CN102502825A - A kind of bayberry shape V2O5 nanometer material and preparation method thereof - Google Patents
A kind of bayberry shape V2O5 nanometer material and preparation method thereof Download PDFInfo
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Abstract
Description
技术领域 technical field
本发明涉及半导体材料、光电子材料与器件技术领域，具体地涉及一种杨梅状V2O5纳米材料及其制备方法。 The invention relates to the technical field of semiconductor materials, optoelectronic materials and devices, in particular to a bayberry-shaped V 2 O 5 nanometer material and a preparation method thereof.
背景技术 Background technique
V2O5是黄色晶体，熔点为670℃，沸点为1690℃，具有斜方晶系结构，晶格常数a＝1.1519nm，b＝0.3564nm，c＝0.4373nm。每个钒原子被周围6个氧原子包围，形成八面体结构。V2O5晶体具有层状结构，显示出有趣的电子、离子、电化学性，在这种结构中，钒所处的环境是一个畸变四方棱锥体，钒原子与五个氧原子形成五个钒－氧键。使VO4四面体单元通过氧桥结合为链状。两条这样的链彼此以第五个氧原子通过另一氧桥连接成一条复链，从而构成起皱的层状排列。若从另一层中引入第六个氧原子、距离为280pm，使各层连接起来，这样最终便构成了一个V2O5晶体。V2O5的均匀范围很窄，为VO2.45-VO2.50。V2O5在685℃时熔融，在熔融的V2O5表面上的气相由V4O10,V6O14,V6O12和V4O8等组成。V2O5晶体的转换温度在257℃。当V2O5晶体处于半导体相时，禁带宽度为2.24 ev，且具有负的电阻温度系数。此外，V2O5光电导性质，这些性质使得V2O5可作普通离子吸收基质材料、湿敏传感器、微电池、电致变色显示材料，智能窗、滤色片、热辐射检测材料或光学记忆材料等。 V 2 O 5 is a yellow crystal with a melting point of 670°C and a boiling point of 1690°C. It has an orthorhombic structure with lattice constants a=1.1519nm, b=0.3564nm, and c=0.4373nm. Each vanadium atom is surrounded by six oxygen atoms, forming an octahedral structure. V 2 O 5 crystals have a layered structure, showing interesting electronic, ionic, and electrochemical properties. In this structure, the environment of vanadium is a distorted square pyramid, and vanadium atoms form five oxygen atoms. Vanadium-oxygen bond. The VO 4 tetrahedral units are combined into chains through oxygen bridges. Two such chains are connected to each other by a fifth oxygen atom through another oxygen bridge to form a complex chain, thus forming a wrinkled layered arrangement. If the sixth oxygen atom is introduced from another layer with a distance of 280pm, the layers are connected, and finally a V 2 O 5 crystal is formed. The uniform range of V 2 O 5 is very narrow, VO 2.45 -VO 2.50 . V 2 O 5 melts at 685°C, and the gas phase on the surface of the molten V 2 O 5 consists of V 4 O 10 , V 6 O 14 , V 6 O 12 and V 4 O 8 . The transition temperature of V 2 O 5 crystal is 257°C. When the V 2 O 5 crystal is in the semiconductor phase, the band gap is 2.24 ev, and it has a negative temperature coefficient of resistance. In addition, V 2 O 5 photoconductive properties, these properties make V 2 O 5 can be used as common ion absorption matrix materials, humidity sensors, micro batteries, electrochromic display materials, smart windows, color filters, thermal radiation detection materials or Optical memory materials, etc.
近来，人们利用各种方法（溶液法、分子束外延、溅射法、脉冲激光沉积、金属有机物化学气相沉积等）制备出了各种不同的V2O5纳米结构，例如纳米线、纳米带、纳米棒等，并对这些纳米结构的光电特性进行了研究，但是能应用于大规模生产的方法很少，且反应条件苛刻，生产成本高昂。 Recently, various methods (solution method, molecular beam epitaxy, sputtering method, pulsed laser deposition, metal-organic chemical vapor deposition, etc.) have been used to prepare various V 2 O 5 nanostructures, such as nanowires, nanoribbons , nanorods, etc., and the photoelectric properties of these nanostructures have been studied, but there are few methods that can be applied to large-scale production, and the reaction conditions are harsh and the production cost is high.
