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CN116574483A - A kind of preparation method of tellurium nanowire multi-component composite material - Google Patents

A kind of preparation method of tellurium nanowire multi-component composite material Download PDF

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CN116574483A
CN116574483A CN202310534446.1A CN202310534446A CN116574483A CN 116574483 A CN116574483 A CN 116574483A CN 202310534446 A CN202310534446 A CN 202310534446A CN 116574483 A CN116574483 A CN 116574483A
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heating
stirring
tellurium
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布和巴特尔
王新雨
孙源涛
陈芾霖
花雨
谭庆浩
文子良
姚蓉
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Heilongjiang Institute of Technology
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Abstract

A preparation method of tellurium nanowire multi-element composite material, belonging to the technical field of composite material preparation. The method comprises the following steps: mixing a tellurium source with a volatilizable alcohol solvent, heating and stirring uniformly to obtain a solution I; mixing, heating and uniformly stirring a surfactant and a volatilizable alcohol solvent to obtain a solution II; mixing an alkaline compound with an alcohol solvent, heating and stirring uniformly to obtain a solution III; heating and uniformly stirring the solution I, the solution II and the solution III to obtain a mixed solution; introducing inert gas into the mixed solution, adding a reducing agent, heating and stirring uniformly to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain a tellurium nanowire composite material mixed solution; and (3) washing the final product with the mixed solvent for multiple times, and centrifugally drying to obtain the tellurium nanowire multi-element composite material. The invention has the advantages of short preparation period, simple and controllable process, safety, no pollution, low energy consumption, excellent product performance, suitability for laboratory preparation, large-scale production in factories and the like.

Description

一种碲纳米线多元复合材料的制备方法A kind of preparation method of tellurium nanowire multi-component composite material

技术领域technical field

本发明属于复合材料制备技术领域,具体涉及一种碲纳米线多元复合材料的制备方法。The invention belongs to the technical field of composite material preparation, and in particular relates to a preparation method of tellurium nanowire multi-component composite material.

背景技术Background technique

碲是一种准金属元素,现如今逐渐发展成为一种支撑高精技术发展的材料,在冶金工业、石油化工、电子工业、新能源技术中可作为新型红外探测材料、玻璃着色剂、发电组件、新型薄膜太阳能电池关键材料等。将碲制成纳米线,利用其各向异性获得优异的光电性能,碲纳米线与贵金属或化合物的二元复合可进一步增强其光电性能。但是研究碲纳米线及其复合材料的电磁波吸收性能的报道较少。石墨烯和Mxene等2D结构材料在电磁波吸收领域应用时有比重轻、吸收值高等优点,如果将碲纳米线与2D结构石墨烯和Mxene进行复合,有望进一步提高其电磁波吸收性能。但是关于碲纳米线/石墨烯/Mxene等多元复合材料的制备及在电磁吸收性能的分析相关报道较少。因此,如果发明一种可大规模低成本制备碲纳米线/石墨烯/Mxene复合材料的方法,有望获得一种高性能电磁波吸收材料来满足该领域的应用需求。Tellurium is a metalloid element, and now it has gradually developed into a material that supports the development of high-precision technology. It can be used as a new type of infrared detection material, glass colorant, and power generation component in metallurgical industry, petrochemical industry, electronic industry, and new energy technology. , Key materials for new thin-film solar cells, etc. Tellurium is made into nanowires, and its anisotropy is used to obtain excellent photoelectric properties. Binary recombination of tellurium nanowires with noble metals or compounds can further enhance its photoelectric properties. However, there are few reports on the electromagnetic wave absorption properties of tellurium nanowires and their composites. 2D structural materials such as graphene and Mxene have the advantages of light specific gravity and high absorption value in the field of electromagnetic wave absorption. If tellurium nanowires are combined with 2D structured graphene and Mxene, it is expected to further improve their electromagnetic wave absorption performance. However, there are few reports on the preparation of multiple composite materials such as tellurium nanowires/graphene/Mxene and the analysis of their electromagnetic absorption properties. Therefore, if a method for large-scale and low-cost preparation of tellurium nanowires/graphene/Mxene composites is invented, it is expected to obtain a high-performance electromagnetic wave absorbing material to meet the application requirements in this field.

《基于水热法的碲化物纳米线的合成》(材料科学2018年04期)中以维生素C、CTAB、亚碲酸钠、四水硝酸镉为原材料,利用水热法制备了碲化物纳米线。该方法虽然有制备环境容易等优点。但实验过程中危险性较大,制备的纳米线容易团聚,影响了其性能。In "Synthesis of Telluride Nanowires Based on Hydrothermal Method" (Material Science, Issue 04, 2018), vitamin C, CTAB, sodium tellurite, and cadmium nitrate tetrahydrate were used as raw materials to prepare telluride nanowires by hydrothermal method . Although this method has advantages such as preparation environment is easy. However, the risk is greater during the experiment, and the prepared nanowires are easy to agglomerate, which affects their performance.

《热蒸发法制备金属碲纳米线》(稀有金属材料与工程.2021,50(10))中将高纯Bi2Te3作为蒸发源,在涂有Au的石英片上成功制备出了一维碲纳米线,该实验深度分析了高纯一维Te纳米线的生长机制。该实验需要高温条件才能获得最终产品,而且产率较低,制备成本相对较高,产品没有市场竞争力。In "Preparation of Metal Tellurium Nanowires by Thermal Evaporation" (Rare Metal Materials and Engineering. 2021, 50(10)), high-purity Bi 2 Te 3 was used as the evaporation source, and one-dimensional tellurium was successfully prepared on Au-coated quartz wafers. Nanowires, this experiment deeply analyzed the growth mechanism of high-purity one-dimensional Te nanowires. This experiment requires high temperature conditions to obtain the final product, and the yield is low, the preparation cost is relatively high, and the product has no market competitiveness.

《Environmentally Benign Synthesis ofUltrathin Metal TellurideNanowires》(美国化学学会杂志2014年7月8日)中以TeO2、KOH、抗坏血酸为原材料制备出前驱体,利用水热法将Cu、Ag等贵金属与前驱体复合,制备出了超薄碲纳米线复合材料。该实验制备过程绿色环保,最终实验产品纳米线直径短。"Environmentally Benign Synthesis of Ultrathin Metal Telluride Nanowires" (Journal of the American Chemical Society, July 8, 2014) prepared precursors using TeO 2 , KOH, and ascorbic acid as raw materials, and used the hydrothermal method to compound precious metals such as Cu and Ag with the precursors. Ultrathin tellurium nanowire composites were prepared. The experimental preparation process is green and environmentally friendly, and the final experimental product nanowire has a short diameter.

