CN109485088A - A kind of flower shape zinc oxide nanometer sheet aggregate material and preparation method thereof, application - Google Patents
A kind of flower shape zinc oxide nanometer sheet aggregate material and preparation method thereof, application Download PDFInfo
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- CN109485088A CN109485088A CN201910019097.3A CN201910019097A CN109485088A CN 109485088 A CN109485088 A CN 109485088A CN 201910019097 A CN201910019097 A CN 201910019097A CN 109485088 A CN109485088 A CN 109485088A
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Abstract
The invention discloses a kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, include the following steps: for zinc salt to be added to the water and be hydrolyzed, obtains prefabricated material a；Prefabricated material a is poured into lye, in alkaline condition heating water bath, obtains prefabricated material b；Prefabricated material b is cooling, it stands still for crystals, washs, it is dry, obtain flower shape zinc oxide nanometer sheet aggregate material.The invention also discloses a kind of flower shape zinc oxide nanometer sheet aggregate materials；The invention also discloses a kind of application of flower shape zinc oxide nanometer sheet aggregate material in Electrochemical Detection concentration of heavy metal ion；Gained of the invention has bright and clean, big small-scale uniform flower-like nanometer chip architecture for the flower shape zinc oxide nanometer sheet of Electrochemical Detection heavy metal ion, it can be used as quick, the accurate detection of heavy metal ion in electrochemistry, realized to heavy metal ion High sensitivity, highly selective and glitch-free detection.
Description
Technical field
The present invention relates to Zinc oxide nano sheet technical field more particularly to a kind of flower shape zinc oxide nanometer sheet aggregate material and
Preparation method, application.
Background technique
It is well known that water resource is tellurian basic resource, it has the development of civilization of human society very heavy
The effect wanted.However, the pollution problem of Heavy Metals in Water Environment ion, which becomes increasingly conspicuous, has become global environmental problem, seriously
Endanger human health.Heavy metal ion, such as Pb, Cu, Hg, Cd, Cr, Zn and As are extremely toxic substances, it is very difficult to be given birth to
Object degradation, but can under the biomagnification of the food chain thousands of hundred times ground enrichment, finally enter human body give rise to diseases and
Biological function disorder.Industrial wastewater containing heavy metal ion is discharged into river, in lake, and heavy metal usually exists after entering water body
Absorption, complexing, precipitating etc. chemokines effect under be enriched in deposit, and easily when environmental condition changes settling flux and
Dissolution forms secondary pollution, generates persistent influence, constitutes to the life security of the plant in biosphere, animal and the mankind
Greatly threaten.It would therefore be desirable to which one kind can be quick, there is highly sensitive simple detection means.
Some traditional analysis methods are widely used for the detection of heavy metal ion in aqueous solution, including atomic absorption light
It composes (AAS), inductive coupling plasma mass spectrometry (ICP-MS), X-ray fluorescence spectra (XRF), instrumental neutron activation analysis (INAA),
Raman spectrum (SERS) and surface plasma resonance spectrum (SPR) analysis etc..And these traditional detection methods need mostly
Expensive, heavy, complicated instrument, operating cost are higher；Preparation of samples process is more complicated, and multi-step is needed to handle, and time-consuming
Low efficiency limits the application in batch samples context of detection.Electrochemical method excellent properties as possessed by itself
The features such as (sensitive, efficient, easy to operate, low in cost, easy to carry, expense is low and sample is easy to handle) and be widely used in
The analysis detection of heavy metal ion, and be most hopeful to realize to the method for Heavy Metals In Environment field monitoring and screening it
One.Wherein, anodic stripping voltammetry (SWASV) sensitivity is very high and most widely used.
