CN115142075B - Preparation method of ZnO nanowire catalyst with controllable crystal face - Google Patents
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Abstract
The invention relates to a crystal faceA preparation method of a controllable ZnO nanowire catalyst belongs to the field of new energy nano materials and the technical field of catalysis. The method aims at solving the problems of low current density, poor product selectivity and the like in the electrocatalytic reduction process of carbon dioxide caused by poor intrinsic activity of the conventional Zn-based catalyst. The main scheme includes hydrothermal synthesis of zinc foil, ammonium persulfate and sodium hydroxide, in-situ growth of ZnO nanometer wire on zinc foil, high temperature pyrolysis in Ar atmosphere to obtain ZnO nanometer wire catalyst with different crystal face ratio, and the prepared Zn-based catalyst has relatively high catalytic activity and stability and may be used in electrocatalytic CO 2 Electrode material for reduction reaction.
Description
Technical Field
The invention relates to a preparation method of a ZnO nanowire catalyst with controllable crystal faces, and belongs to the field of new energy nano materials and the technical field of catalysis.
Background
Excessive dependence of people on fossil fuels leads to a large amount of greenhouse gases (mainly CO 2 ) The emission into the atmosphere poses serious threats to the ecological environment and human health. Thus, by introducing CO 2 Conversion to valuable chemical fuels to carbon neutral cycle, thereby reducing CO 2 Concentration is a current research hotspot. In various CO 2 In the utilization technology, CO is reduced by electrochemical catalysis 2 Is considered as one of the most promising solutions because it has the advantages of convenient operation, reusable electrolyte, low cost of renewable energy power generation, high feasibility, etc. But electrochemically reduce CO 2 Also present serious challenges in the process of (a), on the one hand, CO 2 The molecules themselves are very stable, so a large negative potential is required to trigger this reaction process, resulting in CO 2 It is almost impossible to convert into the desired chemical with high selectivity. On the other hand, hydrogen Evolution Reactions (HER) in aqueous electrolytes always occur within the same potential range. Hydrogen will appear as a by-product, resulting in a relatively low faraday efficiency of the carbon-based compound. Thus, the first and second substrates are bonded together,electrochemical reduction of CO 2 Whether or not it can be applied to actual production on a large scale depends on the development and design of the catalyst
In recent years, researchers have been around designing highly active and highly selective CO 2 RR catalysts have conducted a great deal of research effort. Wherein the noble metal catalyst is in CO 2 The RR reaction has better stability and high product selectivity, but the noble metal reserves are limited, and the price is high, so that the industrial large-scale use of the RR reaction is greatly limited. In the non-noble metal catalyst, the Zn-based material is in CO 2 The method has the advantages of good activity and selectivity on CO in the reduction reaction, rich content in the crust, low price, potential for large-scale application and the like, and is a research hotspot in recent years. However, the problems of high overpotential, low current density, further improvement of selectivity and the like limit the practical application of Zn-based materials. Based on the above consideration, we synthesize a ZnO nanowire catalyst with controllable crystal face by an autonomous invention pyrolysis strategy, and the prepared catalyst is characterized in that CO 2 Exhibits excellent electrocatalytic properties in the reduction test.
Disclosure of Invention
The invention aims to provide a method for preparing CO with high efficiency, which has simple process and low cost 2 The Zn-based catalyst with RR performance solves the problems of poor intrinsic activity, low product selectivity and the like of the existing Zn catalyst.
The invention adopts the following technical scheme for realizing the purposes:
a preparation method of a ZnO nanowire catalyst with controllable crystal faces comprises the following steps:
step 3, placing the zinc foil obtained in the step 3 into the solution A, and placing the solution A into a high-pressure reaction kettle for hydrothermal reaction;
step 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, drying in a vacuum drying oven, and annealing in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire;
and 5, annealing the zinc foil loaded ZnO nanowire obtained in the step 4 in Ar atmosphere, and regulating and controlling annealing conditions to obtain ZnO nanowire catalysts with different crystal face ratios.
The technical scheme is as follows: the mixed solution of ammonium persulfate and sodium hydroxide in step 1 must be stirred to a colorless transparent solution.
The technical scheme is as follows: in the step 3, the temperature of the hydrothermal reaction is 150 ℃ and the reaction time is 2 hours.
