CN107915249B - 方形核壳结构的纳米Cu2O/Cu3N材料的制备方法 - Google Patents
方形核壳结构的纳米Cu2O/Cu3N材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种具有方形核壳结构的纳米Cu2O/Cu3N材料的制备方法，该制备方法主要采用酸碱微刻蚀方法，以氯化铜为铜盐，以十二烷基苯磺酸钠为表面活性剂，氢氧化钠和盐酸羟胺为刻蚀剂，二者以不同比例加入；在40℃～90℃水浴下加热10min后，将前驱体离心分离。生成的Cu2O再进行氮化，再将Cu2O材料在200℃～250℃下氮化1‑4小时。可获取具有方形核壳结构的纳米Cu2O/Cu3N材料。本发明方法具有合成方法简便、反应温度低等优点。
Description
技术领域
本发明涉及一种方形核壳结构的纳米Cu2O/Cu3N的制备方法.
背景技术
Cu2O禁带宽度介于2.0-2.2eV之间，是一种具有可见光响应的p型氧化物半导体，在光催化领域具有良好的应用前景，逐渐成为国内外研究的热点。Cu2O晶体特殊的晶体结构和能带结构特点以及对其进行的掺杂和复合等改性研究，概述了Cu2O及其改性材料在光解水制氢及光降解有机污染物方面的研究进展，阐明提高Cu2O光催化效率的关键是抑制光生载流子的复合和Cu2O的光腐蚀，Cu2O的光催化反应还存在着许多问题。
吴志国及其团队用柱状靶多弧直流磁控溅射法合成了纳米Cu3N薄膜，其中Cu3N纳米微晶具有立方反ReO3结构。通过X射线光电子能谱对薄膜表面的成分分析表明，Cu3N薄膜表面铜元素同时以+1价和+2价存在。Cu3N 的Cu2p3，Cu2p2及N1s峰分别位于932.7，952.7和399.9eV。
此发明中，首次用氨气氮化法将Cu2O材料进行改性，合成了链接界面紧密的Cu2O/Cu3N异质结，合成方法简单，获得材料性能优良。
发明内容
本发明的目的就在于提供一种原料易得，工艺过程简单的制备方形核壳结构的纳米Cu2O/Cu3N材料的制备方法。
本发明的目的是通过下述方案达到的。
方形核壳结构的纳米Cu2O/Cu3N材料的制备方法，将铜盐溶于溶剂中，加入表面活性剂，随之加入刻蚀剂，搅拌后放入水浴加热，将产物离心分离；将生成的前驱体材料Cu2O进行氮化处理，可制备方形核壳结构的纳米 Cu2O/Cu3N材料。
1.铜盐与水的摩尔比为0.005M。
2.水浴的温度要控制在40℃～90℃。
3.氨气氮化处理温度控制在200℃-250℃。
本发明提供了一种制备方形结构的纳米Cu2O材料的方法，其特点是：
1.制备流程及设备简单。
2.所用氮源为工业氨气，相比氢气和氮气混合气体更为安全。
3.本发明的反应过程温度低，时间相对较短，容易控制。
4.本方法操作简便。
附图说明
图1为Cu2O/Cu3N的XRD图。
图2为Cu2O/Cu3N的SEM图。
图3为Cu2O/Cu3N的TEM图。
具体实施方式
为了进一步说明本发明，列举以下实施实例。
实施例1
控制铜盐与水的摩尔比为0.005M，将铜盐(CuCl2)加入到水溶液中搅拌均匀。随后加入0.03M的十二烷基苯磺酸钠，充分搅拌使之完全溶解。加入1M的NaOH溶液0.18ml，0.1M的盐酸羟胺溶液0.4ml。搅拌30s 后将烧杯转入水浴中60℃加热20min。离心并用水和乙醇溶液分别清洗。得到方形结构的纳米Cu2O材料，将Cu2O材料放入氮化炉中抽真空，通氨气，升温至230℃，氮化2小时，经XRD表征，可得到Cu2O/Cu3N材料(图 1)，经SEM,TEM表征，可以看出Cu2O/Cu3N材料具有方形结构,外层大部分为Cu3N(图2，3)。
实施例2
控制铜盐与水的摩尔比为0.005M，将铜盐(CuCl2)加入到水溶液中搅拌均匀。随后加入0.01M的十二烷基苯磺酸钠，充分搅拌使之完全溶解。加入1M的NaOH溶液0.1ml，0.1M的盐酸羟胺溶液0.2ml。搅拌30s后将烧杯转入水浴中40℃加热10min。离心并用水和乙醇溶液分别清洗。得到纳米Cu2O材料，将Cu2O材料放入氮化炉中抽真空，通氨气，升温至250℃，氮化1小时，经XRD表征，可得到Cu2O/Cu材料。
实施例3
控制铜盐与水的摩尔比为0.005M，将铜盐(CuCl2)加入到水溶液中搅拌均匀。随后加入0.01M的十二烷基苯磺酸钠，充分搅拌使之完全溶解。加入1M的NaOH溶液0.1ml，0.1M的盐酸羟胺溶液0.2ml。搅拌30s后将烧杯转入水浴中40℃加热30min。离心并用水和乙醇溶液分别清洗。得到纳米Cu2O材料，将Cu2O材料放入氮化炉中抽真空，通氨气，升温至250℃，氮化2小时，经XRD表征，可得到Cu2O/Cu材料。
实施例4
控制铜盐与水的摩尔比为0.005M，将铜盐(CuCl2)加入到水溶液中搅拌均匀。随后加入0.01M的十二烷基苯磺酸钠，充分搅拌使之完全溶解。加入1M的NaOH溶液0.1ml，0.1M的盐酸羟胺溶液0.2ml。搅拌30s后将烧杯转入水浴中40℃加热30min。离心并用水和乙醇溶液分别清洗。得到纳米Cu2O材料，将Cu2O材料放入氮化炉中抽真空，通氨气，升温至250℃，氮化1小时，经XRD表征，可得到Cu2O/Cu材料。