本发明克服现有技术制备方法中所存在的反应条件苛刻、生产成本高昂等缺陷，提供了一种一维纳米线组成的杨梅状V2O5纳米材料及其制备方法，本发明制备方法操作简便，成本低，可重复性高，可用于大规模的工业生产。本发明所制备出的V2O5纳米材料杂质少，其本身具有层状结构及相变性能，其构成纳米杨梅状的V2O5的纳米线具有很大的纵横比，有大量可作为发射点的纳米尖端，有很好的场发射特性，在纳米光电子领域有广阔的应用前景。 The present invention overcomes the defects of harsh reaction conditions and high production costs in the preparation methods of the prior art, and provides a bayberry-shaped V2O5 nanomaterial composed of one-dimensional nanowires and a preparation method thereof. The preparation method of the present invention operates It is simple, low in cost and high in repeatability, and can be used in large-scale industrial production. The V 2 O 5 nano material prepared by the present invention has few impurities, and it has a layered structure and phase transition performance. The nano wires of the V 2 O 5 that constitute the nano bayberry shape have a large aspect ratio, and there are a large number of them that can be used as The nano-tip of the emission point has good field emission characteristics and has broad application prospects in the field of nano-optoelectronics.
发明内容 Contents of the invention
本发明提出了一种杨梅状V2O5纳米材料，包括自中心衍生生长出的一维V2O5纳米线，所述杨梅状V2O5纳米材料为斜方晶系结构，晶格常数为a = 11.516 Å, b = 3.566 Å, c = 4.373Å。 The present invention proposes a bayberry-like V 2 O 5 nanomaterial, which includes a one-dimensional V 2 O 5 nanowire grown from the center . The constants are a = 11.516 Å, b = 3.566 Å, c = 4.373 Å.
其中，所述，所述一维V2O5纳米线长度范围为10−20 微米，直径为30−50 纳米。 Wherein, said one-dimensional V 2 O 5 nanowires have a length ranging from 10−20 micrometers and a diameter of 30−50 nanometers.
本发明还提出了一种所述的杨梅状V2O5纳米材料的制备方法，包括以下步骤： The present invention also proposes a method for preparing the bayberry-shaped V 2 O 5 nanometer material, comprising the following steps:
a、将偏钒酸铵溶于去离子水后，加入H2O2，调节pH值至2，加入聚乙烯吡咯烷酮； a. After dissolving ammonium metavanadate in deionized water, add H 2 O 2 , adjust the pH value to 2, and add polyvinylpyrrolidone;
b、在密封高压环境中，于180℃温度下反应24小时，经过滤、清洗得到黄色粉末状材料； b. In a sealed high-pressure environment, react at a temperature of 180°C for 24 hours, filter and wash to obtain a yellow powdery material;
c、将所述黄色粉末状材料于60℃-80℃温度下烘干，得到所述的杨梅状V2O5纳米材料。 c. drying the yellow powdery material at a temperature of 60° C. to 80° C. to obtain the bayberry-like V 2 O 5 nanometer material.
其中，所述步骤a中，所述偏钒酸铵与H2O2的摩尔质量比V:H2O2为1:10。 Wherein, in the step a, the molar mass ratio V:H 2 O 2 of the ammonium metavanadate to H 2 O 2 is 1:10.
其中，所述步骤a中，所述H2O2的质量浓度为30%，所述聚乙烯吡咯烷酮的浓度范围为0.05-0.1mol/L。 Wherein, in the step a, the mass concentration of the H 2 O 2 is 30%, and the concentration range of the polyvinylpyrrolidone is 0.05-0.1 mol/L.
