纳米粒子、步骤(2)所加PdCl2以及水合肼的摩尔比为1:50:30。
3.权利要求1所述的方法，其特征在于，步骤(1)所用表面活性剂浓度为0.03mol/L。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111069625A (zh) * | 2020-01-06 | 2020-04-28 | 昆明理工大学 | 一种片状铂纳米颗粒的制备方法 |
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| US3275787A (en) * | 1963-12-30 | 1966-09-27 | Gen Electric | Process and apparatus for producing particles by electron melting and ultrasonic agitation |
| CN1911782A (zh) * | 2006-07-21 | 2007-02-14 | 东莞理工学院 | 一种钯纳米线有序阵列材料的制备方法 |
| CN101310899A (zh) * | 2008-03-18 | 2008-11-26 | 江苏工业学院 | 大批量制备银纳米线的方法 |
| CN101935017A (zh) * | 2010-07-29 | 2011-01-05 | 中国科学院生态环境研究中心 | 用于贵重金属超细纳米线水相合成及其自沉降构建贵重金属纳孔膜的方法 |
| CN103252501A (zh) * | 2013-04-27 | 2013-08-21 | 宁波大学 | 一种尺寸可控的金属钯纳米线的制备方法 |
| CN104018189A (zh) * | 2014-06-05 | 2014-09-03 | 东北大学 | 一种新型纳米银线的制备方法 |
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- 2016-12-30 CN CN201611265514.5A patent/CN106975754B/zh active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3275787A (en) * | 1963-12-30 | 1966-09-27 | Gen Electric | Process and apparatus for producing particles by electron melting and ultrasonic agitation |
| CN1911782A (zh) * | 2006-07-21 | 2007-02-14 | 东莞理工学院 | 一种钯纳米线有序阵列材料的制备方法 |
| CN101310899A (zh) * | 2008-03-18 | 2008-11-26 | 江苏工业学院 | 大批量制备银纳米线的方法 |
| CN101935017A (zh) * | 2010-07-29 | 2011-01-05 | 中国科学院生态环境研究中心 | 用于贵重金属超细纳米线水相合成及其自沉降构建贵重金属纳孔膜的方法 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111069625A (zh) * | 2020-01-06 | 2020-04-28 | 昆明理工大学 | 一种片状铂纳米颗粒的制备方法 |
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