With the development of nanosecond science and technology, nano structural material is applied to point of heavy metal contaminants by a lot of research work
Analysis as electrode material increasingly by the concern of researcher, and constantly promotes electrochemical analysis method in detection weight
Application in terms of contaminant metal ions.Research shows that nano structural material modified electrode can be significantly improved to heavy metal pollution
The Electrochemical Detection performance of object, for example improve sensitivity and selectivity, reduce detection limit etc..Therefore, nano electrochemical analysis side
Method is expected to realize effective analysis to heavy metal contaminants in water body environment.Common used electrode material includes noble metal
Nano particle (Au, Ag, Pt), carbon material (carbon nanotube, graphene, carbon ball), metal oxide and organic biomolecules etc., this
The electrode of a little material modifications achieves many achievements in terms of detection of heavy metal ion.However, finding nano electrochemical through investigation
There is also some urgent problems to be solved for analysis method, as detection sensitivity and selectivity be not high；Monitoring lower-cut is not low enough；It coexists
Serious interference between heavy metal ion, it is not easy to realize and the highly selective of certain ion, high accuracy are detected；In complex system
Also it is easy the interference by other ions coexisted when middle detection, is unfavorable for the practical popularization and application of constructed electrode.For example,
M.O.Park,H.B.Noh,D.S.Park,J.H.Yoon,Y.B.Shim,Long-life heavy metal ions sensor
based on graphene oxide-anchored conducting polymer,Electroanalysis 29(2017)
514-520. has constructed a kind of novel sensor that can be used for a long time, the electricity by dressing agent of graphene oxide/conducting polymer
It is great to have good chemical property, Zn (II), Pb (II), Cd (II), Cu (II) and Hg (II) can be carried out while being detected,
But its sensitivity is not high, and can not achieve the highly selective detection to certain specific heavy metal ion；S.Q.Xiong,
B.Y.Yang,D.Q.Cai,G.N.Qiu,Z.Y.Wu,Individual and simultaneous stripping
voltammetric and mutual interference analysis of Cd2+,Pb2+and Hg2+ with reduced
graphene oxide-Fe3O4The green slope thread of nanocomposites, Electrochim.Acta 185 (2015) 52-61.
Stone/ionic liquid composite material carrys out modified electrode, and has studied modified electrode in individually detection Pb (II), Cd (II), Cu (II)
Chemical property when being detected simultaneously with Hg (II), the results showed that while the sensitivity of Pb (II) will be far below individually detection when detecting
Sensitivity when Pb (II)；J.Mettakoonpitak,J.Mehaffy,J.Volckens,C.S.Henry,AgNP/Bi/
Nafion-modified disposable electrodes for sensitive Zn(II),Cd(II),and Pb(II)
29 (2017) 880-889. of detection in aerosol samples, Electroanalysis using Ag nano particle/
The electrode of Bi modification obtains preferable sensitivity and detection limit to detect Zn (II), Pb (II), Cd (II), but is being interfered
In the research of experiment find Cu (II) presence in system Pb (II) and Cd (II) detect cause apparent interference, it is right
The interference of Zn (II) is relatively small.Therefore, in order to obtain accurately and reliably testing result, we should continue to be dedicated to design newly
Sensitive interface, novel electrochemical sensor is constructed, to realize to heavy metal ion High sensitivity, highly selective and glitch-free
Detection.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of flower shape zinc oxide nanometer sheet aggregate material and
Preparation method, application, preparation is simple by the present invention, and experiment condition is mild, both goes back in the whole process without addition
Former agent, also without using activating agent；And uniform laminated structure is presented in gained Nano silver piece aggregation in a big way, can incite somebody to action
Its quick, accurate detection for being used as heavy metal ion in electrochemistry is realized to heavy metal ion High sensitivity, highly selective and nothing
The detection of interference.
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material proposed by the present invention, includes the following steps:
S1, it zinc salt is added to the water is hydrolyzed, obtain prefabricated material a；
S2, prefabricated material a is poured into lye, in alkaline condition heating water bath, obtains prefabricated material b；
S3, prefabricated material b is cooled down, is stood still for crystals, washed, it is dry, obtain flower shape zinc oxide nanometer sheet aggregate material.
Preferably, in S1, the zinc salt is zinc acetate, zinc nitrate hexahydrate, six zinc sulphate hydrates, hypochlorous acid zinc, silicon
At least one of sour zinc, zinc sulphide.
Preferably, in S1, the zinc salt is zinc acetate；It is further preferred that acetic acid zinc concentration is 1-5mmol/L.