其中，所述步骤a中，通过滴加硝酸调节pH值。 Wherein, in the step a, the pH value is adjusted by dropping nitric acid.
其中，所述步骤b中，使用无水乙醇和去离子水进行清洗。 Wherein, in the step b, absolute ethanol and deionized water are used for cleaning.
本发明的目的之一在于提供一种由一维纳米线呈发射状地组成的杨梅状V2O5纳米材料，杨梅状V2O5纳米材料是由一维纳米线相互间结合生长而构成，其一维纳米线的长度范围为10−20 微米，直径为30−50 纳米。杨梅状V2O5的结构为斜方晶系结构，其晶格常数为a = 11.516 Å, b = 3.566 Å, c = 4.373Å。 One of the objectives of the present invention is to provide a bayberry-shaped V 2 O 5 nanomaterial composed of one-dimensional nanowires in a radial form, and the bayberry-shaped V 2 O 5 nanomaterial is formed by combining and growing one-dimensional nanowires , whose one-dimensional nanowires have a length ranging from 10−20 μm and a diameter of 30−50 nm. The structure of bayberry-like V 2 O 5 is orthorhombic, and its lattice constants are a = 11.516 Å, b = 3.566 Å, c = 4.373 Å.
现有技术中合成的V2O5纳米结构多为纳米线、纳米带、纳米棒，之类，目前尚未有报道由一维纳米线组成的杨梅状V2O5纳米材料。本发明首次提供一种形貌新颖的、由一维纳米线组成的杨梅状V2O5纳米材料，且生成的V2O5晶体具有特殊的纳米结构，具有很好的场发射特性。 Most of the V 2 O 5 nanostructures synthesized in the prior art are nanowires, nanoribbons, nanorods, etc., and no bayberry-like V 2 O 5 nanomaterials composed of one-dimensional nanowires have been reported yet. The invention firstly provides a bayberry-shaped V 2 O 5 nano material composed of one-dimensional nano wires with novel appearance, and the generated V 2 O 5 crystal has a special nano structure and good field emission characteristics.
本发明的另一目的是提供一种由无数一维纳米线连接在一起形成的杨梅状V2O5纳米材料的制备方法，将偏钒酸铵溶于去离子水中，再加入30% H2O2，适当地加入聚乙烯吡咯烷酮做为表面活化剂，搅拌形成均匀的混合溶液，置于密封的高压釜中反应得到黄色粉末，再将黄色粉末经过在鼓风干燥箱中60℃温度下保持12小时烘干，制得由一维纳米线组成的杨梅状V2O5纳米材料。其中，反应是在密封的高压釜中进行。 Another object of the present invention is to provide a preparation method of bayberry-shaped V 2 O 5 nanomaterials formed by connecting together numerous one-dimensional nanowires, dissolving ammonium metavanadate in deionized water, and then adding 30% H 2 O 2 , appropriately add polyvinylpyrrolidone as a surfactant, stir to form a uniform mixed solution, place it in a sealed autoclave to react to obtain a yellow powder, and then pass the yellow powder through a blast drying oven at a temperature of 60°C Keep drying for 12 hours to prepare a bayberry-shaped V 2 O 5 nanomaterial composed of one-dimensional nanowires. Wherein, the reaction is carried out in a sealed autoclave.
本发明首次提出由一维纳米线组成的杨梅状的V2O5纳米材料制备方法，以偏钒酸铵溶液和30% H2O2为反应溶液，聚乙烯吡咯烷酮(PVP)为表面活化剂。本发明的反应过程中不需要催化剂，节省资源；设备要求简单，普通实验室设备都能达到；反应过程非常简单，不需要复杂的操作；本发明制备的V2O5纳米材料杂质少，制备方法成本低，重复性好，适用于大批量制备。 The present invention proposes for the first time the preparation method of bayberry-like V 2 O 5 nanomaterials composed of one-dimensional nanowires, using ammonium metavanadate solution and 30% H 2 O 2 as the reaction solution, and polyvinylpyrrolidone (PVP) as the surfactant . No catalyst is needed in the reaction process of the present invention, which saves resources; the equipment requirements are simple, and common laboratory equipment can meet; the reaction process is very simple and does not require complicated operations; The method has low cost and good repeatability, and is suitable for mass preparation.
