CN102897722A - A kind of solvothermal synthesis method of α-In2Se3 nano curd - Google Patents
A kind of solvothermal synthesis method of α-In2Se3 nano curd Download PDFInfo
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- 238000004729 solvothermal method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000011669 selenium Substances 0.000 claims abstract description 33
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 30
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 17
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005642 Oleic acid Substances 0.000 claims abstract description 15
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 15
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- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
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- AKUCEXGLFUSJCD-UHFFFAOYSA-N indium(3+);selenium(2-) Chemical compound [Se-2].[Se-2].[Se-2].[In+3].[In+3] AKUCEXGLFUSJCD-UHFFFAOYSA-N 0.000 description 27
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- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于环境友好型纳米材料技术领域，涉及纳米材料的制备方法，尤其是涉及一种α-In2Se3纳米花球溶剂热合成方法。本发明提供了一种α-In2Se3纳米花球溶剂热合成方法，是以油酸为溶剂，抗坏血酸为还原剂，将硝酸铟、硒粉在反应釜中进行溶剂热合成反应，然后用无水乙醇洗涤，并离心分离干燥后制得。从生长机理上推断，该方法能适用于其他硒金属化合物纳米材料的制备。本发明的制备方法简单、成本低廉、可控性强、产物结晶性好、绿色环保；从对其低倍扫描电镜图（SEM）、高倍扫描电镜图（SEM）以及透射电镜图（TEM）的分析，制得的α-In2Se3纳米花球直径在1~2微米，是由厚度为13~15纳米的纳米片所组成的。
The invention belongs to the technical field of environment-friendly nano materials, and relates to a preparation method of nano materials, in particular to a solvothermal synthesis method of α-In 2 Se 3 nano curds. The invention provides a method for solvothermal synthesis of α-In 2 Se 3 nano curds, using oleic acid as a solvent and ascorbic acid as a reducing agent, carrying out solvothermal synthesis of indium nitrate and selenium powder in a reactor, and then using Washed with absolute ethanol, and obtained after centrifugation and drying. Inferred from the growth mechanism, this method can be applied to the preparation of other selenium metal compound nanomaterials. The preparation method of the present invention is simple, low in cost, strong in controllability, good in product crystallinity, and environmentally friendly; from its low-power scanning electron microscope (SEM), high-power scanning electron microscope (SEM) and transmission electron microscope (TEM) According to the analysis, the diameter of the prepared α-In 2 Se 3 nano curd is 1-2 microns, and it is composed of nano-sheets with a thickness of 13-15 nanometers.
Description
技术领域 technical field
本发明属于环境友好型纳米材料技术领域，涉及纳米材料的制备方法，尤其是涉及一种α-In2Se3纳米花球溶剂热合成方法。 The invention belongs to the technical field of environment-friendly nano materials, and relates to a preparation method of nano materials, in particular to a solvothermal synthesis method of α-In 2 Se 3 nano curds.
背景技术 Background technique
硒化物金属半导体纳米材料由于其独特的物理性能和化学性能，同时可以广泛应用于能量、医药、传感器等重要的领域而引起了越来越多人的重视。在众多的硒化物中，硒化铟作为重要的Ⅲ-Ⅵ 主族化合物，是由Se-In-In-Se键组成的层状结构，层与层之间强烈的共价键和微弱的范德华力使得其具有高度的各向异性、电学、光学和磁学、催化和气敏等性能，从而使硒化铟在相转换器、偏振辐射、光电太阳能电池、锂电池、荧光装置、电介质、场效应晶体管等装置上有了广泛的应用。同时，硒化铟还可以作为结构单元制备不同的三元物质如CuInSe2, AgInSe2 和 四元物质Cu(In,Ga)Se2，而这些物质也是很好的光电材料被广泛应用于光电材料装置上。另外，硒化铟是一种直接能带隙为1.7eV的光电材料，由于光电子的各向异性，在可见光波范围内有很高的吸收系数，能有效的将太阳能转化为电能，是一种优异的光伏能源材料。同时，与硒化镉和硒化铅等良好的光电材料相比，硒化铟在低能带隙纳米材料中还具有低毒性和环境友好性。 Selenide metal semiconductor nanomaterials have attracted more and more attention due to their unique physical and chemical properties, and can be widely used in important fields such as energy, medicine, and sensors. Among many selenides, indium selenide, as an important III-VI main group compound, is a layered structure composed of Se-In-In-Se bonds, strong covalent bonds between layers and weak van der Waals The force makes it have a high degree of anisotropy, electricity, optics and magnetism, catalysis and gas sensitivity, so that indium selenide can be used in phase converters, polarized radiation, photoelectric solar cells, lithium batteries, fluorescent devices, dielectrics, field effects Transistors and other devices have been widely used. At the same time, indium selenide can also be used as a structural unit to prepare different ternary substances such as CuInSe 2 , AgInSe 2 and quaternary substance Cu(In,Ga)Se 2 , and these substances are also good optoelectronic materials and are widely used in optoelectronic materials on the device. In addition, indium selenide is a photoelectric material with a direct energy bandgap of 1.7eV. Due to the anisotropy of photoelectrons, it has a high absorption coefficient in the visible light range and can effectively convert solar energy into electrical energy. Excellent photovoltaic energy materials. At the same time, compared with good optoelectronic materials such as cadmium selenide and lead selenide, indium selenide also has low toxicity and environmental friendliness among low energy bandgap nanomaterials.