Preferably, in S2, the lye is at least one of sodium hydroxide solution, thiourea solution, potassium hydroxide solution.
Preferably, in S2, the lye is sodium hydroxide solution；It is further preferred that the concentration of sodium hydroxide is 15-
30mmol/L。
Preferably, in S1, the water is ultrapure water, it is preferable that the volume ratio of ultrapure water and zinc salt is 20-40:1, into one
Preferably, ultrapure water resistivity is 18.25M to step.
Preferably, in S2, the heating water bath time is 1-12h, it is preferable that water bath heating temperature≤100 DEG C.
The invention also provides a kind of flower shape zinc oxide nanometer sheet aggregate materials, poly- using the flower shape zinc oxide nanometer sheet
The preparation method for collecting material is made.
The invention also provides a kind of flower shape zinc oxide nanometer sheet aggregate materials in Electrochemical Detection concentration of heavy metal ion
In application.
Preferably, the heavy metal ion includes Zn (II), Pb (II), Cd (II), Cu (II) and Hg (II).
In the present invention, zinc salt is hydrolyzed into zinc source and weak acid radical ion in water, weak acid radical ion is consumed in lye, then
It is coupled in the remaining hydroxide ion of atmosphere of alkalinity and zinc source, forms a zinc and couple four states hydroxy, by adding
Pyrohydrolysis forms ZnO, and due to the power of alkaline atmosphere, coupling effect difference is polymerized together in hydrolytic process, is just with zinc core
Center carries out oriented crystal growth, to obtain Zinc oxide nano sheet aggregation；Gained Nano silver piece aggregation is by multiple needles
The small pieces of shape form, and the edge of nanometer sheet is more smooth, are conducive to the specific surface area for improving particle surface, so that Zinc oxide nano sheet
Corner angle have very strong redox property, and its intersect to form nano gap and hole be greatly improved electrochemistry inspection
The sensitivity of survey.
Preparation is simple by the present invention, and experiment condition is mild, is entirely preparing Zinc oxide nano sheet aggregate material mistake
Both without addition reducing agent in journey, also without using activating agent；And gained Nano silver piece aggregation is presented in a big way
One laminated structure not only guarantees its sensitivity as Electrochemical Detection, but also has reliable reproducibility, the detection to Hg
5ppb can be reached.
Detailed description of the invention
Fig. 1 is the scanning electron microscopy of 1 gained flower shape zinc oxide nanometer aggregate material different resolution of comparative example of the present invention
Mirror (SEM) picture.
Fig. 2 is the scanning electron microscopy of 7 gained flower shape zinc oxide nanometer aggregate material different resolution of the embodiment of the present invention
Mirror (SEM) picture.
Fig. 3 is the scanning electron microscopy of 8 gained flower shape zinc oxide nanometer aggregate material different resolution of the embodiment of the present invention
Mirror (SEM) picture.
Fig. 4 is 8 gained flower shape zinc oxide nanometer aggregate material of the embodiment of the present invention for detecting various concentration Hg in water
Feedback current peak figure piece.
Fig. 5 is the scanning electron microscopy of 9 gained flower shape zinc oxide nanometer aggregate material different resolution of the embodiment of the present invention
Mirror (SEM) picture.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, it zinc salt is added to the water is hydrolyzed, obtain prefabricated material a；
S2, prefabricated material a is poured into lye, in alkaline condition heating water bath, obtains prefabricated material b；
S3, prefabricated material b is cooled down, is stood still for crystals, washed, it is dry, obtain flower shape zinc oxide nanometer sheet aggregate material.
Embodiment 2
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, it is hydrolyzed with acetic acid zinc solution addition ultrapure water, obtains prefabricated material a；
S2, prefabricated material a is poured into lye, the heating water bath 12h in the atmosphere of alkalinity, water bath heating temperature is 100 DEG C；
S3, it is cooled to room temperature, stood still for crystals completely, take out washing, it is dry, obtain flower shape zinc oxide nanometer sheet aggregation material
Material.
