CN102219254A - Preparation method of zinc oxide nanorod - Google Patents

Preparation method of zinc oxide nanorod Download PDF

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Publication number
CN102219254A
CN102219254A CN2011101650041A CN201110165004A CN102219254A CN 102219254 A CN102219254 A CN 102219254A CN 2011101650041 A CN2011101650041 A CN 2011101650041A CN 201110165004 A CN201110165004 A CN 201110165004A CN 102219254 A CN102219254 A CN 102219254A
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zinc oxide
preparation
zinc
white precipitate
oxide nanorod
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孟彦超
周忠华
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Xiamen University
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Abstract

The invention provides a preparation method of a zinc oxide nanorod and relates to an inorganic nanomaterial. The preparation method comprises the following steps of: dissolving zinc salt into water; adding excessive aqueous alkali until white precipitate is completely dissolved; pouring the obtained solution into a polytetrafluoroethylene high-pressure kettle to perform hydrothermal reaction; filtering and washing; generating white precipitate; and drying to obtain zinc oxide nanorod. The prepared product is rod-like zinc oxide, wherein the diameter is about 150 nm and the average length is about 800 nm; the raw material cost is low; the process is simple and convenient to operate; high-temperature sintering is not required; yield is high; and the reaction condition is controllable. In addition, by the low-temperature preparation method, the process applicability of the nano zinc oxide in different fields can be enlarged.

Description

一种氧化锌纳米棒的制备方法A kind of preparation method of zinc oxide nanorod

技术领域technical field

本发明涉及一种无机纳米材料,尤其是涉及一种氧化锌纳米棒的制备方法。The invention relates to an inorganic nanometer material, in particular to a preparation method of zinc oxide nanorods.

背景技术Background technique

氧化锌(ZnO)作为一种多功能材料,具有很多优异的特性。随着近几年纳米材料的研究发展,颗粒尺寸的细微化,比表面积急剧增加,使得纳米ZnO具有表面效应,小尺寸效应和宏观量子隧道效应等。因而,纳米ZnO在磁、电、光、化学、物理学,敏感性方面具有一般ZnO所没有的特殊性能和新用途,可被广泛地应用于压电转换、透明电极、声波器件、压敏电阻、湿敏、气敏传感器、涂料,光催化剂,和太阳能电池等诸多领域,表现出广阔的应用前景。Zinc oxide (ZnO), as a multifunctional material, has many excellent properties. With the research and development of nanomaterials in recent years, the finer particle size and the sharp increase in specific surface area make nano-ZnO have surface effects, small size effects and macroscopic quantum tunneling effects. Therefore, nano-ZnO has special properties and new uses that general ZnO does not have in terms of magnetism, electricity, light, chemistry, physics, and sensitivity, and can be widely used in piezoelectric conversion, transparent electrodes, acoustic wave devices, and piezoresistors. , moisture sensitive, gas sensitive sensors, coatings, photocatalysts, and solar cells and many other fields, showing broad application prospects.

近年来,已有一些有关制备纳米氧化锌的相关专利申请,例如公开号为CN1657415A的中国专利申请,采用微波辐照,均相沉淀的方法,制备了纳米氧化锌,虽然该发明反应速率快,但是设备较复杂,并且使用表面改性剂,使成本增加。In recent years, there have been some relevant patent applications related to the preparation of nano-zinc oxide, such as the Chinese patent application with publication number CN1657415A, which uses microwave irradiation and homogeneous precipitation to prepare nano-zinc oxide. Although the reaction rate of this invention is fast, However, the equipment is more complicated, and the surface modifier is used, which increases the cost.

公开号为CN101172641A的中国专利申请,采用添加助燃剂,通过机械研磨前躯体,再在600~900℃下烧结,制得纳米氧化锌。该发明所得到的纳米粉粒度小,分布均匀,但是需要高温烧结。The Chinese patent application with the publication number CN101172641A adopts adding a combustion aid, mechanically grinding the precursor, and then sintering at 600-900° C. to prepare nano-zinc oxide. The nanometer powder obtained by the invention has small particle size and uniform distribution, but requires high-temperature sintering.