尽管对于硒化铟的研究从未停歇过，但是要合成单一、纯相的硒化铟并非易事。在合成过程中，硒化铟所遇到的困难主要来自于硒化铟相图的局限性。硒化铟有InSe, In2Se3, In4Se3和In6Se7 四种复杂的组合形式，这几种不同的组成成分在某一范围之内往往同时存在于硒化铟中。另外单单In2Se3这种组成形式，其成相***就特别复杂，例如，In2Se3有 α, β, γ, δ和 κ五种晶型，而晶型与晶型之间很容易相互进行转换，所以要想得到单一组成并且单一晶型的In2Se3，显得尤其困难。 Although the research on indium selenide has never stopped, it is not easy to synthesize a single, pure phase of indium selenide. During the synthesis process, the difficulties encountered by indium selenide mainly come from the limitations of the phase diagram of indium selenide. Indium selenide has four complex combinations of InSe, In 2 Se 3 , In 4 Se 3 and In 6 Se 7. These different components often exist in indium selenide at the same time within a certain range. In addition, the composition form of In 2 Se 3 alone has a particularly complex phase system. For example, In 2 Se 3 has five crystal forms of α, β, γ, δ, and κ, and the crystal forms are easily separated. mutual conversion, so it is particularly difficult to obtain In 2 Se 3 with a single composition and a single crystal form.
目前为止，有关合成In2Se3的方法陆续报道出来，但是大部分的合成方法则局限于气相合成方法、有机化学蒸汽分解法以及电化学沉积法等传统的方法。而且上述合成方法需要高端精密的仪器，反应温度在400~1000℃，能耗大，并且会产生毒性气体，对人体和环境造成一定的危害，并且这些方法得到的样品还具有不均一和低产量等特点。因此寻找一个简单、低廉、绿色、可控的方法，合成硒化铟纳米结构是很有必要并且富有挑战性的。 So far, methods for synthesizing In 2 Se 3 have been reported successively, but most of the synthesis methods are limited to traditional methods such as gas phase synthesis, organic chemical vapor decomposition, and electrochemical deposition. Moreover, the above synthesis methods require high-end precision instruments, the reaction temperature is 400-1000°C, the energy consumption is large, and toxic gases will be produced, which will cause certain harm to the human body and the environment, and the samples obtained by these methods are also inhomogeneous and low-yield. Features. Therefore, it is necessary and challenging to find a simple, cheap, green, and controllable method to synthesize InSe nanostructures.