Embodiment 3
A kind of preparation method for flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 20ml is added in the hypochlorous acid zinc solution that 1ml concentration is 5mmol/L is carried out with magnetic stirrer stirring
Hydrolysis, obtains prefabricated material a；
S2, by the zinc acetate sufficiently dissolved it is molten be poured slowly into concentration be 30mmol/L thiourea solution in, alkalinity atmosphere
Middle heating water bath, 100 DEG C of bath temperature, water bath time 1h；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Embodiment 4
A kind of preparation method for flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 40ml is added in the zinc solution that 1ml concentration is 1mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；Wherein, ultrapure water resistivity is 18.25M；
Zinc solution is by acetic acid zinc solution, zinc nitrate hexahydrate solution and six zinc sulphate hydrate solution compositions；
S2, by the zinc acetate sufficiently dissolved it is molten pour into concentration be 15mmol/L potassium hydroxide solution in, alkalinity atmosphere
Middle heating water bath, 50 DEG C of bath temperature, water bath time 12h；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Embodiment 5
A kind of preparation method for flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 38ml is added in the acetic acid zinc solution that 1ml concentration is 2mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；Wherein, ultrapure water resistivity is 18.25M；
S2, prefabricated material a is poured into concentration be 21mmol/L lye in, alkalinity atmosphere in heating water bath, bath temperature
80 DEG C, water bath time 6h；
The lye includes sodium hydroxide solution, thiourea solution, potassium hydroxide solution；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Embodiment 6
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 30ml is added in the acetic acid zinc solution that 1ml concentration is 2mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；
S32, by prefabricated material a be poured slowly into concentration be 10mmol/L sodium hydroxide solution in, alkalinity atmosphere in water
Bath heating, bath temperature are 60 DEG C；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Embodiment 7
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 30ml is added in the acetic acid zinc solution that 1ml concentration is 1mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；
S2, prefabricated material a is poured into the sodium hydroxide solution that concentration is 20mmol/L, water-bath adds in the atmosphere of alkalinity
Heat, bath temperature are 80 DEG C, water bath time 4h；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Different resolution scanning electron microscope (SEM) figure of flower shape zinc oxide nanometer sheet aggregate material obtained by the present embodiment
As shown in Fig. 2, being apparent that the flower shape zinc oxide nanometer sheet aggregation that Macroscale homogenous is presented from Fig. 2.
Embodiment 8
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 30ml is added in the acetic acid zinc solution that 1ml concentration is 1mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；
S2, prefabricated material a is poured into the sodium hydroxide solution that concentration is 20mmol/L, water-bath adds in the atmosphere of alkalinity
Heat, bath temperature are 90 DEG C, water bath time 4h；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material nanometer sheet.
Different resolution scanning electron microscope (SEM) figure of flower shape zinc oxide nanometer sheet aggregate material obtained by the present embodiment
As shown in figure 3, as can be seen from Figure 3 well-proportioned laminated structure is still presented in Zinc oxide nano sheet in a big way.
Flower shape zinc oxide nanometer sheet aggregate material obtained by the present embodiment is used as heavy metal in Electrochemical Detection water；
I, the AC/ACNa buffer for the PH=5 for taking the Hg ion of 3 kinds of various concentrations to optimize before being added drop-wise to respectively respectively
In, under the best experimental conditions, Hg is detected using electrochemical workstation, as shown in figure 4, Fig. 4 is various concentration
The feedback current peak that Hg occurs under the detection of the material.As can be seen from Figure 4: the characteristic peak of Hg can be identified clearly and by force
Degree increases with the increase of concentration.
Embodiment 9
A kind of preparation method for flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 30ml is added in the acetic acid zinc solution that 1ml concentration is 1mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；
S2, by the zinc acetate sufficiently dissolved it is molten pour into concentration be 30mmol/L sodium hydroxide solution in, alkalinity atmosphere
Middle heating water bath, bath temperature are 100 DEG C, water bath time 4h；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Different resolution scanning electron microscope (SEM) figure of flower shape zinc oxide nanometer sheet aggregate material obtained by the present embodiment
As shown in figure 5, as can be seen from Figure 5 well-proportioned laminated structure is still presented in Zinc oxide nano sheet in a big way.