《一种柔性还原石墨烯与碲纳米线复合热电薄膜的制备方法》(申请号201511023207.1)中以氧化石墨烯粉末和苯乙烯磺酸钠为原料,通过水热法、真空抽滤等步骤获得碲纳米线/玻璃纤维膜初始样品,在高温、惰性气体保护下反应得到最终产品。该产品具有较高的Seebeck系数,具有很好的热电转换性能。但因为该方法制备流程过于复杂,实验环境苛刻,严重影响了推广应用。"A Preparation Method for Flexible Reduced Graphene and Tellurium Nanowire Composite Thermoelectric Film" (application number 201511023207.1) uses graphene oxide powder and sodium styrene sulfonate as raw materials to obtain tellurium through hydrothermal method, vacuum filtration and other steps The initial sample of nanowire/glass fiber membrane is reacted at high temperature and under the protection of inert gas to obtain the final product. The product has a high Seebeck coefficient and has good thermoelectric conversion performance. However, the preparation process of this method is too complicated and the experimental environment is harsh, which seriously affects the popularization and application.

综上所述,碲纳米线已经成为重要的功能材料而被广泛研究,特别是与其它材料复合后能表现出更加优异的性能。但是对碲纳米线/石墨烯/Mxene等层状2d结构复合的报道较少。To sum up, tellurium nanowires have become important functional materials and have been widely studied, especially when combined with other materials, they can show more excellent performance. However, there are few reports on the recombination of layered 2d structures such as tellurium nanowires/graphene/Mxene.

发明内容Contents of the invention

本发明解决了目前国内没有碲纳米线多元复合材料的空白,提供一种碲纳米线多元复合材料的制备方法,该方法将碲纳米线与性能优良材料如石墨烯、Mxene等进行复合,可以得到光电磁性能优异半导体材料,可应用在电磁波吸收等领域。The present invention solves the gap that there is no multi-component composite material of tellurium nanowires in China at present, and provides a preparation method of multi-component composite material of tellurium nanowires. In the method, the tellurium nanowires are composited with materials with excellent performance such as graphene, Mxene, etc., and can obtain Semiconductor materials with excellent optical and electromagnetic properties can be used in electromagnetic wave absorption and other fields.

为实现上述目的,本发明采取的技术方案如下:In order to achieve the above object, the technical scheme that the present invention takes is as follows:

一种碲纳米线多元复合材料的制备方法,所述方法为:A method for preparing a tellurium nanowire multi-component composite material, the method comprising:

步骤一:将碲源与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅰ;Step 1: Mix the tellurium source and the volatile alcohol solvent in a certain ratio, heat and stir to obtain a solution I;

步骤二:将表面活性剂与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅱ;Step 2: Mix the surfactant and the volatile alcohol solvent in a certain proportion, heat and stir evenly to obtain solution II;

步骤三:将碱性化合物与醇类溶剂以一定比例混合加热搅拌均匀获得溶液III;Step 3: Mix the basic compound and alcohol solvent in a certain proportion, heat and stir to obtain solution III;

步骤四:将溶液Ⅰ、溶液Ⅱ、溶液Ⅲ置于三颈烧瓶加热并搅拌均匀得到混合溶液;Step 4: Put solution I, solution II, and solution III in a three-necked flask to heat and stir to obtain a mixed solution;

步骤五:向混合溶液中通入惰性气体,于一定温度下加入还原剂并加热搅拌均匀得到前驱体,向前驱体中加入需要复合的材料、抗氧化剂后得到碲纳米线复合材料混合溶液;Step 5: Inject an inert gas into the mixed solution, add a reducing agent at a certain temperature, heat and stir evenly to obtain a precursor, add materials to be composited and an antioxidant to the precursor to obtain a mixed solution of tellurium nanowire composite material;

步骤六:用一定体积比例的混合溶剂将最终产物进行水洗多次离心干燥得到碲纳米线多元复合材料。Step 6: The final product is washed with water for several times and centrifugally dried with a mixed solvent in a certain volume ratio to obtain a multi-component tellurium nanowire composite material.

进一步地,步骤一中,所述碲源为二氧化碲、三氧化碲或亚碲酸钠中的一种或多种;所述可挥发醇类溶剂为乙二醇、乙醇、丙三醇、异丁醇或甲醇中的一种或多种;所述碲源与可挥发醇类溶剂的质量比为1:1~10;所述加热为直接加热或磁力加热,使用的加热器为可控电磁加热炉、加热棒或红外线加热器中的一种;所述搅拌为磁力搅拌或机械搅拌,搅拌转速为50r/min~500r/min;所述加热温度为25℃~100℃;所述加热搅拌时间为10min~100min。Further, in step 1, the tellurium source is one or more of tellurium dioxide, tellurium trioxide or sodium tellurite; the volatile alcohol solvent is ethylene glycol, ethanol, glycerol, One or more of isobutanol or methanol; the mass ratio of the tellurium source to the volatile alcohol solvent is 1:1-10; the heating is direct heating or magnetic heating, and the heater used is controllable One of electromagnetic heating furnace, heating rod or infrared heater; the stirring is magnetic stirring or mechanical stirring, and the stirring speed is 50r/min~500r/min; the heating temperature is 25°C~100°C; the heating Stirring time is 10min~100min.

进一步地,步骤二中,所述表面活性剂为聚乙烯吡咯烷酮、十六烷基溴化铵、油酸钠、十八胺、月桂酸钠、硬脂酸钠、十二烷基硫酸钠或十二烷基苯磺酸钠中的一种或多种;所述可挥发醇类溶剂为乙二醇、乙醇、丙三醇、异丁醇或甲醇中的一种或多种;所述表面活性剂和醇类溶剂的质量比为1:1~8;所述加热为直接加热或磁力加热;所述加热温度为30℃~90℃;所述搅拌器转速为30r/min~600r/min;所述加热搅拌时间为20min~80min。Further, in step 2, the surfactant is polyvinylpyrrolidone, cetyl ammonium bromide, sodium oleate, stearylamine, sodium laurate, sodium stearate, sodium lauryl sulfate or One or more of sodium dialkylbenzene sulfonate; the volatile alcohol solvent is one or more of ethylene glycol, ethanol, glycerol, isobutanol or methanol; the surface active The mass ratio of solvent to alcohol solvent is 1:1-8; the heating is direct heating or magnetic heating; the heating temperature is 30°C-90°C; the speed of the agitator is 30r/min-600r/min; The heating and stirring time is 20 min to 80 min.

