CN114031107A - A kind of zinc oxide with controllable morphology, preparation method and application thereof - Google Patents

A kind of zinc oxide with controllable morphology, preparation method and application thereof Download PDF

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CN114031107A
CN114031107A CN202111439865.4A CN202111439865A CN114031107A CN 114031107 A CN114031107 A CN 114031107A CN 202111439865 A CN202111439865 A CN 202111439865A CN 114031107 A CN114031107 A CN 114031107A
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zinc oxide
controllable
zinc
shape
minutes
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杨化桂
史迎利
毛芳欣
刘鹏飞
温春芳
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East China University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention relates to zinc oxide with controllable appearance, a preparation method and application thereof. Comprises the following steps: (1) dissolving a zinc source in deionized water, and stirring for 5-30 minutes to form a zinc source precursor solution; (2) adding urotropine into the zinc source precursor solution obtained in the step (1), and stirring for 5-30 minutes; (3) adding sodium hydroxide solution into the solution obtained in the step (2) to adjust the pH value of the solution; (4) and (4) placing the liquid obtained in the step (3) in a microwave reactor, cooling and centrifuging under normal pressure and under the conditions of ultrasonic power, upper limit of microwave power, temperature rise and heat preservation time to obtain a product, cleaning the product with methanol, and drying the product in an oven at the temperature of 50-80 ℃ to obtain the zinc oxide with the corresponding morphology. The zinc oxide synthesized by the method plays an important role in the fields of environment and energy, and can convert CO into CO2Efficient electrocatalytic reduction to CO and faradaic efficiency can exceed 90%.

