CN106495219B - 激光诱导制备KNb3O8纳米线的方法 - Google Patents
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- 239000002070 nanowire Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000002086 nanomaterial Substances 0.000 claims abstract description 15
- 229910052737 gold Inorganic materials 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004065 semiconductor Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 14
- 239000010931 gold Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000005424 photoluminescence Methods 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 230000006698 induction Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 238000011056 performance test Methods 0.000 abstract 1
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 abstract 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 8
- 239000010936 titanium Substances 0.000 description 6
- 239000012670 alkaline solution Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
激光诱导制备KNb3O8纳米线的方法属于新型功能材料技术领域。本发明使用405nm的半导体激光器，实验前在石英玻璃上镀Ti和Au，作为铌酸钾纳米线生长的衬底。向氢氧化钾溶液中加入Nb2O5粉末，使K：Nb的比例为50:1，并用磁力搅拌器搅拌15min，使Nb2O5充分溶解；激光照射时间分别为4‑12min。通过XRD、SEM等技术手段对微结构表征，表明产物为最强衍射峰在(110)晶面上的KNb3O8一维纳米线。通过紫外‑可见吸收和光致发光性能的测试，表明KNb3O8的带隙为2.98eV，具有潜在的蓝光发光特性。本发明通过激光照射时间的控制，生成长度，粗细不同的一维纳米结构，首次利用激光生成一维线状的KNb3O8纳米结构。
Description
技术领域
激光诱导生成纳米线的方法，属于新型功能材料的制备技术领域。
背景技术
激光诱导在衬底上制备纳米线的方法，是新颖的制备一维纳米结构的方法，其产物的形貌取决于激光照射的时间、激光功率、衬底表面催化剂的厚度和反应物浓度等多个因素的控制。与一些传统制备手段相比，具有许多优点，如样品制备时间较短、所制备出的纳米线结构长径比较大、形貌丰富多样等。
目前对KNb3O8纳米结构材料的制备主要有固相烧结法、熔盐法、高压水热法。但是用激光诱导方法制备KNb3O8纳米结构的研究和报道几乎还是空白。
本发明在适当的反应物配比及激光功率条件下，通过反应时间的控制，激光水热技术生成了KNb3O8一维纳米结构；获得的纳米线长度可达70μm，长径比可达50；并对其进行紫外-可见光谱测试和光致发光(PL)测试发现其可以有效的吸收400～475nm波长范围内的光谱。该方法的开拓有利于更简单的制备目标产物及性能研究，推动了新材料制备技术的实质性发展。
发明内容
本发明提供了一种在适当的反应物配比及激光功率条件下，通过反应时间的控制，激光水热技术生成KNb3O8一维纳米结构的方法。
本发明所采用的激光诱导方法，包括以下工艺步骤：
1)将KOH晶体溶解到水中，配置浓度为25mol/L的氢氧化钾溶液；
2)称取的五氧化二铌粉体(Nb2O5)；将称取好的五氧化二铌粉末，加入到已经配好的氢氧化钾溶液中，使K：Nb的摩尔比例为50:1，用磁力搅拌器充分搅拌，使溶液混合均匀；
3)将石英玻璃用酒精超声清洗，再用去离子水洗涤若干次；
4)使用直流溅射方法，在石英衬底上先镀一层厚度为15nm～25nm的Ti；再使用喷金仪镀一层厚度为130nm～140nm的Au，作为KNb3O8纳米线生长的衬底；
5)将制备好的衬底放入一个耐碱容器底部，有金膜的一面朝上。将制备好的溶液倒入小容器中，没过衬底；
6)使用波长为405nm的半导体激光，激光电流为50mA，功率为1.2W，分别照射 4-12min。
7)照射完毕，从溶液中用镊子取出衬底，用去离子水冲洗几次，从衬底的上表面得到KNb3O8一维纳米结构。
本发明的有益效果在于:
本发明利用简单的设备和巧妙的工艺控制，实现了激光水热法制备的KNb3O8一维纳米结构，获得了高长径比、形貌丰富的KNb3O8纳米线。
附图说明
图1a激光照射4min获得的KNb3O8扫描电镜图之一
图1b激光照射4min获得的KNb3O8扫描电镜图之二
图2激光照射6min获得的KNb3O8扫描电镜图
图3激光照射8min获得的KNb3O8扫描电镜图
图4激光照射10min获得的KNb3O8扫描电镜图
图5激光照射12min获得的KNb3O8扫描电镜图
图6激光照射10min获得的KNb3O8纳米线的XRD图
图7激光照射10min获得的KNb3O8紫外-可见光谱图
图8激光照射获得的KNb3O8光致发光(PL)光谱图
具体实施方式