The technical scheme is as follows: in the step 4, the muffle furnace is set at 300 ℃, the annealing time is 2h, and the heating rate is 1 ℃/min.
By adopting the technical scheme, the invention has the following beneficial effects:
the invention has the advantage that the proportion of different crystal faces of ZnO can be effectively regulated and controlled by adopting a pyrolysis strategy on the basis of not damaging the structure of the ZnO nanowire. CO by different crystal planes 2 The intermediate has different binding effects in the reduction process, and the annealing condition is regulated and controlled, so that the activity and the selectivity of the catalyst can be regulated and controlled, and the problems of low activity and poor selectivity of the Zn-based catalyst at present are effectively solved. The preparation method is simple and easy to operate, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is an SEM image of ZnO nanowires obtained in example 1;
FIG. 2 is an SEM image of ZnO nanowires obtained in example 3;
FIG. 3 is a TEM image of the ZnO nanowires obtained in example 3;
FIG. 4 is an XRD pattern of ZnO nanowires obtained in examples 1 to 4;
fig. 5 is XPS spectra of ZnO nanowires obtained in example 1 and example 3;
FIG. 6 is a graph showing electrochemical test i-t of ZnO nanowires obtained in example 3
FIG. 7 is a plot of the selectivity for CO corresponding to the (a) total current density plot (b) for the catalysts obtained in examples 2, 3, and 4.
Fig. 8 is a plot of the total current density of the obtained samples from examples 5 and 6 and a corresponding selectivity histogram for CO.
FIG. 9 is CO of the ZnO nanowire obtained in example 3 2 Stability test chart of reduction reaction.
Detailed Description
The present invention will be described in further detail with reference to the embodiments and the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
The invention discloses a preparation method of a ZnO nanowire catalyst with controllable crystal faces, which comprises the steps of firstly adopting zinc foil, sodium hydroxide and ammonium persulfate to grow ZnO nanowires on the zinc foil in situ through hydrothermal synthesis, and then carrying out high-temperature pyrolysis in Ar atmosphere to obtain ZnO nanowire catalysts with different crystal face proportions, and is characterized by comprising the following steps:
and 3, placing the zinc foil obtained in the step 3 into the solution A, and placing the solution A into a high-pressure reaction kettle for hydrothermal reaction, wherein the temperature of the hydrothermal reaction is 150 ℃, and the reaction time is 2 hours.
And 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, then drying in a vacuum drying oven, and annealing in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire, wherein the muffle furnace is set at 300 ℃, the annealing time is 2h, and the heating rate is 1 ℃/min.
And 5, annealing the zinc foil loaded ZnO nanowire obtained in the step 4 in Ar atmosphere, regulating and controlling annealing conditions to obtain ZnO nanowire catalysts with different crystal face ratios, wherein the temperature of heat treatment in the step 5 is 300 ℃, the time range of heat treatment is 2h,6h and 10h respectively, and the heating rate is 1 ℃/min.
Example 1
A ZnO nanowire catalyst with controllable crystal faces adopts a hydrothermal method to prepare ZnO nanowires growing in situ on zinc foil, and comprises the following steps:
the preparation method comprises the following specific steps:
step 3, placing the zinc foil obtained in the step 3 into the solution A, placing the solution A into a high-pressure reaction kettle, and performing hydrothermal reaction at 150 ℃ for 2 hours;
step 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, then drying in a vacuum drying oven, and annealing for 2 hours at 300 ℃ in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire;
example 2
step 3, placing the zinc foil obtained in the step 3 into the solution A, placing the solution A into a high-pressure reaction kettle, and performing hydrothermal reaction at 150 ℃ for 2 hours;
step 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, then drying in a vacuum drying oven, and annealing for 2 hours at 300 ℃ in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire;
and 5, annealing the zinc foil loaded ZnO nanowire obtained in the step 4 for 2 hours at 300 ℃ in Ar atmosphere to obtain ZnO nanowire catalysts with different crystal face ratios, wherein the (002) crystal face ratio is reduced, and the (100) crystal face and (101) crystal face ratio is increased compared with the embodiment 1. (002, 100 and 101 are respectively the crystal plane indices of different crystal planes of ZnO, are the reciprocal ratios of the intercept coefficients of the crystal planes in 3 crystal axes)
Example 3
step 3, placing the zinc foil obtained in the step 3 into the solution A, placing the solution A into a high-pressure reaction kettle, and performing hydrothermal reaction at 150 ℃ for 2 hours;
step 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, then drying in a vacuum drying oven, and annealing for 2 hours at 300 ℃ in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire;
and 5, annealing the zinc foil loaded ZnO nanowire obtained in the step 4 at 300 ℃ for 6 hours in Ar atmosphere to obtain ZnO nanowire catalysts with different crystal face ratios, wherein the (002) crystal face ratio is reduced, and the (100) crystal face and (101) crystal face ratio is increased compared with the embodiment 1.