进一步地,步骤三中,所述碱性化合物为氢氧化钾、氢氧化钠、三乙醇胺、甲胺、尿素、乙胺、乙醇胺、乙二胺、二甲胺、三甲胺、三乙胺、丙胺或异丙胺中的一种或多种;所述醇类溶剂为乙二醇、乙醇、丙三醇、异丁醇或甲醇中的一种或多种;所述搅拌为磁力搅拌或机械搅拌;所述碱性化合物和醇类溶剂的质量比为1:1~8;所述加热为直接加热或磁力加热;所述加热温度为20℃~90℃;所述搅拌器转速为30r/min~500r/min;所述加热搅拌时间为20min~90min。Further, in step three, the basic compound is potassium hydroxide, sodium hydroxide, triethanolamine, methylamine, urea, ethylamine, ethanolamine, ethylenediamine, dimethylamine, trimethylamine, triethylamine, propylamine Or one or more in isopropylamine; Described alcohol solvent is one or more in ethylene glycol, ethanol, glycerol, isobutanol or methyl alcohol; Described stirring is magnetic stirring or mechanical stirring; The mass ratio of the basic compound to the alcohol solvent is 1:1-8; the heating is direct heating or magnetic heating; the heating temperature is 20°C-90°C; the speed of the agitator is 30r/min- 500r/min; the heating and stirring time is 20min-90min.

进一步地,步骤四中,所述加热为直接加热或磁力加热;所述搅拌为磁力搅拌或机械搅拌;所述加热温度为10℃~90℃;所述搅拌器转速为20r/min~400r/min;所述加热搅拌时间为10min~90min。Further, in step 4, the heating is direct heating or magnetic heating; the stirring is magnetic stirring or mechanical stirring; the heating temperature is 10°C-90°C; the speed of the stirrer is 20r/min-400r/min min; the heating and stirring time is 10 min to 90 min.

进一步地,步骤五中,所述惰性气体为氮气或氩气中的一种或多种,气体流速为0.1L/min~5L/min;所述温度为40℃~200℃;所述还原剂为抗坏血酸、硼氢化钠、氯化亚锡、草酸或硼氢化钾中的一种或多种;所述加热为直接加热或磁力加热;所述加热时间为1h~60h;所述搅拌为磁力搅拌或机械搅拌,转速为50r/min~800r/min;所述搅拌时间为1h~60h;所述需要复合的材料为Mxene、石墨烯、硫酸铜、硝酸镍或硫酸锌中的一种或多种;所述抗氧化剂为抗坏血酸、硼氢化钠、氯化亚锡、草酸或硼氢化钾中的一种或多种。Further, in step five, the inert gas is one or more of nitrogen or argon, the gas flow rate is 0.1L/min-5L/min; the temperature is 40°C-200°C; the reducing agent One or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride; the heating is direct heating or magnetic heating; the heating time is 1h to 60h; the stirring is magnetic stirring or mechanical stirring, with a rotating speed of 50r/min to 800r/min; the stirring time is 1h to 60h; the material to be composited is one or more of Mxene, graphene, copper sulfate, nickel nitrate or zinc sulfate ; The antioxidant is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride.

进一步地,步骤六中,所述混合溶剂为乙醇和水的混合液,乙醇和水的体积比为2:1~10;混合溶剂与碲纳米线复合材料混合溶液的体积比为1:2~10;水洗次数为5~10次;离心方式为高速离心机;所述离心的速度为3000r/min~5000r/min,时间为2min~20min;所述干燥的温度为100℃~200℃,时间为1h~2h;所述碲纳米线复合材料中的碲纳米线直径为50nm~500nm,所述碲纳米线复合材料中的碲纳米线长度为10mm~50mm;所述碲纳米线复合材料的反射率为-10dB~-60dB。Further, in step six, the mixed solvent is a mixed solution of ethanol and water, and the volume ratio of ethanol and water is 2:1-10; the volume ratio of the mixed solvent and the mixed solution of the tellurium nanowire composite material is 1:2- 10; the number of washing times is 5 to 10 times; the centrifugation method is a high-speed centrifuge; the speed of the centrifugation is 3000r/min to 5000r/min, and the time is 2min to 20min; the drying temperature is 100°C to 200°C, and the time is 1h~2h; the tellurium nanowire diameter in the tellurium nanowire composite material is 50nm~500nm, the tellurium nanowire length in the tellurium nanowire composite material is 10mm~50mm; the reflection of the tellurium nanowire composite material Rate -10dB ~ -60dB.

本发明相对于现有技术的有益效果为:The beneficial effect of the present invention relative to prior art is:

1、本发明制备的碲纳米线/石墨烯/Mxene复合材料,通过将一维碲纳米线与二维石墨烯和Mxene等进行复合形成三维结构复合材料,电磁波在三维结构材料中通过多次折射达到较高的损耗。1. The tellurium nanowire/graphene/Mxene composite material prepared by the present invention forms a three-dimensional structural composite material by combining one-dimensional tellurium nanowire with two-dimensional graphene and Mxene, etc., and electromagnetic waves are refracted multiple times in the three-dimensional structural material achieve higher losses.

2、利用极性溶剂和表面活性剂的极性将碲纳米线、石墨烯和Mxene三种材料紧密的结合一起,当收到电磁波辐射时会产生多种界面极化从而损耗电磁波。2. Using the polarity of polar solvents and surfactants to closely combine the three materials of tellurium nanowires, graphene and Mxene, when receiving electromagnetic wave radiation, various interface polarizations will be generated and electromagnetic waves will be lost.

3、本发明可以调控各步骤的反应时间和温度和表面活性剂官能团变化来控制碲纳米线半径和长度。3. In the present invention, the radius and length of the tellurium nanowires can be controlled by adjusting the reaction time and temperature of each step and the change of the functional group of the surfactant.

4、本发明具有制备周期短,工艺简单可控,安全无污染耗能低,产物性能优良,适合实验室制备和工厂大规模生产等优点。4. The present invention has the advantages of short preparation cycle, simple and controllable process, safety, no pollution, low energy consumption, excellent product performance, and is suitable for laboratory preparation and large-scale production in factories.

5、本发明利用热分解法可调控制备了一种具有多种极化效应界面的碲纳米线/石墨烯/Mxene三维结构复合材料。5. In the present invention, a tellurium nanowire/graphene/Mxene three-dimensional structure composite material with multiple polarization effect interfaces can be regulated and prepared by using a thermal decomposition method.

6、本发明中碲纳米线在反应过程中可以直接加入其他复合材料,可以获得多种紧密结合的复合材料。6. In the present invention, the tellurium nanowires can be directly added to other composite materials during the reaction process, and various tightly combined composite materials can be obtained.

7、将三维结构材料应用在电磁波吸收领域,最佳含量在20%(80%的石蜡)时的反射率-26dB,获得很低含量条件下的高吸收值。7. The three-dimensional structure material is applied in the field of electromagnetic wave absorption. The reflectivity is -26dB when the optimum content is 20% (80% paraffin), and the high absorption value is obtained under the condition of very low content.

附图说明Description of drawings

图1为碲纳米线/石墨烯/Mxene复合材料XRD图谱。Figure 1 is the XRD spectrum of the tellurium nanowire/graphene/Mxene composite material.

图2为碲纳米线的透射电镜图。Figure 2 is a transmission electron microscope image of tellurium nanowires.