水热法具有设备简单、原料容易获得、得到的产物纯度高、均匀性好、化学组成控制准确等优点而受到许多研究学者的青睐。水热法是在特制的密闭反应器（高压釜）中，以水或有机溶剂等流体为反应物质，通过将反应体系加热至临界温度（或者是接近临界温度），创造出一个高温高压反应环境，促使反应在液相或气相中进行，使原本难溶或不溶的物质溶剂并重结晶，再经过分离和热处理得到产物的一种有效方法。水热法具有以下优点：（1）采用中温（一般在120~220℃之间）液相控制，能耗相对较低，适用性广，既可用于尺寸较小的纳米粒子制备，也可以得到尺寸较大的单晶；（2）原料相对廉价易得，反应在液相快速对流中进行，产率高、物相均匀、纯度高、结晶良好，而且形状大小可控;（3）在水热过程中，可通过调节反应温度、压力、时间、pH 值、前驱物和表面活性剂等，达到有效控制反应和晶体生长特性的目的；（4）反应在密封的容器中进行，适用于有毒体系中的合成反应，可减少环境污染。 The hydrothermal method has the advantages of simple equipment, easy access to raw materials, high purity, good uniformity, and accurate control of chemical composition of the obtained product, so it is favored by many researchers. The hydrothermal method is to create a high-temperature and high-pressure reaction environment by heating the reaction system to the critical temperature (or close to the critical temperature) in a special closed reactor (autoclave) with fluids such as water or organic solvents as the reaction substance. It is an effective method to promote the reaction to proceed in the liquid phase or gas phase, to solvent and recrystallize the originally poorly soluble or insoluble substance, and then to obtain the product through separation and heat treatment. The hydrothermal method has the following advantages: (1) It adopts medium temperature (generally between 120~220°C) liquid phase control, relatively low energy consumption, and wide applicability. Single crystal with large size; (2) The raw materials are relatively cheap and easy to obtain, and the reaction is carried out in the rapid convection of the liquid phase, with high yield, uniform phase, high purity, good crystallization, and controllable shape and size; (3) In water In the thermal process, the purpose of effectively controlling the reaction and crystal growth characteristics can be achieved by adjusting the reaction temperature, pressure, time, pH value, precursors and surfactants; (4) The reaction is carried out in a sealed container, suitable for toxic The synthesis reaction in the system can reduce environmental pollution.
但是利用水热法制备硒化铟却鲜有报道，只有2011年，杨等人用乙醇作为溶剂在220℃下水热合成出了γ-In2Se3的微球，这种球的直径在2-4微米。由于物质的尺寸对于性质有很大的影响，所以合成小尺寸的硒化铟是很有必要的。另外，截止目前，还没有对于形貌可控的α-In2Se3溶剂热合成的报道。因此，应用溶剂热合成方法，合成单一成分、形貌可控的α-In2Se3势在必行。 However, there are few reports on the preparation of indium selenide by the hydrothermal method. Only in 2011, Yang et al. used ethanol as a solvent to hydrothermally synthesize γ-In 2 Se 3 microspheres at 220°C. -4 microns. Since the size of the substance has a great influence on the properties, it is necessary to synthesize small-sized indium selenide. In addition, up to now, there is no report on the solvothermal synthesis of α-In 2 Se 3 with controllable morphology. Therefore, it is imperative to synthesize α-In 2 Se 3 with single component and controllable morphology by solvothermal synthesis method.
发明内容 Contents of the invention
针对现有技术中存在的缺陷和不足，本发明提供了一种α-In2Se3纳米花球的溶剂热合成方法，是以油酸为溶剂，抗坏血酸为还原剂，将硝酸铟、硒粉在反应釜中溶剂热合成反应，然后用无水乙醇洗涤，并离心分离干燥后制得。从生长机理上推断，该方法能适用于其他硒金属化合物纳米材料的制备。 Aiming at the defects and deficiencies in the prior art, the invention provides a solvothermal synthesis method of α-In 2 Se 3 nano curds, which uses oleic acid as a solvent and ascorbic acid as a reducing agent, and indium nitrate, selenium powder Solvothermal synthesis reaction in a reaction kettle, then washed with absolute ethanol, and obtained after centrifugal separation and drying. Inferred from the growth mechanism, this method can be applied to the preparation of other selenium metal compound nanomaterials.
一种α-In2Se3纳米花球溶剂热合成方法，所述的溶剂热合成反应包括如下步骤： A method for solvothermal synthesis of α-In 2 Se 3 nano curds, wherein the solvothermal synthesis reaction comprises the steps:
步骤Ａ、称取一定量的硝酸铟、硒粉、抗坏血酸于反应釜中混合，其中，所述的硝酸铟、硒粉、抗坏血酸的摩尔比为3:1:1~2； Step A, taking a certain amount of indium nitrate, selenium powder, and ascorbic acid and mixing them in a reaction kettle, wherein the molar ratio of the indium nitrate, selenium powder, and ascorbic acid is 3:1:1~2;
步骤Ｂ、加入油酸搅拌30min，其中所述油酸的体积占反应釜的60%~80%； Step B, adding oleic acid and stirring for 30 minutes, wherein the volume of oleic acid accounts for 60% to 80% of the reactor;
步骤C、将反应釜于190℃~220℃下反应12h~24h，然后冷却至室温。 Step C, react the reactor at 190°C~220°C for 12h~24h, then cool to room temperature.
