CN110117028A - 一种蓝色发光二硫化钛纳米晶的制备技术 - Google Patents
一种蓝色发光二硫化钛纳米晶的制备技术 Download PDFInfo
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Abstract
一种蓝色发光二硫化钛纳米晶的制备技术是利用物理和化学相结合的方法制备TiS2纳米晶。物理研磨的目的是引入线缺陷(位错)使得晶体存在张应力,能使带隙增大,尺寸更小更可控,利于纳米晶的形成。通过细胞破碎仪制备出的TiS2纳米晶显示出良好的分散性,并具有较强的荧光性。本发明提出的一种蓝色发光二硫化钛纳米晶的制备技术,其特征在于实验方法简便,可制备出分散性好、尺寸小且均匀的产物。通过透射电子显微镜表征可知TiS2纳米晶的晶格条纹间距为0.267nm,平均粒径为3.1nm。此外,该纳米晶在365nm紫外灯照射下发出蓝色荧光,有望在基因识别、生物成像、光电子成像及器件制备等领域得到应用。
Description
技术领域
本发明涉及一种蓝色发光二硫化钛纳米晶的制备技术,具体涉及改变二硫化钛的尺寸,调节二硫化钛的带隙达到蓝色发光的效果。
背景技术
近年来,二维过渡金属硫族化合物(2D-TMDs)由于其独特的物理和化学性质,已经成为当前研究的热点。二硫化钛(TiS2)具有和石墨烯类似的层状结构,层与层之间以弱的范德华力结合,因而被誉为“无机石墨烯”(Inorganic Graphene)。相比于石墨烯的零带隙性质,许多层状TiS2存在直接带隙,因此产生一系列新颖而独特的光学、电学、磁学、力学、化学等性质,已经成为材料研究领域的热点。
目前虽然有一些关于TiS2纳米材料制备、性质及应用的研究报道,但研究对象的尺寸主要集中在数百纳米级,针对尺寸仅为几纳米的TiS2材料的研究仍然很少。如果材料的尺寸减小到德布罗意波长时,存在小尺寸效应、表面效应、量子限域效应、介电效应等一系列介观效应的存在,材料往往会表现出完全异于其体材料的物理化学性质,其中以TiS2纳米晶最为典型。这一新型的纳米晶不仅保留了二维材料的结构特征,而且零维结构会带来更强的边缘效应和量子限域效应,能展现出比多层的TiS2纳米片更独特的光电性质。尽管如此,严格控制TiS2 纳米晶的厚度和横向尺寸,实现TiS2 纳米晶的可控制备仍然面临很多困难。
就传统的制备方法而言,采用分子束外延、化学气相沉积、磁控溅射等设备制备纳米晶存在成本昂贵、颗粒团聚严重、分散性差、粒径大、尺寸不均等问题,所以在不影响材料性能的情况下,寻找一种操作简便、成本低廉、便于实施的制备技术对拓展纳米材料在多领域的应用尤为重要。细胞破碎法与传统的制备方法相比具有明显的优势,可以解决如成本昂贵、工艺繁琐、产率较低等一系列技术难题,而且可实现工业化生产,为纳米晶的规模化应用开辟了一条新途径。
中国专利号为:201710638898.9,名称为:一种二硫化钛纳米片及其制备方法。其特征在于:以手风琴状碳化钛为原料,通过硫化氢气体高温处理以及后续的液相超声剥离,制备得到二维二硫化钛纳米片,厚度在1-50 nm之间,可以作为锂离子电池的负极材料。本发明的技术与上述不同,本发明是先研磨TiS2粉末,然后直接一步使用细胞破碎法制得尺寸可控、带隙可调、尺寸更小的TiS2纳米晶溶液,再经过离心得到上层的TiS2纳米晶,其粒径在1-5nm之间,本技术的可操作性强,是环境友好型的一种制备纳米晶的方法。