公开号为CN101016165的中国专利申请,采用甘油常压结晶法,制备了氧化锌纳米粉,但是过程较复杂,较难产业化。The Chinese patent application whose publication number is CN101016165 adopts glycerol atmospheric pressure crystallization method to prepare zinc oxide nanopowder, but the process is complicated and difficult to industrialize.

在现有的诸多制备方法中,主要存在工艺复杂、成本较高等缺点,因此寻求低成本,工艺简单的制备方法具有重要的现实意义。Among the many existing preparation methods, there are mainly disadvantages such as complex process and high cost. Therefore, it is of great practical significance to seek a low-cost and simple process preparation method.

发明内容Contents of the invention

本发明旨在提供一种氧化锌纳米棒的制备方法。The invention aims to provide a preparation method of zinc oxide nanorods.

本发明的具体步骤为:Concrete steps of the present invention are:

将锌盐溶解在水中,滴入过量的碱溶液,至白色沉淀完全溶解,将所得的溶液倒入聚四氟乙烯高压釜,进行水热反应后,过滤,洗涤,生成白色沉淀,烘干后,即得氧化锌纳米棒。Dissolve zinc salt in water, drop excess alkali solution until the white precipitate is completely dissolved, pour the resulting solution into a polytetrafluoroethylene autoclave, perform hydrothermal reaction, filter, wash to form a white precipitate, and dry it , to obtain ZnO nanorods.

所述锌盐可采用有机锌盐或无机锌盐;所述锌盐最好选自醋酸锌或硝酸锌等;所述锌盐的浓度可为0.1~0.2mol/L;所述碱可采用无机碱,所述无机碱可采用氢氧化钠等;所述无机碱的浓度可为0.5~2mol/L;所述水热反应的温度可为70℃,水热反应的时间可为24h。The zinc salt can be organic zinc salt or inorganic zinc salt; the zinc salt is preferably selected from zinc acetate or zinc nitrate; the concentration of the zinc salt can be 0.1~0.2mol/L; the alkali can be inorganic Alkali, the inorganic base can be sodium hydroxide or the like; the concentration of the inorganic base can be 0.5-2mol/L; the temperature of the hydrothermal reaction can be 70°C, and the time of the hydrothermal reaction can be 24h.

本发明所制备的产物为棒状氧化锌,直径大约150nm,平均长度大约800nm,本发明具有以下突出优点:原料成本低,工艺简单,操作方便,无需高温烧结,产率高,反应条件可控制。另外,低温制备法可以扩大纳米氧化锌在不同领域的工艺适用性。The product prepared by the invention is rod-shaped zinc oxide with a diameter of about 150nm and an average length of about 800nm. The invention has the following outstanding advantages: low raw material cost, simple process, convenient operation, no high temperature sintering, high yield and controllable reaction conditions. In addition, the low-temperature preparation method can expand the process applicability of nano-zinc oxide in different fields.

附图说明Description of drawings

图1是本发明样品的SEM照片。在图1中,标尺为1μm。Fig. 1 is the SEM photograph of the sample of the present invention. In Figure 1, the scale bar is 1 μm.

图2是本发明样品的能谱图。在图2中,横坐标为能量(KeV)。Fig. 2 is the energy spectrogram of the sample of the present invention. In FIG. 2, the abscissa is energy (KeV).