下面通过实施例进一步阐明本发明的实质性特点，但本发明决不仅局限于以下实施例。实施例中所涉及的主要参数的设置如下表所示：
根据激光吸收率公式：ρ为电阻率；λ为激光波长。
钛的电阻率为0.556μΩ·m；金的电阻率为2.4μΩ·m。激光波长为405nm，因此Au的吸收率远远大于Ti的吸收率。
Ti的热膨胀系数为9.41～10.03×10-6/℃；Au的热膨胀系数为14.2×10-6/℃激光照射时，金吸收的热量多，热膨胀系数大，实验时如果不镀Ti作为缓冲层，Au容易脱落。因此选择在石英玻璃衬底上镀Ti膜和Au膜。
实验过程中由于实验仪器的限制，激光电流不能超过60mA，而电流在46mA和55mA时，并没有线状物质生成。而且激光照射时间大于15min时，由于激光能量过大，金膜脱落。照射时间小于4min时，衬底表面没有物质生成。因此实验室采用激光电流55mA，在 4～12min时间内照射。
产物的粉末X射线衍射(XRD)图谱采用的仪器为Bruker D-8 Advance粉末衍射仪(Cu Kα辐射，)；扫描电镜所用仪器为Hitachi S-3500型扫描电子显微镜；紫外-可见光谱仪型号为UV-3101PC；利用FLS980荧光光谱仪测试光致发光性能。
实施例1
称取2.0g(7.5mmol)的五氧化二铌粉体，然后将43.6682 g的KOH晶体溶解到30 mL的水中，配制成25mol/L浓度的氢氧化钾溶液，利用磁力搅拌器使其充分溶解；将称取研磨好的五氧化二铌粉末，加入到已经配好的25mol/L的氢氧化钾碱性溶液中，使用磁力搅拌器充分搅拌，使其充分混合；加入已放入衬底的容器中，用激光照射4 min。实验结束后将衬底从溶液里取出，用去离子水冲洗几次，得到KNb3O8一维纳米结构。
实施例2
称取2.0g(7.5mmol)的五氧化二铌粉体，然后将43.6682 g的KOH晶体溶解到30 mL的水中，配制成25mol/L浓度的氢氧化钾溶液，利用磁力搅拌器使其充分溶解；将称取研磨好的五氧化二铌粉末，加入到已经配好的25mol/L的氢氧化钾碱性溶液中，使用磁力搅拌器充分搅拌，使其充分混合；加入已放入衬底的容器中，用激光照射6 min。实验结束后将衬底从溶液里取出，用去离子水冲洗几次，得到KNb3O8一维纳米结构。实例2与实例1对比，纳米线成针尖状，长度比较长。由于纳米线数量增多，发光强度略高于照射4min 时。
实施例3
称取2.0g(7.5mmol)的五氧化二铌粉体，然后将43.6682g的KOH晶体溶解到30mL的水中，配制成25mol/L浓度的氢氧化钾溶液，利用磁力搅拌器使其充分溶解；将称取研磨好的五氧化二铌粉末，加入到已经配好的25mol/L的氢氧化钾碱性溶液中，使用磁力搅拌器充分搅拌，使其充分混合；加入已放入衬底的容器中，用激光照射8min。实验结束后将衬底从溶液里捞取出，用去离子水冲洗几次，得到KNb3O8一维纳米结构。与实例2对比，纳米线比较分散，并未从团簇中长出，长度更长。纳米线数量更多，发光强度最大。
实施例4
称取2.0g(7.5mmol)的五氧化二铌粉体，然后将43.6682g的KOH晶体溶解到30mL的水中，配制成25mol/L浓度的氢氧化钾溶液，利用磁力搅拌器使其充分溶解；将称取研磨好的五氧化二铌粉末，加入到已经配好的25mol/L的氢氧化钾碱性溶液中，使用磁力搅拌器充分搅拌，使其充分混合；加入已放入衬底的容器中，用激光照射10min。实验结束后将衬底从溶液里取出，用去离子水冲洗几次，得到KNb3O8一维纳米结构。得到纳米线长度达到70μm，从团簇中长出。纳米线长度最长，但由于数量有限，发光强度并不是最高。
实施例5
称取2.0g(7.5mmol)的五氧化二铌粉体，然后将43.6682g的KOH晶体溶解到30mL的水中，配制成25mol/L浓度的氢氧化钾溶液，利用磁力搅拌器使其充分溶解；将称取研磨好的五氧化二铌粉末，加入到已经配好的25mol/L的氢氧化钾碱性溶液中，使用磁力搅拌器充分搅拌，使其充分混合；加入已放入衬底的容器中，用激光分别照射12min。实验结束后将衬底从溶液里取出，用去离子水冲洗几次，得到KNb3O8一维纳米结构。由于温度梯度变小，实施例5中的纳米线长度变短，发光强度较弱。
Claims (1)
1.激光诱导制备KNb3O8纳米线的方法，其特征在于，包括以下工艺步骤：
1)将KOH溶解到去离子水中，配置浓度为25mol/L的氢氧化钾溶液；
2)称取五氧化二铌粉体；将称取好的五氧化二铌粉末，加入到已经配好的氢氧化钾溶液中，使K：Nb的摩尔比例为50:1，用磁力搅拌器充分搅拌，使溶液混合均匀；
3)将石英玻璃，用酒精超声清洗，再用去离子水洗涤若干次；
4)使用直流溅射方法，在清洗干净的石英玻璃上先镀一层厚度为15～20nm的Ti；再使用喷金仪镀一层厚度为130～140nm的Au，作为KNb3O8纳米线生长的衬底；
5)将制备好的衬底平放入一个耐碱容器底部，有金膜的一面朝上；将制备好的溶液倒入小容器中，没过衬底；
6)使用波长为405nm的半导体激光，激光电流为50mA，功率为1.2W，照射4-12min；
7)照射完毕，从溶液中用镊子取出衬底，用去离子水冲洗几次，在衬底的上表面得到KNb3O8一维纳米结构。
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| CN101857272A (zh) * | 2010-06-22 | 2010-10-13 | 浙江大学 | 一种微纳针状结构KNbO3的制备方法 |
| CN102502833B (zh) * | 2011-10-27 | 2014-06-18 | 浙江大学 | 一种微纳结构K3Nb7O19六棱片的制备方法 |
| CN105502498A (zh) * | 2015-12-20 | 2016-04-20 | 北京工业大学 | 一种水热制备金字塔形KNbO3纳米结构的方法 |
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