Description

Shape-controllable zinc oxide, preparation method and application thereof
Technical Field
The invention relates to a preparation method of wurtzite zinc oxide material, wherein the size of the prepared material is 0.1-5.0 mu m. The surface appearance can be controllably adjusted by controlling corresponding parameters during synthesis. The material has very important function in the fields of environmental science and energy.
Background
The large consumption of traditional energy provides convenience for people, and has potential hidden dangers, such as excessive carbon dioxide (CO) discharged by the combustion of fossil energy2) Not only the global greenhouse effect is intensified, but also a series of problems such as ocean acidification are caused. Electrocatalytic CO2The reduction can not only reduce CO in the atmosphere2In a concentration such that CO can be converted2Conversion to other high value carbonaceous products such as chemicals or fuels, etc., and thus can also alleviate global demand for fossil fuels. Based on the above background, electrocatalysis of CO2The reduction technology is an effective way to solve the energy and environmental problems, so that the selective research of CO2The process of conversion to chemical feedstock is of great importance.
Noble metal based material albeit to CO2Has high reduction performance, but still has the factors of rare resources, high price and the like, so that the large-scale application cannot be realized. The zinc-based material is rich in resources, low in price and CO2The high reduction activity is a good source of the electrocatalyst. The invention provides a simple microwave-ultrasonic synthesis method, which can regulate and control the appearance structure of the generated zinc oxide by regulating corresponding parameters during synthesis, and the obtained zinc oxide can convert CO into CO2The high-efficiency reduction is carried out to CO, and the Faraday efficiency can reach more than 90%. And the current density can be as high as 300mA cm-2. This can effectively alleviate environmental problems such as greenhouse effect.
Disclosure of Invention
The invention aims to develop a preparation method of zinc oxide with low cost, simplicity, convenience, rapidness and controllable appearance.
The specific technical scheme of the invention is as follows: a preparation method of zinc oxide with controllable morphology comprises the following steps:
(1) dissolving a zinc source in deionized water, and stirring for 5-30 minutes to form a zinc source precursor solution;
(2) adding urotropine into the zinc source precursor solution obtained in the step (1), and stirring for 5-30 minutes;
(3) adding sodium hydroxide solution into the solution obtained in the step (2) to adjust the pH value of the solution;
(4) and (4) transferring the liquid obtained in the step (3) to a special-shaped three-neck flask, installing the special-shaped three-neck flask in a microwave reactor, cooling and centrifuging to obtain a product after certain ultrasonic power, microwave power upper limit, temperature rise and heat preservation time under normal pressure, cleaning the product for several times by using methanol, and drying the product in a drying oven at 50-80 ℃ to obtain the zinc oxide with the corresponding morphology.
Furthermore, the zinc source is zinc nitrate hexahydrate, and the using amount is 1-5 g.
Furthermore, the amount of the deionized water is 80-150 mL.
Further, the amount of the urotropin is 1-5 g.
Further, the pH value is 7-14.
Further, the concentration of the sodium hydroxide solution is 2-4 mol/L.
Furthermore, the ultrasonic power is 0-2000W.
Furthermore, the upper limit of the microwave power is 200-500W.
Further, the temperature is 80-100 ℃.
Further, the temperature rise time is 5-15 minutes.
Further, the heat preservation time is 5-45 minutes.
The invention also provides an application of the zinc oxide with controllable appearance, which is to apply the zinc oxide with controllable appearance to the technical field of environment and energy and can use CO2Efficient electrocatalytic reduction to CO, faradaic efficiency can exceed 90%.
According to the invention, by a microwave-ultrasonic synthesis method, corresponding parameters in the synthesis process, namely the pH value of the precursor and the ultrasonic power in the reaction process, are adjusted to regulate and control the appearance and structural characteristics of the obtained zinc oxide, so that the appearance structures of the micrometer flower, the spindle body, the polygonal pyramid and the like are synthesized. Compared with the prior art for preparing zinc oxide products, the invention has the following advantages: the cost is low, the synthesis method is simple and efficient, and the morphology can be regulated and controlled according to the regulation of experimental parameters.
Drawings
FIG. 1 is an X-ray diffraction pattern of zinc oxide prepared in examples 1 to 9;
FIG. 2 is a scanning electron micrograph of zinc oxide prepared according to examples 1 to 9;
FIG. 3 is a linear scanning voltammogram of the zinc oxide prepared in example 1;
FIG. 4 is CO of zinc oxide prepared in example 12Reduction performance diagram.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. It is to be noted that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as many insubstantial modifications and adaptations of the invention may be made by those skilled in the art based on the teachings herein.
Example 1
Step one, preparing zinc oxide with controllable appearance:
1.5g of zinc nitrate hexahydrate is dissolved in 100mL of deionized water and stirred for 5-10 minutes. And dissolving 1.4g of urotropin in the solution and stirring for 5-10 minutes. Thereafter, 3M NaOH was added dropwise thereto for adjusting the pH value to 13. Then the obtained liquid is transferred to a 250mL special-shaped three-neck flask, and the special-shaped three-neck flask is arranged in a microwave reactor, under the normal pressure, the ultrasonic power is set to be 0W, the upper limit of the microwave power is set to be 300W, the temperature is raised to 96 ℃ for 10 minutes, and the temperature is maintained for 20 minutes. Cooling, centrifuging to obtain a product, washing with methanol for 3 times, and drying in a vacuum oven at 60 deg.C to obtain zinc oxide with micrometer flower morphology.
Step two, electrocatalysis of CO2Application in the reduction field-Performance characterization test:
in electrocatalysis of CO2The reduction performance test is carried out in a flow reaction tank, a three-electrode system is used for the test, pretreated foamed nickel is used as a counter electrode, a saturated silver/silver chloride electrode is used as a reference electrode, and the obtained zinc oxide material is sprayed on a gas diffusion electrode to be used as workAnd an electrode. The electrolyte is a 1M KOH solution. The product obtained by catalysis of the prepared material was analyzed by gas chromatography. The electrochemical performance of all materials was tested by an electrochemical workstation (CHI 660). Introducing CO2The gas flow rate was set to 20mL/min into the cathode chamber and finally piped to a gas chromatograph (rami, GC2060) along with the product gas. The gas phase product was then analyzed by GC gas chromatography every 15 minutes.
FIG. 1 is an X-ray diffraction pattern of the zinc oxide prepared in examples 1 to 9, which shows that the samples synthesized by the method are zinc oxide with wurtzite structure. FIG. 2 is a scanning electron microscope image of the zinc oxide prepared in examples 1 to 9, which shows different morphologies such as micro-flowers, spindles, polygonal pyramids, etc., formed under different synthesis conditions, and the size of the zinc oxide is 0.3 to 2 um. FIG. 3 is a linear scanning voltammogram of the zinc oxide prepared in example 1, and the current density can be higher than 500mA cm at-2.5V-2Indicating the CO of this sample2The reduction activity is high. FIG. 4 is CO of the sample obtained in example 12The electroreduction performance diagram shows that the catalyst has high selectivity and high activity to CO, the Faraday efficiency can reach 90 percent, and the current density can reach 300mA cm-2。
Example 2
The procedure of step one of example 1 was repeated except that the ultrasonic power was 0W and the pH was adjusted to 10 to obtain spindle-shaped zinc oxide.
Example 3
The procedure of step one of example 1 was repeated except that the ultrasonic power was 0W and the pH was adjusted to 7.27 (i.e., no sodium hydroxide was added), to obtain zinc oxide in the form of micro-flowers composed of nanoneedles.
Example 4
The procedure of step one of example 1 was repeated except that the ultrasonic power was 500W and the pH was adjusted to 13, to obtain micrometer flower-like zinc oxide.
Example 5
The procedure of step one of example 1 was repeated except that the ultrasonic power was 500W and the pH was adjusted to 10 to obtain spindle-shaped zinc oxide.
Example 6
The procedure of step one of example 1 was repeated except that the ultrasonic power was 500W and the pH was adjusted to 7.27 (i.e., without adding sodium hydroxide), to obtain a polyprismatic zinc oxide.
Example 7
The procedure of step one of example 1 was repeated except that the ultrasonic power was 1500W and the pH was adjusted to 13 to obtain flaky zinc oxide.
Example 8
The procedure of step one of example 1 was repeated except that the ultrasonic power was 1500W and the pH was adjusted to 10 to obtain spindle-shaped zinc oxide.
Example 9
The procedure of step one of example 1 was repeated except that the ultrasonic power was 1500W and the pH was adjusted to 7.27 (i.e., without adding sodium hydroxide), to obtain a polyprismatic zinc oxide.