实施例5
控制铜盐与水的摩尔比为0.005M，将铜盐(CuCl2)加入到水溶液中搅拌均匀。随后加入0.02M的十二烷基苯磺酸钠，充分搅拌使之完全溶解。加入1M的NaOH溶液0.3ml，0.1M的盐酸羟胺溶液0.3ml。搅拌30s后将烧杯转入水浴中50℃加热10min。离心并用水和乙醇溶液分别清洗。得到方形结构的纳米Cu2O材料，将Cu2O材料放入氮化炉中抽真空，通氨气，升温至200℃，氮化4小时，经XRD表征，可得到Cu2O材料。
实施例6
控制铜盐与水的摩尔比为0.005M，将铜盐(CuCl2)加入到水溶液中搅拌均匀。随后加入0.02M的十二烷基苯磺酸钠，充分搅拌使之完全溶解。加入1M的NaOH溶液0.3ml，0.1M的盐酸羟胺溶液0.3ml。搅拌30s后将烧杯转入水浴中80℃加热1小时。离心并用水和乙醇溶液分别清洗。得到方形结构的纳米Cu2O材料，将Cu2O材料放入氮化炉中抽真空，通氨气，升温至200℃，氮化3小时，经XRD表征，可得到Cu2O材料。
综上所述，得到方形核壳结构Cu2O/Cu3N材料的合成关键点：
1)合成前驱体材料时，原材料投加顺序不能调换；
2)水浴加热温度影响产物反应时间，进而影响产物最终形貌；
氮化温度和时间的控制极为重要，会影响产物生成路径。过低氮化温度下产物为氧化亚铜，氮化温度适度为Cu2O/Cu3N混合材料，过高的氮化温度会产生Cu单质。
Claims (4)
1.方形核壳结构的纳米Cu2O/Cu3N材料的制备方法，其特征是：将铜盐溶于溶剂中，加入表面活性剂，随之加入刻蚀剂氢氧化钠和盐酸羟胺，搅拌后放入水浴加热，将产物离心分离；将生成的前驱体材料Cu2O进行氮化处理，可制备方形核壳结构的纳米Cu2O/Cu3N材料；
所述水浴的温度为60 ℃，时间为20分钟；产物离心分离得到方形结构的纳米Cu2O材料；
所述的氮化处理氮源为氨气；
将纳米Cu2O材料在氨气中进行氮化处理，所述的氮化温度为230 ℃,氮化时间为2小时。
2.按照权利要求1所述的制备方法，其特征是：所述的铜盐为CuCl2；所述的溶剂为水；控制铜盐溶液浓度为0.005mol/L。
3.按照权利要求1所述的制备方法，其特征是：所述的表面活性剂为十二烷基苯磺酸钠，其用量与铜盐摩尔量比值为(10-30):5。
4.按照权利要求1所述的制备方法，其特征是：所述的刻蚀剂中氢氧化钠的浓度为1mol/L，盐酸羟胺的浓度为0.1 mol/L，它们用量分别为0.1 - 0.3 ml和0.2 - 0.4 ml。
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| CN101559970A (zh) * | 2009-05-26 | 2009-10-21 | 上海大学 | 电子束辐照和压缩空气氧化两步法制备纳米氧化亚铜 |
| CN102275975A (zh) * | 2011-06-01 | 2011-12-14 | 重庆工商大学 | 利用氮掺杂氧化亚铜制备纳米氧化亚铜的合成方法 |
| CN105129835A (zh) * | 2015-08-06 | 2015-12-09 | 上海应用技术学院 | 一种二十六面体氧化亚铜纳米粒子的制备方法 |
| CN105152199A (zh) * | 2015-08-06 | 2015-12-16 | 上海应用技术学院 | 一种十四面体氧化亚铜纳米粒子的制备方法 |
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| CN101559970A (zh) * | 2009-05-26 | 2009-10-21 | 上海大学 | 电子束辐照和压缩空气氧化两步法制备纳米氧化亚铜 |
| CN102275975A (zh) * | 2011-06-01 | 2011-12-14 | 重庆工商大学 | 利用氮掺杂氧化亚铜制备纳米氧化亚铜的合成方法 |
| CN105129835A (zh) * | 2015-08-06 | 2015-12-09 | 上海应用技术学院 | 一种二十六面体氧化亚铜纳米粒子的制备方法 |
| CN105152199A (zh) * | 2015-08-06 | 2015-12-16 | 上海应用技术学院 | 一种十四面体氧化亚铜纳米粒子的制备方法 |
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| "纳米Cu3N 薄膜的制备与性能";吴志国等;《物理学报》;20050430;第54卷(第4期);第1262页EXPERIMENTAL SECTION部分 * |
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