Example 4
step 3, placing the zinc foil obtained in the step 3 into the solution A, placing the solution A into a high-pressure reaction kettle, and performing hydrothermal reaction at 150 ℃ for 2 hours;
step 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, then drying in a vacuum drying oven, and annealing for 2 hours at 300 ℃ in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire;
and 5, annealing the zinc foil loaded ZnO nanowire obtained in the step 4 at 300 ℃ for 10 hours in Ar atmosphere to obtain ZnO nanowire catalysts with different crystal face ratios, wherein the (002) crystal face ratio is reduced, and the (100) crystal face and (101) crystal face ratio is increased compared with the embodiment 1.
Example 5
The procedure of example 5 was similar to that of example 3, except that the heat treatment temperature in step 5 was changed to 200 ℃.
Example 6
The procedure of example 6 was similar to that of example 3, except that the heat treatment temperature in step 5 was changed to 400 ℃.
Fig. 8 is a plot of the total current density of the obtained samples from examples 5 and 6 and a corresponding selectivity histogram for CO. KHCO with electrolyte of 0.5M 3 A solution. As can be seen from fig. 7, the catalyst current density obtained by the heat treatment at 200 ℃ was lower and the selectivity of the catalyst CO obtained by the heat treatment at 400 ℃ was worse than the sample obtained by the heat treatment at 300 ℃, indicating that the temperature of the heat treatment at 300 ℃ was optimal for the catalyst.
And carrying out morphology characterization on the obtained ZnO nanowire catalyst by adopting a scanning electron microscope.
FIG. 1 is an SEM image of the ZnO nanowire obtained in example 1, from which it can be seen that the ZnO nanowire uniformly grows on a Zn foil with a diameter of about 100 nm.
Fig. 2 is an SEM image of the ZnO nanowires obtained in example 3, and it can be seen from fig. 2 that the material still maintains a uniform nanowire structure after heat treatment.
FIG. 3 is a TEM image of the ZnO nanowire obtained in example 3, from which the nanowire structure can be seen, with a diameter of about 100 nm.
Fig. 4 is an XRD pattern of the ZnO nanowires obtained in examples 1 to 4, and it can be seen from fig. 4 that the (002) crystal face ratio gradually decreases and the (100) crystal face and (101) crystal face ratio gradually increases with an increase in pyrolysis time.
FIG. 5 is XPS spectra of ZnO nanowires obtained in example 1 and example 4, and pyrolysis 6 under Ar atmosphere can be seen from FIG. 5After h, zn 2+ Reduced valence state, zn 0 Increasing, oxygen vacancies increase.
FIG. 6 is a graph showing the electrochemical test i-t of the ZnO nanowire obtained in example 3, wherein constant potential electrolysis is performed in a potential range of-0.6V to-1.0V (vs. RHE), and it can be seen from the graph that the ZnO nanowire after pyrolysis has higher electrochemical activity, and the current density can reach 30mA/cm at-1.0V (vs. RHE) -2 。
Fig. 7 is a plot of the total current density for the catalysts obtained in examples 2, 3, 4 and the corresponding selectivity for CO for fig. 7 in example 1. Different crystal planes and CO 2 The binding energy of key intermediates COOH and CO in the reduction process is different, so that the crystal face proportion is regulated, the electrochemical catalytic activity can be optimized, and further performance tests find that: the CO selectivity of the ZnO nanowires obtained in example 3 was highest at-0.8 (vs. rhe). The faraday efficiency of CO can reach 92%.
Fig. 8 is a plot of the total current density of the obtained samples from examples 5 and 6 and a corresponding selectivity histogram for CO.
