CN105328204B - 一种二维铜纳米棒的制备方法 - Google Patents
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- 229910052802 copper Inorganic materials 0.000 title claims abstract description 34
- 239000010949 copper Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000011268 mixed slurry Substances 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 11
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 7
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 4
- -1 neopelex Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000002925 chemical effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
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- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 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
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Abstract
本发明提供一种二维铜纳米棒的制备方法，该方法的步骤如下：将去离子水、十二烷基苯磺酸钠、聚乙烯吡咯烷酮混合均匀，得到溶液A；边搅拌边向溶液A加入硫酸铜水溶液，加完后继续搅拌2~5h，得到溶液B；向溶液B中加入氨三乙酸，得到混合浆料，将混合浆料转移到水热反应釜中，于160~200℃反应3~6h，得到产物；将产物离心后依次使用去离子水和无水乙醇洗涤，然后在温度为45~55℃下进行真空干燥，即得二维铜纳米棒。本发明提供的制备方法使用设备简单、工艺参数可控、可重复性极高；制备所需原料丰富，成本低，无废弃物产生；制备所得的二维铜纳米棒在固体润滑剂、催化剂、导电材料等方面有着广泛的应用。
Description
技术领域
本发明属于纳米材料技术领域，尤其涉及一种二维铜纳米棒的制备方法。
背景技术
纳米尺寸的超细粒子由于其独特的力学、光学、电学、磁学及化学效应，正越来越多的受到人们的关注。纳米尺寸的铜粉具有诸多优异的性能。纳米铜粉可以用作固体润滑剂，以适当的方式分散于润滑油中成为一种稳定的悬浮液，与固体表面相结合形成光滑的保护层，同时填塞划痕，从而降低摩擦和磨损。在化工领域使用甲醇脱氢制甲醛的催化过程中，纳米铜粉还可用作催化甲醇制得甲醛和氢气的催化剂。同时由于纳米铜粉具有低电阻特性，可用于制造导电浆料，广泛用于微电子工业中的封装等。
纳米颗粒的形貌会直接影响其物理和化学性能。纳米金属的形貌控制合成与应用属于材料研究领域的重要研究方向，利用表面活性剂参与化学合成，进行颗粒尺寸及形貌控制的纳米金属制备及应用研究具有深远的理论及应用价值。铜属于高对称性的面心立方的晶体结构，其二维纳米结构的制备非常困难。铜纳米棒的合成途径目前主要采用电化学沉积法，但是该方法过程复杂，反应条件苛刻，不适合大批量生产。虽然，目前有不少铜纳米材料制备的公开文献记载，但是关于大规模二维铜纳米棒的制备却极少。
发明内容
解决的技术问题：针对现有的电化学沉积方法产量小，反应条件苛刻等不足，本发明提供一种二维铜纳米棒的制备方法，该制备方法成本低、操作简单、可大规模形成二维铜纳米棒。
技术方案：一种二维铜纳米棒的制备方法，该方法的步骤如下：
第一步：将去离子水、十二烷基苯磺酸钠、聚乙烯吡咯烷酮混合均匀，得到溶液A，每升溶液中含十二烷基苯磺酸钠10~20g、含聚乙烯吡咯烷酮10~40g；
第二步：边搅拌边向溶液A加入硫酸铜水溶液，加完后继续搅拌2~5h，得到溶液B，其中硫酸铜与十二烷基苯磺酸钠的摩尔比为（0.1~0.5）:1；