本发明的制备方法解决了现有V2O5纳米材料制备方法条件苛刻，成本高的问题，从而提供一种低成本，高重复性，适用于大规模工业生产的新方法。本发明制备的V2O5纳米材料因为其本身具有层状结构，还具有相变性能，可以被用来制备智能温控型器件，智能温控玻璃涂层及锂离子电极材料。由于生成的V2O5晶体具有特殊的纳米结构，组成纳米杨梅状的V2O5的纳米线具有很大的纵横比，有大量可作为发射点的纳米尖端，可作为良好的场发射阴极材料，有很好的场发射特性，在纳米光电子领域有广阔的应用前景。可结合目前成熟的半导体硅集成电路工艺，适合于集成纳米光电子器件的发展。 The preparation method of the invention solves the problems of harsh conditions and high cost in the existing V2O5 nano material preparation method, thereby providing a new method with low cost, high repeatability and suitable for large-scale industrial production. The V 2 O 5 nanometer material prepared by the present invention has a layered structure and phase transition performance, and can be used to prepare intelligent temperature-controlled devices, intelligent temperature-controlled glass coatings and lithium ion electrode materials. Due to the special nanostructure of the generated V 2 O 5 crystals, the nanowires that make up the nano-red bayberry-like V 2 O 5 have a large aspect ratio and a large number of nano-tips that can be used as emission points, which can be used as a good field emission cathode Materials have good field emission characteristics and have broad application prospects in the field of nano-optoelectronics. It can be combined with the current mature semiconductor silicon integrated circuit technology, and is suitable for the development of integrated nano-optoelectronic devices.
附图说明 Description of drawings
图1是本发明杨梅状V2O5纳米材料的X射线衍射图。 Fig. 1 is an X-ray diffraction diagram of the bayberry-like V 2 O 5 nanomaterial of the present invention.
图2是本发明杨梅状V2O5纳米材料的SEM图。 Fig. 2 is a SEM image of the bayberry-shaped V 2 O 5 nanomaterial of the present invention.
图3是本发明杨梅状V2O5纳米材料的中倍SEM图。 Fig. 3 is a medium-magnification SEM image of the bayberry-like V 2 O 5 nanomaterial of the present invention.
图4 是本发明杨梅状V2O5纳米材料的高倍TEM图。 Fig. 4 is a high magnification TEM image of the bayberry-like V 2 O 5 nanomaterial of the present invention.
图5 是本发明杨梅状V2O5纳米材料的场发射性能测试的电流-电压（J-E）曲线图，插图为其对应的F-N曲线。 Fig. 5 is the current-voltage (JE) curve of the field emission performance test of the bayberry-shaped V 2 O 5 nanomaterial of the present invention, and the inset is the corresponding FN curve.
具体实施方式 Detailed ways
结合以下具体实施例和附图，对本发明作进一步的详细说明，本发明的保护内容不局限于以下实施例。在不背离发明构思的精神和范围下，本领域技术人员能够想到的变化和优点都被包括在本发明中，并且以所附的权利要求书为保护范围。 The present invention will be described in further detail in conjunction with the following specific examples and accompanying drawings, and the protection content of the present invention is not limited to the following examples. Without departing from the spirit and scope of the inventive concept, changes and advantages conceivable by those skilled in the art are all included in the present invention, and the appended claims are the protection scope.