图3为碲纳米线/石墨烯/Mxene复合材料的透射电镜图。Figure 3 is a transmission electron microscope image of the tellurium nanowire/graphene/Mxene composite material.

图4为碲纳米线/石墨烯/Mxene复合材料的电磁波吸收图。Fig. 4 is the electromagnetic wave absorption diagram of the tellurium nanowire/graphene/Mxene composite material.

具体实施方式Detailed ways

下面结合附图和实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。The technical solution of the present invention will be further described below in conjunction with the accompanying drawings and embodiments, but it is not limited thereto. Any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should cover In the protection scope of the present invention.

实施例1:Example 1:

一种碲纳米线/石墨烯/Mxene复合材料的制作方法,所述方法具体是按以下步骤完成的:A kind of preparation method of tellurium nanowire/graphene/Mxene composite material, described method is specifically finished according to the following steps:

步骤一:将碲源与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅰ;Step 1: Mix the tellurium source and the volatile alcohol solvent in a certain ratio, heat and stir to obtain a solution I;

所述碲源为二氧化碲;所述可挥发醇类溶剂为乙二醇;所述碲源与可挥发醇类溶剂的质量比为1:2;所述加热方式为直接加热;所述加热器为可控电磁加热炉;所述搅拌为磁力搅拌;所述加热温度为30℃,时间为10min;所述搅拌器转速为100r/min;The tellurium source is tellurium dioxide; the volatile alcohol solvent is ethylene glycol; the mass ratio of the tellurium source to the volatile alcohol solvent is 1:2; the heating method is direct heating; the heating The device is a controllable electromagnetic heating furnace; the stirring is magnetic stirring; the heating temperature is 30°C, and the time is 10min; the speed of the stirrer is 100r/min;

步骤二:将表面活性剂与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅱ;Step 2: Mix the surfactant and the volatile alcohol solvent in a certain proportion, heat and stir evenly to obtain solution II;

所述表面活性剂为聚乙烯吡咯烷酮;所述可挥发醇类溶剂为乙二醇;所述表面活性剂和醇类溶剂的质量比为1:2;所述加热方式为直接加热;所述加热温度为40℃,时间为30min;所述搅拌器转速为100r/min;The surfactant is polyvinylpyrrolidone; the volatile alcohol solvent is ethylene glycol; the mass ratio of the surfactant to the alcohol solvent is 1:2; the heating method is direct heating; The temperature is 40°C, the time is 30min; the speed of the agitator is 100r/min;

步骤三:将碱性化合物与醇类溶剂以一定比例混合加热搅拌均匀获得溶液III。Step 3: Mix the basic compound and the alcohol solvent in a certain proportion, heat and stir to obtain a solution III evenly.

所述碱性化合物为氢氧化钾;所述醇类溶剂为乙二醇;所述搅拌为磁力搅拌;所述碱性化合物和醇类溶剂的质量比为1:2;所述加热方式为直接加热;所述加热温度为30℃;所述搅拌器转速为100r/min;所述加热搅拌时间为30min;The basic compound is potassium hydroxide; the alcohol solvent is ethylene glycol; the stirring is magnetic stirring; the mass ratio of the basic compound to the alcohol solvent is 1:2; the heating method is direct Heating; the heating temperature is 30°C; the stirrer speed is 100r/min; the heating and stirring time is 30min;

步骤四:将溶液Ⅰ、溶液Ⅱ、溶液Ⅲ置于三颈烧瓶加热并搅拌均匀得到混合溶液。Step 4: Put solution I, solution II, and solution III in a three-necked flask, heat and stir evenly to obtain a mixed solution.

所述加热方式为直接加热;所述搅拌为磁力搅拌;所述加热温度为20℃;所述搅拌器转速为100r/min;所述加热搅拌时间为20min;The heating method is direct heating; the stirring is magnetic stirring; the heating temperature is 20°C; the stirrer speed is 100r/min; the heating and stirring time is 20min;

步骤五:向混合溶液中通入惰性气体,于一定温度下加入还原剂并加热搅拌均匀得到前驱体,向前驱体中加入需要复合的材料、抗氧化剂后得到碲纳米线复合材料混合溶液。Step 5: Inject an inert gas into the mixed solution, add a reducing agent at a certain temperature, heat and stir evenly to obtain a precursor, add materials to be composited and an antioxidant to the precursor to obtain a mixed solution of tellurium nanowire composite material.

所述惰性气体为氩气;所述气体流速为1L/min;所述温度为50℃;所述还原剂为抗坏血酸;所述加热方式为直接加热;所述加热时间为20h;搅拌方式为磁力搅拌;所述搅拌器转速为100r/min;所述搅拌时间为2h;所述需要复合的材料为Mxene和石墨烯;所述抗氧化剂为抗坏血酸;The inert gas is argon; the gas flow rate is 1L/min; the temperature is 50°C; the reducing agent is ascorbic acid; the heating method is direct heating; the heating time is 20h; the stirring method is magnetic Stir; the stirrer speed is 100r/min; the stirring time is 2h; the material that needs to be composited is Mxene and graphene; the antioxidant is ascorbic acid;

步骤六:用一定体积比例的混合溶剂将最终产物进行水洗多次离心干燥得到碲纳米线复合材料固体。Step 6: The final product is washed with water for several times and centrifuged and dried with a mixed solvent in a certain volume ratio to obtain a solid tellurium nanowire composite material.

所述混合溶剂为乙醇和水的混合溶剂;所述混合溶剂的体积比为2:3;混合溶剂与碲纳米线复合材料混合溶液的体积比为1:3;水洗次数为6次;离心方式为高速离心机;离心速度为3500r/min;离心时间为3min;干燥温度为100℃;干燥时间为1h;所述碲纳米线/石墨烯/Mxene复合材料中的碲纳米线长度为16mm,直径为206nm;所述碲纳米线/石墨烯/Mxene复合材料的反射率为-26dB。The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:3; the volume ratio of the mixed solvent to the mixed solution of the tellurium nanowire composite material is 1:3; the number of washing times is 6; the centrifugal method It is a high-speed centrifuge; the centrifugal speed is 3500r/min; the centrifugal time is 3min; the drying temperature is 100°C; the drying time is 1h; is 206nm; the reflectance of the tellurium nanowire/graphene/Mxene composite material is -26dB.