第三步：向溶液B中加入氨三乙酸，得到混合浆料，将混合浆料转移到水热反应釜中，于160~200℃反应3~6h，得到产物，其中氨三乙酸与硫酸铜的质量比为（0.8~2.5）:1，
第四步：将产物离心后依次使用去离子水和无水乙醇洗涤，然后在温度为45~55℃下进行真空干燥，即得二维铜纳米棒。
优选的，第一步中每升溶液中含十二烷基苯磺酸钠15g、含聚乙烯吡咯烷酮20g。
优选的，第二步中继续搅拌时间为3h，硫酸铜与十二烷基苯磺酸钠的摩尔比为0.25:1。
优选的，第三步中将混合浆料转移到水热反应釜中，于180℃反应4h。
优选的，第三步中氨三乙酸与硫酸铜的质量比为2:1。
优选的，第四步中在温度为50℃下进行真空干燥。
有益效果：本发明提供的一种二维铜纳米棒的制备方法，该方法使用设备简单、工艺参数可控、可重复性极高；制备所需原料丰富，成本低，无废弃物产生；制备所得的二维铜纳米棒在固体润滑剂、催化剂、导电材料等方面有着广泛的应用。
附图说明
图1 是本发明的实施例1中制备得到的二维铜纳米棒的SEM图片，从图中可以看出，二维铜纳米棒呈长方体棒状，长度约2μm，宽度约500nm。
图2 是本发明的实施例1中制备得到的二维铜纳米棒的XRD图片，从图中可以看出，金属铜的X射线衍射图谱，不含杂质。
具体实施方式
实施例1
将1L去离子水与15g十二烷基苯磺酸钠和20g聚乙烯吡咯烷酮混合，得到溶液A，在搅拌条件下，向溶液A加入0.096 mol/L硫酸铜水溶液50ml，搅拌3h得到溶液B；向溶液B中加入1.2g氨三乙酸作为还原剂，将混合浆料转移到水热反应釜中于180℃反应4h；将产物离心，依次使用去离子水、无水乙醇洗涤、45℃真空干燥后即得二维铜纳米棒。
实施例2
将1L去离子水与20g十二烷基苯磺酸钠和30g聚乙烯吡咯烷酮混合，得到溶液A，在搅拌条件下，向溶液A加入0.16 mol/L 硫酸铜的水溶液 50ml，搅拌5h得到溶液B；向溶液B中加入2.5g氨三乙酸作为还原剂，将混合浆料转移到水热反应釜中于200℃反应6h；将产物离心，依次使用去离子水、无水乙醇洗涤、55℃真空干燥后即得二维铜纳米棒。
实施例3
将1L去离子水与10g十二烷基苯磺酸钠和10g聚乙烯吡咯烷酮混合，得到溶液A，在搅拌条件下，向溶液A加入0.064 mol/L硫酸铜的水溶液 50ml，搅拌4h得到溶液B；向溶液B中加入1.5g氨三乙酸作为还原剂，将混合浆料转移到水热反应釜中于160℃反应4h；将产物离心，依次使用去离子水、无水乙醇洗涤、50℃真空干燥后即得二维铜纳米棒。
实施例4
将1L去离子水与20g十二烷基苯磺酸钠和20g聚乙烯吡咯烷酮混合，得到溶液A，在搅拌条件下，向溶液A加入0.064 mol/L硫酸铜的水溶液 50ml，搅拌6h得到溶液B；向溶液B中加入3g氨三乙酸作为还原剂，将混合浆料转移到水热反应釜中于190℃反应3h；将产物离心，依次使用去离子水、无水乙醇洗涤、50℃真空干燥后即得二维铜纳米棒。
Claims (6)
1.一种二维铜纳米棒的制备方法，其特征在于该方法的步骤如下：
第一步：将去离子水、十二烷基苯磺酸钠、聚乙烯吡咯烷酮混合均匀，得到溶液A，每升溶液中含十二烷基苯磺酸钠10~20g、含聚乙烯吡咯烷酮10~40g；
第二步：边搅拌边向溶液A加入硫酸铜水溶液，加完后继续搅拌2~5h，得到溶液B，其中硫酸铜与十二烷基苯磺酸钠的摩尔比为（0.1~0.5）:1；
第三步：向溶液B中加入氨三乙酸，得到混合浆料，将混合浆料转移到水热反应釜中，于160~200℃反应3~6h，得到产物，其中氨三乙酸与硫酸铜的质量比为（0.8~2.5）:1，
第四步：将产物离心后依次使用去离子水和无水乙醇洗涤，然后在温度为45~55℃下进行真空干燥，即得二维铜纳米棒。
2.根据权利要求1所述的一种二维铜纳米棒的制备方法，其特征在于：所述第一步中每升溶液中含十二烷基苯磺酸钠15g、含聚乙烯吡咯烷酮20g。
3.根据权利要求1所述的一种二维铜纳米棒的制备方法，其特征在于：所述第二步中继续搅拌时间为3h，硫酸铜与十二烷基苯磺酸钠的摩尔比为0.25:1。
4.根据权利要求1所述的一种二维铜纳米棒的制备方法，其特征在于：所述第三步中将混合浆料转移到水热反应釜中，于180℃反应4h。
5.根据权利要求1所述的一种二维铜纳米棒的制备方法，其特征在于：所述第三步中氨三乙酸与硫酸铜的质量比为2:1。
6.根据权利要求1所述的一种二维铜纳米棒的制备方法，其特征在于：所述第四步中在温度为50℃下进行真空干燥。
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