在本发明的一个较优实施例中，所述的硝酸铟、硒粉、抗坏血酸的摩尔比为3:1:1； In a preferred embodiment of the present invention, the mol ratio of described indium nitrate, selenium powder, ascorbic acid is 3:1:1;
所述油酸的体积占反应釜的80%； The volume of described oleic acid accounts for 80% of reactor;
所述的反应釜于200℃下反应24h。 The reaction kettle was reacted at 200° C. for 24 hours.
将所得到的产物在室温条件下用无水乙醇洗涤，并离心分离取其下层沉淀，真空干燥后得到黑色的粉末。 The obtained product was washed with absolute ethanol at room temperature, and centrifuged to obtain the lower layer precipitate, which was dried in vacuum to obtain a black powder.
根据上述溶剂热合成方法制备而成的α-In2Se3纳米花球，从对其低倍扫描电镜图（SEM）、高倍扫描电镜图（SEM）以及透射电镜图（TEM）的分析，所述的α-In2Se3纳米花球直径在1~2微米，是由厚度为13~15nm的纳米片所组成的。 The α-In 2 Se 3 nano-curds prepared according to the above solvothermal synthesis method, from the analysis of its low-power scanning electron microscope (SEM), high-power scanning electron microscope (SEM) and transmission electron microscope (TEM), the results are The above-mentioned α-In 2 Se 3 nano curd has a diameter of 1-2 microns and is composed of nano-sheets with a thickness of 13-15 nm.
有益效果Beneficial effect
本发明的制备方法简单、成本低廉、可控性强、产物结晶性好、绿色环保。 The preparation method of the invention is simple, low in cost, strong in controllability, good in product crystallinity, and environmentally friendly.
附图说明 Description of drawings
图1 制备的花球状硒化铟的X射线衍射分析图（XRD）； Figure 1 The X-ray diffraction analysis pattern (XRD) of the prepared flower-like indium selenide;
图2 制备的花球状硒化铟的低倍扫描电镜图（SEM）； Fig. 2 The low-magnification scanning electron microscope (SEM) of the prepared flower-shaped indium selenide;
图3 制备的花球状硒化铟的高倍扫描电镜图（SEM）； Figure 3 The high-magnification scanning electron microscope image (SEM) of the prepared flower-shaped indium selenide;
图4 制备的花球状硒化铟透射电镜图（TEM）。 Fig. 4 Transmission electron microscope image (TEM) of the flower-shaped indium selenide prepared.
具体实施方式 Detailed ways
下面结合实施例对本发明进行详细说明，以使本领域技术人员更好地理解本发明，但本发明并不局限于以下实施例。 The present invention will be described in detail below in conjunction with the examples, so that those skilled in the art can better understand the present invention, but the present invention is not limited to the following examples.
实施例1： Example 1:
一种合成α-In2Se3纳米花球的溶剂热法，具体步骤如下： A kind of solvothermal method of synthesizing α-In 2 Se 3 nano curds, concrete steps are as follows:
（1）用电子天平分别称取0.2292g硝酸铟，0.0158g硒粉，0.0352g抗坏血酸，30ml油酸于50ml反应釜中，磁子进行搅拌30分钟 ； (1) Weigh 0.2292g of indium nitrate, 0.0158g of selenium powder, 0.0352g of ascorbic acid, and 30ml of oleic acid in a 50ml reactor with an electronic balance, and stir for 30 minutes with a magnet;
（2）将反应釜密封放入200℃烘箱中恒温24小时，然后自然冷却至室温，用无水乙醇洗涤8遍，于60℃真空烘箱中干燥得到黑色花球状硒化铟。 (2) Seal the reaction kettle and place it in an oven at 200°C for 24 hours at a constant temperature, then cool it down to room temperature naturally, wash it with absolute ethanol 8 times, and dry it in a vacuum oven at 60°C to obtain a black spherical indium selenide.