通过XRD图谱(图1)可以看出,样品在2θ=23.544°,27.563°,38.261°,43.332°,51.941°,61.585°时的衍射峰分别对应Te晶体的(100),(101),(102),(111),(103),(211)结构晶面,这与标准PDF卡片PDF#36-1452的衍射峰位置一致,说明成功制备Te。在2θ=25.721°,28.263°,29.873°,48.163°,50.983°时的衍射峰分别对应C70晶体的(003),(101),(012),(211),(214)结构晶面,这与标准PDF卡片PDF#48-1449衍射峰的位置一致,与图2的SEM结果相呼应,说明成功包覆石墨烯。在2θ=27.858°,29.733°47.535°,57.168°,60.599°时的衍射峰分别对应C3N4晶体的(110),(200),(111),(220),(310)结构晶面,这与标准PDF卡片PDF#50-1512的衍射峰位置一致,说明成功制备Te/石墨烯/Mxene体系制备的Te化物纳米线。通过谢乐公式由Te的晶面(101)特征峰的半高宽可以计算出Te/石墨烯/Mxene体系制备的Te化物纳米线晶体径粒直径约为206nm。As can be seen from the XRD spectrum (Fig. 1), the diffraction peaks of the sample at 2θ=23.544°, 27.563°, 38.261°, 43.332°, 51.941°, and 61.585° correspond to (100), (101), ( 102), (111), (103), (211) structural crystal planes, which are consistent with the diffraction peak positions of the standard PDF card PDF#36-1452, indicating that Te was successfully prepared. The diffraction peaks at 2θ=25.721°, 28.263°, 29.873°, 48.163°, and 50.983° respectively correspond to (003), (101), (012), (211), (214) structural crystal planes of C 70 crystals, This is consistent with the position of the diffraction peak of the standard PDF card PDF#48-1449, which echoes the SEM results in Figure 2, indicating that graphene was successfully coated. Diffraction peaks at 2θ=27.858°, 29.733°47.535°, 57.168°, 60.599° respectively correspond to (110), (200), (111), (220), (310) crystal planes of C 3 N 4 crystals , which is consistent with the diffraction peak position of the standard PDF card PDF#50-1512, indicating the successful preparation of Te compound nanowires prepared by the Te/graphene/Mxene system. via the Scherrer formula The crystal diameter of the Te compound nanowires prepared by the Te/graphene/Mxene system can be calculated from the half maximum width of the Te crystal plane (101) characteristic peak to be about 206nm.

从图2可以明显看出线性结构,说明成功制备出了碲纳米线。The linear structure can be clearly seen from Figure 2, indicating that tellurium nanowires were successfully prepared.

从图3可以看出,碲纳米线分布在石墨烯和Mxene的表面或内部,尺寸分布在200nm~250nm,由于加入石墨烯和Mxene,制备的纳米线尺寸较小,复合材料中呈现多层结构。It can be seen from Figure 3 that the tellurium nanowires are distributed on the surface or inside of graphene and Mxene, and the size distribution is between 200nm and 250nm. Due to the addition of graphene and Mxene, the size of the prepared nanowires is small, and the composite material presents a multilayer structure .

图4为样品含量在20%(80%的石蜡)时的反射率数据。由图可知,不同厚度有不同频段的吸收最高值,在1-5.5mm厚度时均出现-10以下的反射率(90%以上的吸收率),并且在3mm厚度时的最佳反射率为-26dB。由此得知可以通过调节其厚度来改变吸收频段,表明碲纳米线在低含量的情况下可以达到很好的电磁波吸收效果。Figure 4 is the reflectance data when the sample content is 20% (80% paraffin). It can be seen from the figure that different thicknesses have the highest absorption values in different frequency bands, and the reflectivity below -10 (absorption rate above 90%) appears at a thickness of 1-5.5mm, and the best reflectivity at a thickness of 3mm is - 26dB. It is known that the absorption frequency band can be changed by adjusting its thickness, indicating that the tellurium nanowire can achieve a good electromagnetic wave absorption effect under the condition of low content.

实施例2:Example 2:

一种碲纳米线/硫酸铜/Mxene复合材料的制作方法,所述方法具体是按以下步骤完成的:A kind of preparation method of tellurium nanowire/copper sulfate/Mxene composite material, described method is specifically finished according to the following steps:

步骤一:将碲源与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅰ。Step 1: Mix the tellurium source and the volatile alcohol solvent in a certain ratio, heat and stir to obtain solution I evenly.

所述碲源为三氧化碲;所述可挥发醇类溶剂为乙醇;所述碲源与可挥发醇类溶剂的质量比为1:3;所述加热为磁力加热;所述加热器为加热棒;所述搅拌为机械搅拌;所述加热温度为40℃;所述搅拌器转速为200r/min;所述加热搅拌时间为20min;The tellurium source is tellurium trioxide; the volatile alcohol solvent is ethanol; the mass ratio of the tellurium source to the volatile alcohol solvent is 1:3; the heating is magnetic heating; rod; the stirring is mechanical stirring; the heating temperature is 40°C; the stirrer speed is 200r/min; the heating and stirring time is 20min;

步骤二:将表面活性剂与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅱ。Step 2: Mix the surfactant and the volatile alcohol solvent in a certain proportion, heat and stir evenly to obtain solution II.

所述表面活性剂为十六烷基溴化铵;所述可挥发醇类溶剂为乙醇;所述表面活性剂和醇类溶剂的质量比为1:3;所述加热为磁力加热;所述加热温度为50℃;所述搅拌器转速为200r/min;所述加热搅拌时间为40min;The surfactant is cetyl ammonium bromide; the volatile alcohol solvent is ethanol; the mass ratio of the surfactant to the alcohol solvent is 1:3; the heating is magnetic heating; The heating temperature is 50°C; the speed of the stirrer is 200r/min; the heating and stirring time is 40min;

步骤三:将碱性化合物与醇类溶剂以一定比例混合加热搅拌均匀获得溶液III。Step 3: Mix the basic compound and the alcohol solvent in a certain proportion, heat and stir to obtain a solution III evenly.

所述碱性化合物为氢氧化钠;所述醇类溶剂为乙醇;所述搅拌为机械搅拌;所述碱性化合物和醇类溶剂的质量比为1:3;所述加热为磁力加热;所述加热温度为40℃;所述搅拌器转速为200r/min;所述加热搅拌时间为30min;The basic compound is sodium hydroxide; the alcoholic solvent is ethanol; the stirring is mechanical stirring; the mass ratio of the basic compound to the alcoholic solvent is 1:3; the heating is magnetic heating; The heating temperature is 40°C; the stirrer speed is 200r/min; the heating and stirring time is 30min;

步骤四:将溶液Ⅰ、溶液Ⅱ、溶液Ⅲ置于三颈烧瓶加热并搅拌均匀得到混合溶液。Step 4: Put solution I, solution II, and solution III in a three-necked flask, heat and stir evenly to obtain a mixed solution.

所述加热为磁力加热;所述搅拌为机械搅拌;所述加热温度为30℃;所述搅拌器转速为200r/min;所述加热搅拌时间为40min;The heating is magnetic heating; the stirring is mechanical stirring; the heating temperature is 30°C; the stirrer speed is 200r/min; the heating and stirring time is 40min;

步骤五:向混合溶液中通入惰性气体,于一定温度下加入还原剂并加热搅拌均匀得到前驱体,向前驱体中加入需要复合的材料、抗氧化剂后得到碲纳米线复合材料混合溶液。Step 5: Inject an inert gas into the mixed solution, add a reducing agent at a certain temperature, heat and stir evenly to obtain a precursor, add materials to be composited and an antioxidant to the precursor to obtain a mixed solution of tellurium nanowire composite material.