发明内容
本发明要解决的问题是TiS2的尺寸可控、带隙可调、可发蓝光,以及提高荧光量子产率的问题。
本发明所使用的制备技术既实现了TiS2纳米晶的小尺寸、高产率,又有望进行工业化的规模生产。
一种蓝色发光TiS2纳米晶的制备技术,按照以下步骤进行:
(1)称取0.5g TiS2固体粉末于玛瑙研钵中充分研磨1.5小时;
(2)向(1)中研磨好的粉末样品加入适量N-甲基吡咯烷酮(NMP)溶剂后混合,并将混合液置于细胞破碎仪中破碎4小时;
(3)将(2)中的悬浮液转移到离心机中进行离心,然后收集上层清液即为TiS2纳米晶溶液。
所述(2)中的N-甲基吡咯烷酮(NMP)溶剂的表面张力值为35-70mj/m2。
本发明的TiS2纳米晶的晶格间距为0.267nm。
本发明的制备工艺与传统制备技术相比具有以下创新点。
1.实验方法创新:
工艺简单:目前,用传统方法制备纳米材料纳米晶的过程较复杂,一般包括两步及以上,本发明采用用一步细胞破碎法制备出TiS2纳米晶,操作简便,成本低,且符合生态环境友好型的发展要求。
2.潜在性能突破:
(1)发光特性:本发明制备的TiS2纳米晶在紫外光照射下能发出蓝光,通过光致发光光谱分析其荧光量子产率能达到50%左右,可拓展它在生物成像、荧光标记、光催化等领域的应用;
(2)分散性好:本发明TiS2纳米晶的平均粒径为3nm,纳米晶平均尺寸分布窄且均匀可控;
(3)水溶特性:本发明制备的TiS2纳米晶具有良好的水溶特性,拓展了其在生物、环境等领域的应用。
本发明采用简便的工艺技术通过一步细胞破碎法制备出尺寸均匀、分散性好,且具有蓝色发光特性的TiS2 纳米晶。使TiS2的性能有所突破,在半导体精密光电器件、LED成像等领域具有良好的应用前景。
附图说明
图1是TiS2纳米晶分别在自然光(左图)和365nm紫外光照射下(右图)的图片。
图2是TiS2纳米晶X射线衍射图。
图3是TiS2纳米晶晶格条纹图。
图4是TiS2纳米晶水溶液紫外-可见光吸收光谱图。
具体实施例
实施例1:称取0.5克TiS2固体粉末置于玛瑙研钵中充分研磨1.5小时,将研磨好的粉末转移到烧杯中,向其中加入50ml N-甲基吡咯烷酮(NMP)溶剂后混合均匀,得到的混合液置于细胞破碎仪中破碎4小时。取适量溶液离心,离心后取上层清液即可得到TiS2纳米晶。
Claims (4)
1.一种蓝色发光二硫化钛纳米晶的制备技术,其特征在于该制备方法以TiS2粉末为原料进行研磨,然后向其中加入适量的N-甲基吡咯烷酮(NMP)溶剂,并用细胞破碎仪制备TiS2纳米晶,最后对溶液进行离心分离。
2.如权利要求1所述,一种蓝色发光二硫化钛纳米晶的制备技术,其TiS2粉末的质量为0.5g,NMP溶剂的体积为50ml。
3.如权利要求1所述,一种蓝色发光二硫化钛纳米晶的制备技术,所得TiS2纳米晶要求平均粒径小于5nm。
4.如权利要求1所述,一种蓝色发光二硫化钛纳米晶的制备技术,其步骤包括:
(1)取一定量TiS2固体粉末于玛瑙研钵中充分研磨1.5h;
(2)在研磨好的粉末中加入N-甲基吡咯烷酮(NMP)溶剂,然后将上述混合液置于细胞破碎仪中破碎4小时;
(3)将超声后的溶液转移到离心机中离心,收集上层清液即为TiS2纳米晶溶液。
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