本发明制备方法包括以下具体步骤： The preparation method of the present invention comprises the following concrete steps:
a、将偏钒酸铵溶于80ml去离子水中，加入30% H2O2，再滴加硝酸使其混合溶液的pH值到2，搅拌至完全溶解；加入表面活化剂聚乙烯吡咯烷酮，再次搅拌至完全溶解。其中，偏钒酸铵与H2O2的摩尔质量比V:H2O2为1:10。 a. Dissolve ammonium metavanadate in 80ml deionized water, add 30% H 2 O 2 , then add nitric acid dropwise to make the pH value of the mixed solution reach 2, stir until completely dissolved; add surfactant polyvinylpyrrolidone, again Stir until completely dissolved. Wherein, the molar mass ratio V:H 2 O 2 of ammonium metavanadate to H 2 O 2 is 1:10.
b、将步骤a制备的溶液倒入高压反应釜中，将高压釜密封好后放入鼓风干燥箱，在180℃温度下保持反应24小时，自然降温后，过滤、清洗得到黄色粉末状材料； b. Pour the solution prepared in step a into an autoclave, seal the autoclave, put it into a blast drying oven, and keep the reaction at 180°C for 24 hours. After cooling down naturally, filter and wash to obtain a yellow powdery material ;
c、将步骤b得到黄色粉末状材料在鼓风干燥箱中60℃-80℃温度下保持12小时烘干，制得的由很多一维纳米线组成的杨梅状V2O5纳米材料。 c. Dry the yellow powdery material obtained in step b in a blast drying oven at a temperature of 60° C. to 80° C. for 12 hours to obtain a bayberry-shaped V 2 O 5 nanomaterial composed of many one-dimensional nanowires.
实施例1： Example 1:
本实施例制备一维纳米线组成的杨梅状V2O5纳米材料，具体步骤如下： In this example, a bayberry-shaped V 2 O 5 nanomaterial composed of one-dimensional nanowires is prepared, and the specific steps are as follows:
a、将偏钒酸铵0.65g 溶于80ml去离子水中，再加入30% H2O210mL，使偏钒酸铵与H2O2的摩尔质量比V:H2O2为1:10，搅拌至完全溶解，滴加硝酸使其混合溶液的pH值到2，适量的加入表面活化剂聚乙烯吡咯烷酮，使其浓度为0.05mol/L，搅拌至完全溶解，配制得到反应溶液。
a. Dissolve 0.65g of ammonium metavanadate in 80ml of deionized water, then add 10mL of 30% H 2 O 2 , so that the molar mass ratio V:H 2 O 2 of ammonium metavanadate to H 2 O 2 is 1:10 , stirred until completely dissolved, nitric acid was added dropwise to make the pH value of the
b、将上述的反应溶液倒入高压釜，将高压釜密封好后放入鼓风干燥箱，在180℃温度下保持反应24小时，自然降温后，过滤、用酒精和去离子水清洗得到黄色粉末状材料。 b. Pour the above reaction solution into an autoclave, seal the autoclave, put it into a blast drying oven, and keep the reaction at 180°C for 24 hours. After cooling down naturally, filter, wash with alcohol and deionized water to obtain a yellow color Powdered material.
c、将上述清洗得到黄色粉末状材料，在鼓风干燥箱中60℃温度下保持12小时烘干，即制得所述的由很多一维纳米线组成的杨梅状V2O5纳米材料。 c. Wash the above-mentioned yellow powdery material, and dry it in a blast drying oven at 60° C. for 12 hours to obtain the bayberry-shaped V 2 O 5 nanomaterial composed of many one-dimensional nanowires.
反应是在密封的高压釜中进行的。 The reaction was carried out in a sealed autoclave.