所述惰性气体为氦气;所述气体流速为2L/min;所述温度为:60℃;所述还原剂为硼氢化钠;所述加热为磁力加热;所述加热时间为40h;搅拌方式为机械搅拌;所述搅拌器转速为200r/min;所述搅拌时间为3h;所述需要复合的材料为Mxene、硫酸铜;所述抗氧化剂为硼氢化钠;The inert gas is helium; the gas flow rate is 2L/min; the temperature is: 60°C; the reducing agent is sodium borohydride; the heating is magnetic heating; the heating time is 40h; For mechanical stirring; the stirrer rotating speed is 200r/min; the stirring time is 3h; the material that needs to be compounded is Mxene, copper sulfate; the antioxidant is sodium borohydride;

步骤六:用一定体积比例的混合溶剂将最终产物进行水洗多次离心干燥得到碲纳米线复合材料固体。Step 6: The final product is washed with water for several times and centrifuged and dried with a mixed solvent in a certain volume ratio to obtain a solid tellurium nanowire composite material.

所述混合溶剂为乙醇和水的混合溶剂;所述混合溶剂的体积比为2:3;混合溶剂与碲纳米线复合材料混合溶液的质量比为1:3;水洗次数为7次;离心方式为高速离心机;离心速度为4000r/min;离心时间为4min;干燥温度为150℃;干燥时间为2h;所述碲纳米线/硫酸铜/Mxene复合材料中的碲纳米线长度为18mm,直径为203nm;所述碲纳米线/硫酸铜/Mxene复合材料的反射率为-25dB。The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:3; the mass ratio of the mixed solvent to the mixed solution of the tellurium nanowire composite material is 1:3; the number of washing times is 7 times; the centrifugal method It is a high-speed centrifuge; the centrifugal speed is 4000r/min; the centrifugal time is 4min; the drying temperature is 150°C; the drying time is 2h; is 203nm; the reflectance of the tellurium nanowire/copper sulfate/Mxene composite material is -25dB.

实施例3:Example 3:

一种碲纳米线/硝酸镍/Mxene复合材料的制作方法,所述方法具体是按以下步骤完成的:A kind of preparation method of tellurium nanowire/nickel nitrate/Mxene composite material, described method is specifically finished according to the following steps:

步骤一:将碲源与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅰ。Step 1: Mix the tellurium source and the volatile alcohol solvent in a certain ratio, heat and stir to obtain solution I evenly.

所述碲源为亚碲酸钠;所述可挥发醇类溶剂为丙三醇;所述碲源与可挥发醇类溶剂的质量比为1:4;所述加热为直接加热;所述加热器为红外线加热器;所述搅拌为磁力搅拌;所述加热温度为50℃;所述搅拌器转速为400r/min;所述加热搅拌时间为40min;The tellurium source is sodium tellurite; the volatile alcohol solvent is glycerol; the mass ratio of the tellurium source to the volatile alcohol solvent is 1:4; the heating is direct heating; the heating The device is an infrared heater; the stirring is a magnetic stirring; the heating temperature is 50°C; the stirring speed is 400r/min; the heating and stirring time is 40min;

步骤二:将表面活性剂与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅱ。Step 2: Mix the surfactant and the volatile alcohol solvent in a certain proportion, heat and stir evenly to obtain solution II.

所述表面活性剂为油酸钠;所述可挥发醇类溶剂为丙三醇;所述表面活性剂和醇类溶剂的质量比为1:4;所述加热为直接加热;所述加热温度为60℃;所述搅拌器转速为400r/min;所述加热搅拌时间为40min;The surfactant is sodium oleate; the volatile alcohol solvent is glycerol; the mass ratio of the surfactant to the alcohol solvent is 1:4; the heating is direct heating; the heating temperature 60°C; the stirrer speed is 400r/min; the heating and stirring time is 40min;

步骤三:将碱性化合物与醇类溶剂以一定比例混合加热搅拌均匀获得溶液III。Step 3: Mix the basic compound and the alcohol solvent in a certain proportion, heat and stir to obtain a solution III evenly.

所述碱性化合物为三乙醇胺;所述醇类溶剂为丙三醇;所述搅拌为磁力搅拌;所述碱性化合物和醇类溶剂的质量比为1:4;所述加热为直接加热;所述加热温度为50℃;所述搅拌器转速为400r/min;所述加热搅拌时间为50min;The basic compound is triethanolamine; the alcohol solvent is glycerol; the stirring is magnetic stirring; the mass ratio of the basic compound to the alcohol solvent is 1:4; the heating is direct heating; The heating temperature is 50°C; the stirrer speed is 400r/min; the heating and stirring time is 50min;

步骤四:将溶液Ⅰ、溶液Ⅱ、溶液Ⅲ置于三颈烧瓶加热并搅拌均匀得到混合溶液。Step 4: Put solution I, solution II, and solution III in a three-necked flask, heat and stir evenly to obtain a mixed solution.

所述加热为直接加热;所述搅拌为磁力搅拌;所述加热温度为40℃;所述搅拌器转速为300r/min;所述加热搅拌时间为40min;The heating is direct heating; the stirring is magnetic stirring; the heating temperature is 40°C; the stirrer speed is 300r/min; the heating and stirring time is 40min;

步骤五:向混合溶液中通入惰性气体,于一定温度下加入还原剂并加热搅拌均匀得到前驱体,向前驱体中加入需要复合的材料、抗氧化剂后得到碲纳米线复合材料混合溶液。Step 5: Inject an inert gas into the mixed solution, add a reducing agent at a certain temperature, heat and stir evenly to obtain a precursor, add materials to be composited and an antioxidant to the precursor to obtain a mixed solution of tellurium nanowire composite material.

所述惰性气体为氮气;所述气体流速为3L/min;所述温度为70℃;所述还原剂为氯化亚锡;所述加热方式为直接加热;所述加热时间为4h;搅拌方式为磁力搅拌;所述搅拌器转速为400r/min;所述搅拌时间为4h;所述需要复合的材料为Mxene、硝酸镍;所述抗氧化剂为氯化亚锡;The inert gas is nitrogen; the gas flow rate is 3L/min; the temperature is 70°C; the reducing agent is stannous chloride; the heating method is direct heating; the heating time is 4h; For magnetic stirring; the stirrer rotating speed is 400r/min; the stirring time is 4h; the material that needs to be compounded is Mxene, nickel nitrate; the antioxidant is stannous chloride;

步骤六:用一定体积比例的混合溶剂将最终产物进行水洗多次离心干燥得到碲纳米线复合材料固体。Step 6: The final product is washed with water for several times and centrifuged and dried with a mixed solvent in a certain volume ratio to obtain a solid tellurium nanowire composite material.