具体实施方式Detailed ways

实施例1Example 1

将2.97g的Zn(NO3)2·6H2O和4g的NaOH分别溶解在25mL蒸馏水中,然后将Zn(NO3)2溶液注入NaOH溶液中,溶液中出现大量的白色絮状沉淀,充分搅拌,白色絮状物溶解,将混合溶液转移到100mL聚四氟乙烯高压釜中,在70℃水热3h,过滤、洗涤生成的白色沉淀,烘干。2.97g of Zn(NO 3 ) 2 ·6H 2 O and 4g of NaOH were dissolved in 25mL of distilled water respectively, and then the Zn(NO 3 ) 2 solution was injected into the NaOH solution, a large amount of white flocculent precipitates appeared in the solution, fully Stir to dissolve the white floc, transfer the mixed solution to a 100mL polytetrafluoroethylene autoclave, heat it in water at 70°C for 3 hours, filter, wash the resulting white precipitate, and dry it.

实施例2Example 2

将2.97g的Zn(NO3)2·6H2O和4g的NaOH分别溶解在25mL蒸馏水中,然后将Zn(NO3)2溶液注入NaOH溶液中,溶液中出现大量的白色絮状沉淀,充分搅拌,白色絮状物溶解,将混合溶液转移到100mL聚四氟乙烯高压釜中,在70℃水热5h,过滤、洗涤生成的白色沉淀,烘干。Dissolve 2.97g of Zn(NO3)2·6H2O and 4g of NaOH in 25mL of distilled water respectively, then inject the Zn(NO3)2 solution into the NaOH solution, a large amount of white flocculent precipitates appear in the solution, stir well, the white flocculent The solids were dissolved, and the mixed solution was transferred to a 100mL polytetrafluoroethylene autoclave, heated in water at 70°C for 5h, filtered, washed, and the resulting white precipitate was dried.

实施例3Example 3

将2.97g的Zn(NO3)2·6H2O和4g的NaOH分别溶解在25mL蒸馏水中,然后将Zn(NO3)2溶液注入NaOH溶液中,溶液中出现大量的白色絮状沉淀,充分搅拌,白色絮状物溶解,将混合溶液转移到100mL聚四氟乙烯高压釜中,在70℃水热24h,过滤、洗涤生成的白色沉淀,烘干。Dissolve 2.97g of Zn(NO3)2·6H2O and 4g of NaOH in 25mL of distilled water respectively, then inject the Zn(NO3)2 solution into the NaOH solution, a large amount of white flocculent precipitates appear in the solution, stir well, the white flocculent The solids were dissolved, and the mixed solution was transferred to a 100mL polytetrafluoroethylene autoclave, heated in water at 70°C for 24 hours, filtered, washed, and the resulting white precipitate was dried.

实施例4Example 4

将2.2g的醋酸锌和4g的NaOH分别溶解在25mL蒸馏水中,然后将醋酸锌溶液注入NaOH溶液中,溶液中出现大量的白色絮状沉淀,充分搅拌,白色絮状物溶解,将混合溶液转移到100mL聚四氟乙烯高压釜中,在70℃水热24h,过滤、洗涤生成的白色沉淀,烘干。Dissolve 2.2g of zinc acetate and 4g of NaOH in 25mL of distilled water respectively, then inject the zinc acetate solution into the NaOH solution, a large amount of white flocculent precipitates appear in the solution, stir well, the white flocculent dissolves, transfer the mixed solution Put it into a 100mL polytetrafluoroethylene autoclave, heat it with water at 70°C for 24 hours, filter, wash the white precipitate formed, and dry it.

图1给出本发明实施例所制备的样品的SEM照片,图2给出相应的能谱图,在图2中,谱峰相应于Zn(锌)和O(氧)。Fig. 1 shows the SEM photo of the sample prepared by the embodiment of the present invention, and Fig. 2 provides the corresponding energy spectrum, and in Fig. 2, the spectral peaks correspond to Zn (zinc) and O (oxygen).