本实施例制备得到的一维纳米线组成的杨梅状V2O5纳米材料，由自中心衍生生长出的一维V2O5纳米线构成类似球状结构，其X射线衍射图如图1所示。经扫描电子显微镜检测，其SEM图如图2所示，中倍SEM图如图3所示，高倍TEM图如图4所示。经SEM检测，如图2所示，所得的一维纳米线组成的杨梅状V2O5纳米材料，其中单根的一维纳米线的长宽尺度范围为10−20 微米，直径为30−50 纳米。经晶体结构测定，其结构为斜方晶系结构，其晶格常数为a = 11.516 Å, b = 3.566 Å, c = 4.373Å。 The bayberry-shaped V 2 O 5 nanomaterial composed of one-dimensional nanowires prepared in this example has a similar spherical structure from the one-dimensional V 2 O 5 nanowires derived from the center, and its X-ray diffraction pattern is shown in Figure 1. Show. After scanning electron microscope inspection, the SEM image is shown in Figure 2, the medium-magnification SEM image is shown in Figure 3, and the high-magnification TEM image is shown in Figure 4. After SEM detection, as shown in Figure 2, the obtained bayberry-shaped V 2 O 5 nanomaterial composed of one-dimensional nanowires, in which the length and width scale range of a single one-dimensional nanowire is 10−20 microns, and the diameter is 30− 50 nm. According to the determination of the crystal structure, its structure is orthorhombic, and its lattice constants are a = 11.516 Å, b = 3.566 Å, c = 4.373 Å.
由于组成纳米杨梅状的V2O5的纳米线具有很大的纵横比，具有大量可作为发射点的纳米尖端，有很好的场发射特性。场发射性能的研究实验结果表明，如图5所示杨梅状V2O5纳米材料的电流-电压（J-E）曲线和其对应的F-N曲线，从中可以看出杨梅状V2O5纳米材料具有很低的开启电压和阈值电压 ；很高的场发射因子，分别为2.9 V/µm, 5.7 V/µm 和 2468，说明本发明制备出的杨梅状V2O5纳米材料有很好的场发射特性，在作为场发射电极材料上有很好的应用前景。 Since the nano wires of the V 2 O 5 nanometer bayberry shape have a large aspect ratio, there are a large number of nano-tips that can be used as emission points, and have good field emission characteristics. The experimental results of the field emission performance show that the current-voltage (JE) curve and the corresponding FN curve of the bayberry-shaped V 2 O 5 nanomaterials are shown in Figure 5, from which it can be seen that the bayberry-shaped V 2 O 5 nanomaterials have Very low turn-on voltage and threshold voltage; very high field emission factors, respectively 2.9 V/µm, 5.7 V/µm and 2468, indicating that the bayberry-shaped V 2 O 5 nanomaterials prepared by the present invention have good field emission characteristics, it has a good application prospect as a field emission electrode material.
实施例2： Example 2:
本实施例一维纳米线组成的杨梅状V2O5纳米材料的制备方法与实施例1基本相同。本实施例中，pH调节至2，于180℃温度下反应24小时，于80℃下烘干。聚乙烯吡咯烷酮加入的终浓度为0.1 mol/L，偏钒酸铵的用量为0.83g，偏钒酸铵与H2O2的摩尔质量比V:H2O2为1:10。 The preparation method of the bayberry-like V 2 O 5 nanomaterial composed of one-dimensional nanowires in this example is basically the same as that in Example 1. In this embodiment, the pH was adjusted to 2, the reaction was carried out at 180° C. for 24 hours, and the drying was carried out at 80° C. The final concentration of polyvinylpyrrolidone was 0.1 mol/L, the dosage of ammonium metavanadate was 0.83 g, and the molar mass ratio V:H 2 O 2 of ammonium metavanadate and H 2 O 2 was 1:10.
本实施例制备得到的杨梅状V2O5纳米材料与实施例1结果类似，由自中心衍生生长出的一维V2O5纳米线构成类似球状结构。其中单根的一维纳米线的长宽尺度范围为10−20 微米，直径为30−50 纳米。 The results of the bayberry-shaped V 2 O 5 nanomaterials prepared in this example are similar to those in Example 1, and the one-dimensional V 2 O 5 nanowires grown from the center form a similar spherical structure. Among them, the length and width scale range of a single one-dimensional nanowire is 10−20 microns, and the diameter is 30−50 nanometers.
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