所述混合溶剂为乙醇和水的混合溶剂;所述混合溶剂的体积比为2:5;混合溶剂与碲纳米线复合材料混合溶液的质量比为1:4;水洗次数为8次;离心方式为高速离心机;离心速度为4000r/min;离心时间为6min;干燥温度为100℃;干燥时间为1h;所述碲纳米线复合材料中的碲纳米线长度为20mm;所述碲纳米线/硝酸镍/Mxene复合材料中的碲纳米线直径为210nm;所述碲纳米线/硝酸镍/Mxene复合材料的反射率为-23dB。The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:5; the mass ratio of the mixed solvent to the mixed solution of the tellurium nanowire composite material is 1:4; the number of washing times is 8; It is a high-speed centrifuge; the centrifugal speed is 4000r/min; the centrifugation time is 6min; the drying temperature is 100°C; the drying time is 1h; the length of the tellurium nanowires in the tellurium nanowire composite material is 20mm; The diameter of the tellurium nanowires in the nickel nitrate/Mxene composite material is 210 nm; the reflectivity of the tellurium nanowires/nickel nitrate/Mxene composite material is -23dB.

实施例4:Example 4:

一种碲纳米线/石墨烯/硫酸锌复合材料的制作方法具体是按以下步骤完成的。A manufacturing method of a tellurium nanowire/graphene/zinc sulfate composite material is specifically completed according to the following steps.

步骤一:将碲源与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅰ。Step 1: Mix the tellurium source and the volatile alcohol solvent in a certain ratio, heat and stir to obtain solution I evenly.

所述碲源为二氧化碲;所述可挥发醇类溶剂为异丁醇;所述碲源与可挥发醇类溶剂的质量比为1:10;所述加热为磁力加热;所述加热器为可控电磁加热炉;所述搅拌为机械搅拌;所述加热温度为100℃;所述搅拌器转速为500r/min;所述加热搅拌时间为100min;The tellurium source is tellurium dioxide; the volatile alcohol solvent is isobutanol; the mass ratio of the tellurium source to the volatile alcohol solvent is 1:10; the heating is magnetic heating; the heater It is a controllable electromagnetic heating furnace; the stirring is mechanical stirring; the heating temperature is 100°C; the stirrer speed is 500r/min; the heating and stirring time is 100min;

步骤二:将表面活性剂与可挥发醇类溶剂以一定比例混合加热搅拌均匀获得溶液Ⅱ。Step 2: Mix the surfactant and the volatile alcohol solvent in a certain proportion, heat and stir evenly to obtain solution II.

所述表面活性剂为十二烷基苯磺酸钠;所述可挥发醇类溶剂为异丁醇;所述表面活性剂和醇类溶剂的质量比为1:8;所述加热为磁力加热;所述加热温度为90℃;所述搅拌器转速为600r/min;所述加热搅拌时间为80min;The surfactant is sodium dodecylbenzenesulfonate; the volatile alcohol solvent is isobutanol; the mass ratio of the surfactant to the alcohol solvent is 1:8; the heating is magnetic heating ; The heating temperature is 90°C; the stirrer speed is 600r/min; the heating and stirring time is 80min;

步骤三:将碱性化合物与醇类溶剂以一定比例混合加热搅拌均匀获得溶液III。Step 3: Mix the basic compound and the alcohol solvent in a certain proportion, heat and stir to obtain a solution III evenly.

所述碱性化合物为甲胺;所述醇类溶剂为甲醇;所述搅拌为机械搅拌;所述碱性化合物和醇类溶剂的质量比为1:8;所述加热为磁力加热;所述加热温度为90℃;所述搅拌器转速为500r/min;所述加热搅拌时间为90min;The basic compound is methylamine; the alcohol solvent is methanol; the stirring is mechanical stirring; the mass ratio of the basic compound to the alcohol solvent is 1:8; the heating is magnetic heating; The heating temperature is 90°C; the speed of the stirrer is 500r/min; the heating and stirring time is 90min;

步骤四:将溶液Ⅰ、溶液Ⅱ、溶液Ⅲ置于三颈烧瓶加热并搅拌均匀得到混合溶液。Step 4: Put solution I, solution II, and solution III in a three-necked flask, heat and stir evenly to obtain a mixed solution.

所述加热为磁力加热;所述搅拌为机械搅拌;所述加热温度为90℃;所述搅拌器转速为400r/min;所述加热搅拌时间为90min;The heating is magnetic heating; the stirring is mechanical stirring; the heating temperature is 90°C; the stirrer speed is 400r/min; the heating and stirring time is 90min;

步骤五:向混合溶液中通入惰性气体,于一定温度下加入还原剂并加热搅拌均匀得到前驱体,向前驱体中加入需要复合的材料、抗氧化剂后得到碲纳米线复合材料混合溶液。Step 5: Inject an inert gas into the mixed solution, add a reducing agent at a certain temperature, heat and stir evenly to obtain a precursor, add materials to be composited and an antioxidant to the precursor to obtain a mixed solution of tellurium nanowire composite material.

所述惰性气体为氩气;所述气体流速为5L/min;所述温度为100℃;所述还原剂为草酸;所述加热为磁力加热等;所述加热时间为5h;搅拌方式为机械搅拌;所述搅拌器转速为600r/min;所述搅拌时间为5h;所述需要复合的材料为石墨烯、硫酸锌;所述抗氧化剂为草酸;The inert gas is argon; the gas flow rate is 5L/min; the temperature is 100°C; the reducing agent is oxalic acid; the heating is magnetic heating, etc.; the heating time is 5h; the stirring method is mechanical Stir; the stirrer rotating speed is 600r/min; the stirring time is 5h; the material that needs to be composited is graphene, zinc sulfate; the antioxidant is oxalic acid;

步骤六:用一定体积比例的混合溶剂将最终产物进行水洗多次离心干燥得到碲纳米线复合材料固体。Step 6: The final product is washed with water for several times and centrifuged and dried with a mixed solvent in a certain volume ratio to obtain a solid tellurium nanowire composite material.