Claims (8)

1.一种氧化锌纳米棒的制备方法,其特征在于其具体步骤为:1. a preparation method of zinc oxide nanorods, characterized in that its concrete steps are: 将锌盐溶解在水中,滴入过量的碱溶液,至白色沉淀完全溶解,将所得的溶液倒入聚四氟乙烯高压釜,进行水热反应后,过滤,洗涤,生成白色沉淀,烘干后,即得氧化锌纳米棒。Dissolve zinc salt in water, drop excess alkali solution until the white precipitate is completely dissolved, pour the resulting solution into a polytetrafluoroethylene autoclave, perform hydrothermal reaction, filter, wash to form a white precipitate, and dry it , to obtain ZnO nanorods. 2.如权利要求1所述的一种氧化锌纳米棒的制备方法,其特征在于所述锌盐采用有机锌盐或无机锌盐。2. The preparation method of a kind of zinc oxide nanorod as claimed in claim 1, is characterized in that described zinc salt adopts organic zinc salt or inorganic zinc salt. 3.如权利要求1所述的一种氧化锌纳米棒的制备方法,其特征在于所述锌盐选自醋酸锌或硝酸锌。3. the preparation method of a kind of zinc oxide nanorod as claimed in claim 1 is characterized in that described zinc salt is selected from zinc acetate or zinc nitrate. 4.如权利要求1或2所述的一种氧化锌纳米棒的制备方法,其特征在于所述锌盐的浓度为0.1~0.2mol/L。4. A method for preparing zinc oxide nanorods according to claim 1 or 2, characterized in that the concentration of the zinc salt is 0.1-0.2 mol/L. 5.如权利要求1所述的一种氧化锌纳米棒的制备方法,其特征在于所述碱为无机碱。5. the preparation method of a kind of zinc oxide nanorod as claimed in claim 1 is characterized in that described alkali is inorganic alkali. 6.如权利要求5所述的一种氧化锌纳米棒的制备方法,其特征在于所述无机碱为氢氧化钠。6. the preparation method of a kind of zinc oxide nanorod as claimed in claim 5 is characterized in that described inorganic base is sodium hydroxide. 7.如权利要求1或5或6所述的一种氧化锌纳米棒的制备方法,其特征在于所述无机碱的浓度为0.5~2mol/L。7. A method for preparing zinc oxide nanorods according to claim 1, 5 or 6, characterized in that the concentration of the inorganic base is 0.5-2 mol/L. 8.如权利要求1所述的一种氧化锌纳米棒的制备方法,其特征在于所述水热反应的温度为70℃,水热反应的时间为24h。8 . The method for preparing zinc oxide nanorods according to claim 1 , wherein the temperature of the hydrothermal reaction is 70° C., and the time of the hydrothermal reaction is 24 hours.
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102730747A (en) * 2012-07-16 2012-10-17 河南师范大学 Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process
CN102897849A (en) * 2012-10-10 2013-01-30 华中科技大学 Method of preparing super-capacitor electrode material
CN103111313A (en) * 2013-02-22 2013-05-22 厦门大学 Preparation method of burred BiOI/ZnO microspheres
CN103408061A (en) * 2013-07-25 2013-11-27 南京航空航天大学 Preparation method for zinc oxide nanocrystalline
CN103771493A (en) * 2014-02-14 2014-05-07 常州大学 Method for preparing one-dimensional nano zinc oxide
CN104005070A (en) * 2014-05-04 2014-08-27 昆明理工大学 Preparation method of zinc aluminate nanopore array template
CN105837865A (en) * 2016-03-25 2016-08-10 同济大学 Chitosan/ZnO antibacterial preservative film, preparation method and application thereof
CN107983379A (en) * 2017-11-28 2018-05-04 沈阳师范大学 A kind of ZnO/CoP compound nanometer photocatalysts and preparation method thereof
CN109126759A (en) * 2018-08-17 2019-01-04 阿坝师范学院 ZnO visible light catalyst and its preparation method and application
CN109611419A (en) * 2018-12-11 2019-04-12 吉林大学 A metal-based underwater bionic gas film drag-reducing surface and its preparation method and application
CN110102312A (en) * 2019-05-14 2019-08-09 福州大学 A kind of one-dimensional cuprous oxide/silver/zinc oxide nanometer rods optic catalytic composite material and the preparation method and application thereof
CN110903582A (en) * 2019-11-27 2020-03-24 桂林理工大学 A kind of polyvinyl alcohol/starch nanocomposite material with ultraviolet blocking function and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005062785A2 (en) * 2003-12-17 2005-07-14 The University Of North Carolina At Chapel Hill Solution-phase synthesis of metal oxide nanostructures
CN1686820A (en) * 2005-04-06 2005-10-26 浙江大学 Method for repairing nano stick of zinc oxide in even diameter
CN1907861A (en) * 2006-07-31 2007-02-07 浙江理工大学 Process for preparing zinc oxide nano-stick
CN101182028A (en) * 2007-11-23 2008-05-21 陕西科技大学 A kind of preparation method of ZnO nano rod