Claims (7)

1.一种形貌可控的氧化锌的制备方法，包含以下步骤：1. a preparation method of shape-controllable zinc oxide, comprises the following steps: (1)将锌源溶解于去离子水中，并搅拌5-30分钟，形成锌源前驱体溶液；(1) dissolve the zinc source in deionized water, and stir for 5-30 minutes to form a zinc source precursor solution; (2)向步骤(1)所得的锌源前驱体溶液中加入乌洛托品，并搅拌5-30分钟；(2) adding urotropine to the zinc source precursor solution obtained in step (1), and stirring for 5-30 minutes; (3)向步骤(2)所得溶液中加入氢氧化钠溶液调节其pH值；(3) in step (2) gained solution, add sodium hydroxide solution to adjust its pH value; (4)将步骤(3)所得液体置于微波反应器中，在常压下，在超声功率、微波功率上限、温度、升温及保温时间后，冷却，离心得到产物，并用甲醇清洗后，置于烘箱中50-80℃烘干，得到相应形貌的氧化锌。(4) placing the liquid obtained in step (3) in a microwave reactor, under normal pressure, after ultrasonic power, microwave power upper limit, temperature, temperature rise and holding time, cooling, centrifugation to obtain the product, and after washing with methanol, placing Dry in an oven at 50-80°C to obtain zinc oxide with corresponding morphology. 2.根据权利要求1所述的一种形貌可控的氧化锌的制备方法，其特征在于，步骤(1)中，所述锌源为六水合硝酸锌，用量为1～5g；所述去离子水的量为80～150mL。2. The preparation method of a shape-controllable zinc oxide according to claim 1, characterized in that, in step (1), the zinc source is zinc nitrate hexahydrate, and the amount is 1-5 g; the The amount of deionized water was 80-150 mL. 3.根据权利要求1所述的一种形貌可控的氧化锌的制备方法，其特征在于，步骤(2)中，所述乌洛托品的量为1～5g。3 . The method for preparing zinc oxide with controllable morphology according to claim 1 , wherein, in step (2), the amount of the urotropine is 1-5 g. 4 . 4.根据权利要求1所述的一种形貌可控的氧化锌的制备方法，其特征在于，步骤(3)中，所述pH值为7～14；所述氢氧化钠溶液浓度为2～4mol/L。4. The preparation method of a shape-controllable zinc oxide according to claim 1, characterized in that, in step (3), the pH value is 7 to 14; the concentration of the sodium hydroxide solution is 2 ~4mol/L. 5.根据权利要求1所述的一种形貌可控的氧化锌的制备方法，其特征在于，步骤(4)中，所述超声功率小于2000W；所述微波功率上限为200～500W；所述温度为80～100℃；所述升温时间为5～15分钟；所述保温时间为5～45分钟。5 . The method for preparing zinc oxide with controllable morphology according to claim 1 , wherein in step (4), the ultrasonic power is less than 2000W; the upper limit of the microwave power is 200-500W; The temperature is 80-100° C.; the heating time is 5-15 minutes; the holding time is 5-45 minutes. 6.根据权利要求1至5任一所述制备方法制得的形貌可控的氧化锌，其特征在于，所合成的氧化锌为纤锌矿结构，且其形貌可根据实验参数进行调控，尺寸大小为0.1～5.0μm。6. The shape-controllable zinc oxide obtained according to the preparation method described in any one of claims 1 to 5, is characterized in that, the synthesized zinc oxide has a wurtzite structure, and its shape can be regulated according to experimental parameters , the size is 0.1 ~ 5.0μm. 7.一种权利要求6所述形貌可控的氧化锌的应用，是将该形貌可控的氧化锌应用在环境和能源技术领域，可将CO2有效电催化还原为CO，法拉第效率可超过90％。7. An application of the shape-controllable zinc oxide according to claim 6 is to apply the shape-controllable zinc oxide in the field of environment and energy technology, and CO 2 can be effectively electrocatalytically reduced to CO, and the Faradaic efficiency can exceed 90%.
CN202111439865.4A 2021-11-30 2021-11-30 A kind of zinc oxide with controllable morphology, preparation method and application thereof Pending CN114031107A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115404497A (en) * 2022-10-07 2022-11-29 中国石油大学(华东) A new mass-producible preparation method and application of an amorphous zinc oxide-based electrocatalyst

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115404497A (en) * 2022-10-07 2022-11-29 中国石油大学(华东) A new mass-producible preparation method and application of an amorphous zinc oxide-based electrocatalyst
CN115404497B (en) * 2022-10-07 2023-10-20 中国石油大学(华东) Novel mass production preparation method and application of amorphous zinc oxide-based electrocatalyst

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Application publication date: 20220211