所述混合溶剂为乙醇和水的混合溶剂;所述混合溶剂的体积比为2:7;混合溶剂与碲纳米线复合材料混合溶液的质量比为1:5;水洗次数为9次;离心方式为高速离心机;离心速度为4000r/min;离心时间为6min;干燥温度为150℃;干燥时间为2h;所述碲纳米线/石墨烯/硫酸锌复合材料中的碲纳米线长度为18mm;所述碲纳米线/石墨烯/硫酸锌复合材料中的碲纳米线直径为200nm;所述碲纳米线/石墨烯/硫酸锌复合材料的反射率为-24dB。The mixed solvent is a mixed solvent of ethanol and water; the volume ratio of the mixed solvent is 2:7; the mass ratio of the mixed solvent to the mixed solution of the tellurium nanowire composite material is 1:5; the number of washing times is 9 times; the centrifugal method It is a high-speed centrifuge; the centrifugal speed is 4000r/min; the centrifugal time is 6min; the drying temperature is 150°C; the drying time is 2h; the length of the tellurium nanowires in the tellurium nanowire/graphene/zinc sulfate composite material is 18mm; The diameter of the tellurium nanowires in the tellurium nanowire/graphene/zinc sulfate composite material is 200 nm; the reflectivity of the tellurium nanowire/graphene/zinc sulfate composite material is -24dB.

Claims (7)

1. A preparation method of a tellurium nanowire multi-element composite material is characterized by comprising the following steps of: the method comprises the following steps:
step one: mixing a tellurium source with a volatilizable alcohol solvent, heating and stirring uniformly to obtain a solution I;
step two: mixing, heating and uniformly stirring a surfactant and a volatilizable alcohol solvent to obtain a solution II;
step three: mixing an alkaline compound with an alcohol solvent, heating and stirring uniformly to obtain a solution III;
step four: heating and uniformly stirring the solution I, the solution II and the solution III to obtain a mixed solution;
step five: introducing inert gas into the mixed solution, adding a reducing agent, heating and stirring uniformly to obtain a precursor, and adding a material to be compounded and an antioxidant into the precursor to obtain a tellurium nanowire composite material mixed solution;
step six: and (3) washing the final product with the mixed solvent for multiple times, and centrifugally drying to obtain the tellurium nanowire multi-element composite material.
2. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the first step, the tellurium source is one or more of tellurium dioxide, tellurium trioxide or sodium tellurite; the volatilizable alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the mass ratio of the tellurium source to the volatilizable alcohol solvent is 1:1 to 10; the heating is direct heating or magnetic heating, and the used heater is one of a controllable electromagnetic heating furnace, a heating rod or an infrared heater; the stirring is magnetic stirring or mechanical stirring, and the stirring rotating speed is 50-500 r/min; the heating temperature is 25-100 ℃; the heating and stirring time is 10 min-100 min.
3. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the second step, the surfactant is one or more of polyvinylpyrrolidone, cetyl ammonium bromide, sodium oleate, octadecylamine, sodium laurate, sodium stearate, sodium dodecyl sulfate or sodium dodecyl benzene sulfonate; the volatilizable alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the mass ratio of the surfactant to the alcohol solvent is 1:1 to 8; the heating is direct heating or magnetic heating; the heating temperature is 30-90 ℃; the rotating speed of the stirrer is 30 r/min-600 r/min; the heating and stirring time is 20-80 min.
4. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the third step, the alkaline compound is one or more of potassium hydroxide, sodium hydroxide, triethanolamine, methylamine, urea, ethylamine, ethanolamine, ethylenediamine, dimethylamine, trimethylamine, triethylamine, propylamine or isopropylamine; the alcohol solvent is one or more of glycol, ethanol, glycerol, isobutanol or methanol; the stirring is magnetic stirring or mechanical stirring; the mass ratio of the alkaline compound to the alcohol solvent is 1:1 to 8; the heating is direct heating or magnetic heating; the heating temperature is 20-90 ℃; the rotating speed of the stirrer is 30 r/min-500 r/min; the heating and stirring time is 20-90 min.
5. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the fourth step, the heating is direct heating or magnetic heating; the stirring is magnetic stirring or mechanical stirring; the heating temperature is 10-90 ℃; the rotating speed of the stirrer is 20 r/min-400 r/min; the heating and stirring time is 10 min-90 min.
6. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the fifth step, the inert gas is one or more of nitrogen and argon, and the gas flow rate is 0.1L/min-5L/min; the temperature is 40-200 ℃; the reducing agent is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride; the heating is direct heating or magnetic heating; the heating time is 1-60 h; the stirring is magnetic stirring or mechanical stirring, and the rotating speed is 50-800 r/min; the stirring time is 1-60 h; the material to be compounded is one or more of Mxene, graphene, copper sulfate, nickel nitrate or zinc sulfate; the antioxidant is one or more of ascorbic acid, sodium borohydride, stannous chloride, oxalic acid or potassium borohydride.
7. The method for preparing the tellurium nanowire multi-element composite material according to claim 1, wherein: in the sixth step, the mixed solvent is a mixed solution of ethanol and water, and the volume ratio of the ethanol to the water is 2:1 to 10; the volume ratio of the mixed solvent to the tellurium nanowire composite material mixed solution is 1:2 to 10; the washing times are 5-10 times; the centrifugal mode is a high-speed centrifugal machine; the speed of the centrifugation is 3000 r/min-5000 r/min, and the time is 2 min-20 min; the drying temperature is 100-200 ℃ and the drying time is 1-2 h.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103219066A (en) * 2012-01-19 2013-07-24 中国科学院上海硅酸盐研究所 Flexible conductive thin film compositing two-dimensional graphene and one-dimensional nanowire and preparation method thereof
CN103794265A (en) * 2014-02-26 2014-05-14 无锡格菲电子薄膜科技有限公司 Composite material of graphene and nanowires and preparation method thereof
CN110449169A (en) * 2019-07-04 2019-11-15 中山大学 A kind of semi-metallic Te nano wire/graphene hydrogel composite material and its preparation method and application
CN112680778A (en) * 2020-11-09 2021-04-20 青海大学 Preparation method of single crystal silver telluride nanotubes with uniform size
CN112954991A (en) * 2021-01-27 2021-06-11 武汉工程大学 MXene/metal nanowire composite material and freeze-thaw assembly method and application thereof
CN115807240A (en) * 2022-12-26 2023-03-17 青岛科技大学 A kind of preparation method of carbon-supported tellurium nanowire nanomaterial

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103219066A (en) * 2012-01-19 2013-07-24 中国科学院上海硅酸盐研究所 Flexible conductive thin film compositing two-dimensional graphene and one-dimensional nanowire and preparation method thereof
CN103794265A (en) * 2014-02-26 2014-05-14 无锡格菲电子薄膜科技有限公司 Composite material of graphene and nanowires and preparation method thereof
CN110449169A (en) * 2019-07-04 2019-11-15 中山大学 A kind of semi-metallic Te nano wire/graphene hydrogel composite material and its preparation method and application
CN112680778A (en) * 2020-11-09 2021-04-20 青海大学 Preparation method of single crystal silver telluride nanotubes with uniform size
CN112954991A (en) * 2021-01-27 2021-06-11 武汉工程大学 MXene/metal nanowire composite material and freeze-thaw assembly method and application thereof
CN115807240A (en) * 2022-12-26 2023-03-17 青岛科技大学 A kind of preparation method of carbon-supported tellurium nanowire nanomaterial

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