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005062785A2 (en) * 2003-12-17 2005-07-14 The University Of North Carolina At Chapel Hill Solution-phase synthesis of metal oxide nanostructures
CN1686820A (en) * 2005-04-06 2005-10-26 浙江大学 Method for repairing nano stick of zinc oxide in even diameter
CN1907861A (en) * 2006-07-31 2007-02-07 浙江理工大学 Process for preparing zinc oxide nano-stick
CN101182028A (en) * 2007-11-23 2008-05-21 陕西科技大学 A kind of preparation method of ZnO nano rod

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
S. ERTEN-ELA ET AL.: "Morphological characterizations of ZnO nanostructures synthesized by hydrothermal method", 《OPTOELECTRONICS AND ADVANCED MATERIALS-RAPID COMMUNICATIONS》 *
李世帅等: "简单水热法制备棒状纳米氧化锌及其表征", 《功能材料》 *

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102730747B (en) * 2012-07-16 2014-03-26 河南师范大学 Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process
CN102730747A (en) * 2012-07-16 2012-10-17 河南师范大学 Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process
CN102897849A (en) * 2012-10-10 2013-01-30 华中科技大学 Method of preparing super-capacitor electrode material
CN103111313B (en) * 2013-02-22 2014-12-03 厦门大学 Preparation method of burred BiOI/ZnO microspheres
CN103111313A (en) * 2013-02-22 2013-05-22 厦门大学 Preparation method of burred BiOI/ZnO microspheres
CN103408061A (en) * 2013-07-25 2013-11-27 南京航空航天大学 Preparation method for zinc oxide nanocrystalline
CN103771493B (en) * 2014-02-14 2016-01-27 常州大学 A kind of method preparing one-D nano zinc oxide
CN103771493A (en) * 2014-02-14 2014-05-07 常州大学 Method for preparing one-dimensional nano zinc oxide
CN104005070A (en) * 2014-05-04 2014-08-27 昆明理工大学 Preparation method of zinc aluminate nanopore array template
CN105837865A (en) * 2016-03-25 2016-08-10 同济大学 Chitosan/ZnO antibacterial preservative film, preparation method and application thereof
CN107983379A (en) * 2017-11-28 2018-05-04 沈阳师范大学 A kind of ZnO/CoP compound nanometer photocatalysts and preparation method thereof
CN109126759A (en) * 2018-08-17 2019-01-04 阿坝师范学院 ZnO visible light catalyst and its preparation method and application
CN109611419A (en) * 2018-12-11 2019-04-12 吉林大学 A metal-based underwater bionic gas film drag-reducing surface and its preparation method and application
CN109611419B (en) * 2018-12-11 2021-04-02 吉林大学 A metal-based underwater bionic gas film drag-reducing surface and its preparation method and application
CN110102312A (en) * 2019-05-14 2019-08-09 福州大学 A kind of one-dimensional cuprous oxide/silver/zinc oxide nanometer rods optic catalytic composite material and the preparation method and application thereof
CN110903582A (en) * 2019-11-27 2020-03-24 桂林理工大学 A kind of polyvinyl alcohol/starch nanocomposite material with ultraviolet blocking function and preparation method thereof

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Application publication date: 20111019