FIG. 9 shows KHCO at 0.1M for the ZnO nanowire catalyst obtained in example 3 3 Graph of the cycling stability test in solution. The results show that: the prepared ZnO nanowire catalyst can still maintain higher current density and Faraday efficiency after long-cycle stability test for 20 hours.
Claims (2)
1. A preparation method of a ZnO nanowire catalyst with controllable crystal faces is characterized by comprising the following steps: firstly, zinc foil, sodium hydroxide and ammonium persulfate are adopted to grow ZnO nanowires in situ on the zinc foil through hydrothermal synthesis, and then high-temperature pyrolysis is carried out in Ar atmosphere to obtain ZnO nanowire catalysts with different crystal face ratios, which is characterized by comprising the following steps:
step 1, 7.8-8.2g sodium hydroxide and 9.0-9.3g ammonium persulfate are dissolved in 100mL deionized water, stirred uniformly and marked as solution A;
step 2, taking a piece of zinc foil, repeatedly flushing with deionized water and absolute ethyl alcohol, and performing ultrasonic treatment to remove impurities on the surface of the zinc foil;
step 3, placing the zinc foil obtained in the step 2 into the solution A, and placing the solution A into a high-pressure reaction kettle for hydrothermal reaction, wherein the temperature of the hydrothermal reaction is 150 ℃ and the reaction time is 2 h;
step 4, taking out the zinc foil in the reaction kettle, repeatedly flushing with deionized water to remove the solution remained on the surface of the zinc foil, then drying in a vacuum drying oven, and annealing in a muffle furnace after drying to obtain the zinc foil loaded ZnO nanowire, wherein the muffle furnace is set at 300 ℃, the annealing time is 2h, and the heating rate is 1 ℃/min;
step 5, annealing the zinc foil loaded ZnO nanowire obtained in the step 4 in Ar atmosphere, regulating and controlling annealing conditions to obtain ZnO nanowire catalysts with different crystal face proportions, wherein the heat treatment temperature is 300 ℃, the heat treatment time ranges are 2 hours, 6 hours and 10 hours respectively, and the heating rate is 1 ℃/min;
the (002) crystal face proportion of the ZnO nanowire catalyst is reduced, and the (100) crystal face and (101) crystal face proportion are increased.
2. The method for preparing the crystal face controllable ZnO nanowire catalyst according to claim 1, wherein the method comprises the following steps: the mixed solution of ammonium persulfate and sodium hydroxide in step 1 must be stirred to a colorless transparent solution.
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| US8790614B2 (en) * | 2009-01-09 | 2014-07-29 | Colorado School Of Mines | ZnO structures and methods of use |
| CN102121130A (en) * | 2011-02-17 | 2011-07-13 | 东南大学 | ZnO nano slice/nano wire composite structure with photocatalysis characteristic and preparation method thereof |
| CN103922387B (en) * | 2014-03-28 | 2016-01-20 | 苏州科技学院 | A kind of magnetic nanometic zinc oxide line and preparation method thereof |
| JP2017075077A (en) * | 2015-10-16 | 2017-04-20 | Ｎｅｃトーキン株式会社 | Production method of zinc oxide film |
| CN106186040A (en) * | 2016-06-25 | 2016-12-07 | 延安大学 | A kind of hydro-thermal method prepares the method for transient metal doped ZnO nano-wire |
| CN109652820B (en) * | 2017-10-11 | 2021-03-05 | 中国科学院大连化学物理研究所 | CO (carbon monoxide)2Preparation of electrode for electrochemical reduction, electrode and application thereof |
| CN108249474A (en) * | 2018-03-13 | 2018-07-06 | 江苏巨珩新材料科技有限公司 | A kind of method for preparing three-dimensional zinc oxide nanoassemble structure |
| CN111569889A (en) * | 2020-06-22 | 2020-08-25 | 浙江倪阮新材料有限公司 | Nano zero-valent iron loaded ZnO doped Co3O4Process for preparing catalyst |
| CN113458408A (en) * | 2021-06-04 | 2021-10-01 | 河南师范大学 | Electrocatalysis with nano-wire structure and carbon dioxide reduction function and preparation method thereof |
| CN114032576B (en) * | 2021-11-05 | 2022-11-08 | 电子科技大学 | Preparation method of defect nanofiber carbon carrier coupled iron monatomic catalyst |
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