图1是制备的花球状硒化铟的XRD图，从图中可以看出所得到物质的峰型和粉末衍射标准联合委员会（JCPDS）卡片34-1313相吻合，而且此峰中没有其他杂质的峰，说明得到的是纯相的α-In2Se3。 Figure 1 is the XRD pattern of the prepared flower spherical indium selenide. It can be seen from the figure that the peak shape of the obtained substance is consistent with that of the Joint Committee for Powder Diffraction Standards (JCPDS) card 34-1313, and there are no peaks of other impurities in this peak , indicating that the obtained phase is pure α-In 2 Se 3 .
图2是制备的花球状硒化铟的低倍SEM图，从图中可以看出，花球分散性比较好，而且表面比较粗糙，直径大约在1-2微米。 Figure 2 is a low-magnification SEM image of the prepared curd-shaped indium selenide. It can be seen from the figure that the curd has better dispersion and a rough surface, with a diameter of about 1-2 microns.
图3是制备的花球状硒化铟的高倍SEM图，从图中可以看出，花球是由厚度为15纳米左右的纳米片所组成的。 Fig. 3 is a high-magnification SEM image of the prepared curd-shaped indium selenide. It can be seen from the figure that the curd is composed of nanosheets with a thickness of about 15 nanometers.
图4是制备的花球状硒化铟TEM图，更进一步说明了花球是由片所组成的。 Figure 4 is a TEM image of the prepared curd-shaped indium selenide, which further illustrates that the curd is composed of flakes.
实施例2： Example 2:
一种合成α-In2Se3纳米花球的溶剂热法，具体步骤如下： A kind of solvothermal method of synthesizing α-In 2 Se 3 nano curds, concrete steps are as follows:
（1）用电子天平分别称取0.2292g硝酸铟，0.0158g硒粉，0.0704g抗坏血酸，30ml油酸于50ml反应釜中，磁子进行搅拌30分钟 ； (1) Weigh 0.2292g of indium nitrate, 0.0158g of selenium powder, 0.0704g of ascorbic acid, and 30ml of oleic acid in a 50ml reactor with an electronic balance, and stir for 30 minutes with a magnet;
（2）将反应釜密封放入200℃烘箱中恒温24小时，然后自然冷却至室温，用无水乙醇洗涤8遍，于60℃真空烘箱中干燥得到黑色花球状硒化铟。 (2) Seal the reaction kettle and place it in an oven at 200°C for 24 hours at a constant temperature, then cool it down to room temperature naturally, wash it with absolute ethanol 8 times, and dry it in a vacuum oven at 60°C to obtain a black spherical indium selenide.
实施例3： Example 3:
一种合成α-In2Se3纳米花球的溶剂热法，具体步骤如下： A kind of solvothermal method of synthesizing α-In 2 Se 3 nano curds, concrete steps are as follows:
（1）用电子天平分别称取0.2292g硝酸铟，0.0158g硒粉，0.0352g抗坏血酸，40ml油酸于50ml反应釜中，磁子进行搅拌30分钟 ； (1) Weigh 0.2292g of indium nitrate, 0.0158g of selenium powder, 0.0352g of ascorbic acid, 40ml of oleic acid in a 50ml reactor with an electronic balance, and stir for 30 minutes with a magnet;
（2）将反应釜密封放入200℃烘箱中恒温24小时，然后自然冷却至室温，用无水乙醇洗涤8遍，于60℃真空烘箱中干燥得到黑色花球状硒化铟。 (2) Seal the reaction kettle and place it in an oven at 200°C for 24 hours at a constant temperature, then cool it down to room temperature naturally, wash it with absolute ethanol 8 times, and dry it in a vacuum oven at 60°C to obtain a black spherical indium selenide.
实施例4： Example 4:
一种合成α-In2Se3纳米花球的溶剂热法，具体步骤如下： A kind of solvothermal method of synthesizing α-In 2 Se 3 nano curds, concrete steps are as follows:
（1）用电子天平分别称取0.2292g硝酸铟，0.0158g硒粉，0.0352g抗坏血酸，40ml油酸于50ml反应釜中，磁子进行搅拌30分钟 ； (1) Weigh 0.2292g of indium nitrate, 0.0158g of selenium powder, 0.0352g of ascorbic acid, and 40ml of oleic acid in a 50ml reactor with an electronic balance, and stir for 30 minutes with a magnet;
（2）将反应釜密封放入190℃烘箱中恒温24小时，然后自然冷却至室温，用无水乙醇洗涤8遍，于60℃真空烘箱中干燥得到黑色花球状硒化铟。 (2) Seal the reaction kettle and place it in an oven at 190°C for 24 hours at a constant temperature, then cool it down to room temperature naturally, wash it with absolute ethanol 8 times, and dry it in a vacuum oven at 60°C to obtain a black spherical indium selenide.
实施例5： Example 5:
一种合成α-In2Se3纳米花球的溶剂热法，具体步骤如下： A kind of solvothermal method of synthesizing α-In 2 Se 3 nano curds, concrete steps are as follows:
（1）用电子天平分别称取0.2292g硝酸铟，0.0158g硒粉，0.0352g抗坏血酸，40ml油酸于50ml反应釜中，磁子进行搅拌30分钟 ； (1) Weigh 0.2292g of indium nitrate, 0.0158g of selenium powder, 0.0352g of ascorbic acid, and 40ml of oleic acid in a 50ml reactor with an electronic balance, and stir for 30 minutes with a magnet;
（2）将反应釜密封放入220℃烘箱中恒温24小时，然后自然冷却至室温，用无水乙醇洗涤8遍，于60℃真空烘箱中干燥得到黑色花球状硒化铟。 (2) Seal the reaction kettle and place it in an oven at 220°C for 24 hours at a constant temperature, then cool it down to room temperature naturally, wash it with absolute ethanol 8 times, and dry it in a vacuum oven at 60°C to obtain a black spherical indium selenide.
实施例6： Embodiment 6:
一种合成α-In2Se3纳米花球的溶剂热法，具体步骤如下： A kind of solvothermal method of synthesizing α-In 2 Se 3 nano curds, concrete steps are as follows:
（1）用电子天平分别称取0.2292g硝酸铟，0.0158g硒粉，0.0352g抗坏血酸，40ml油酸于50ml反应釜中，磁子进行搅拌30分钟 ； (1) Weigh 0.2292g of indium nitrate, 0.0158g of selenium powder, 0.0352g of ascorbic acid, and 40ml of oleic acid in a 50ml reactor with an electronic balance, and stir for 30 minutes with a magnet;
（2）将反应釜密封放入200℃烘箱中恒温12小时，然后自然冷却至室温，用无水乙醇洗涤8遍，于60℃真空烘箱中干燥得到黑色花球状硒化铟。 (2) Seal the reaction kettle and place it in an oven at 200°C for 12 hours at a constant temperature, then cool it down to room temperature naturally, wash it with absolute ethanol 8 times, and dry it in a vacuum oven at 60°C to obtain a black spherical indium selenide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273079A (en) * | 2013-05-10 | 2013-09-04 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
| CN111841583A (en) * | 2020-08-12 | 2020-10-30 | 西安近代化学研究所 | Preparation method of indium selenide/titanium dioxide nanosheet composite material |
| CN111960390A (en) * | 2020-08-06 | 2020-11-20 | 西安近代化学研究所 | Preparation method of monodisperse gamma-indium selenide nano particles |
| CN114988371A (en) * | 2022-06-10 | 2022-09-02 | 南昌航空大学 | Size-controllable solvent-thermal synthesized indium zinc selenide nanosheet and preparation method and application thereof |
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Non-Patent Citations (2)
| Title |
|---|
| 《CrystEngComm》 20110221 Xiaoyan Tan et al. Ascorbic acid-assisted solvothermal growth of gamma-In2Se3 hierarchical flowerlike architectures 2792-2798页 1-6 第13卷, * |
| XIAOYAN TAN ET AL.: "Ascorbic acid-assisted solvothermal growth of γ-In2Se3 hierarchical flowerlike architectures", 《CRYSTENGCOMM》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273079A (en) * | 2013-05-10 | 2013-09-04 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN103273079B (en) * | 2013-05-10 | 2015-07-22 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
| CN111960390A (en) * | 2020-08-06 | 2020-11-20 | 西安近代化学研究所 | Preparation method of monodisperse gamma-indium selenide nano particles |
| CN111841583A (en) * | 2020-08-12 | 2020-10-30 | 西安近代化学研究所 | Preparation method of indium selenide/titanium dioxide nanosheet composite material |
| CN111841583B (en) * | 2020-08-12 | 2023-04-18 | 西安近代化学研究所 | Preparation method of indium selenide/titanium dioxide nanosheet composite material |
| CN114988371A (en) * | 2022-06-10 | 2022-09-02 | 南昌航空大学 | Size-controllable solvent-thermal synthesized indium zinc selenide nanosheet and preparation method and application thereof |
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