Comparative example 1
A kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, includes the following steps:
S1, the ultrapure water that 30ml is added in the acetic acid zinc solution that 1ml concentration is 1mmol/L is subjected to water with magnetic stirrer stirring
Solution, obtains prefabricated material a；
S2, prefabricated material a is poured slowly into the sodium hydroxide solution for being 10mmol/L to concentration, the water in the atmosphere of alkalinity
Bath heating, water bath heating temperature are 70 DEG C, water bath time 4h；
S3, it is cooled to room temperature, stands 12 hours and its crystallization is allowed to take out washing drying completely, obtain flower shape zinc oxide nanometer
Piece aggregate material.
Different resolution scanning electron microscope (SEM) figure of flower shape zinc oxide nanometer sheet aggregate material obtained by the present embodiment
As shown in Figure 1, being apparent that the non-flower-shaped aggregation of Zinc oxide nano sheet that Macroscale homogenous is presented from Fig. 1.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.The above, it is only of the invention
Preferable specific embodiment, but scope of protection of the present invention is not limited thereto, any technology people for being familiar with the art
Member in the technical scope disclosed by the present invention, is subject to equivalent replacement according to the technical scheme of the invention and its inventive conception or changes
Become, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of flower shape zinc oxide nanometer sheet aggregate material, which comprises the steps of:
S1, it zinc salt is added to the water is hydrolyzed, obtain prefabricated material a；
S2, prefabricated material a is poured into lye, in alkaline condition heating water bath, obtains prefabricated material b；
S3, prefabricated material b is cooled down, is stood still for crystals, washed, it is dry, obtain flower shape zinc oxide nanometer sheet aggregate material.
2. the preparation method of flower shape zinc oxide nanometer sheet aggregate material according to claim 1, which is characterized in that in S1
In, the zinc salt be zinc acetate, zinc nitrate hexahydrate, six zinc sulphate hydrates, hypochlorous acid zinc, zinc silicate, zinc sulphide at least one
Kind.
3. the preparation method of flower shape zinc oxide nanometer sheet aggregate material according to claim 2, which is characterized in that in S1
In, the zinc salt is zinc acetate；It is further preferred that acetic acid zinc concentration is 1-5mmol/L.
4. the preparation method of flower shape zinc oxide nanometer sheet aggregate material according to claim 1, which is characterized in that in S2
In, the lye is at least one of sodium hydroxide solution, thiourea solution, potassium hydroxide solution.
5. the preparation method of flower shape zinc oxide nanometer sheet aggregate material according to claim 4, which is characterized in that in S2
In, the lye is sodium hydroxide solution；It is further preferred that the concentration of sodium hydroxide is 15-30mmol/L.
6. the preparation method of flower shape zinc oxide nanometer sheet aggregate material according to claim 1, which is characterized in that in S1,
The water is ultrapure water, it is preferable that the volume ratio of ultrapure water and zinc salt is 20-40:1, it is further preferred that ultrapure water resistivity
For 18.25M.
7. the preparation method of flower shape zinc oxide nanometer sheet aggregate material according to claim 1, which is characterized in that in S2,
The heating water bath time is 1-12h, it is preferable that water bath heating temperature≤100 DEG C.
8. a kind of flower shape zinc oxide nanometer sheet aggregate material, which is characterized in that described in any item flower-shaped using claim 1-7
The preparation method of Zinc oxide nano sheet aggregate material is made.
9. a kind of flower shape zinc oxide nanometer sheet aggregate material as claimed in claim 8 is in Electrochemical Detection concentration of heavy metal ion
In application.
10. flower shape zinc oxide nanometer sheet aggregate material according to claim 9 is in Electrochemical Detection concentration of heavy metal ion
In application, which is characterized in that the heavy metal ion includes Zn (II), Pb (II), Cd (II), Cu (II) and Hg (II).
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| CN110526228A (en) * | 2019-09-12 | 2019-12-03 | 北京工业大学 | The preparation method of one type petal-shaped carbon nanosheet |
| CN110526228B (en) * | 2019-09-12 | 2021-03-30 | 北京工业大学 | Preparation method of petal-like carbon nanosheets |
| CN116177590A (en) * | 2023-03-23 | 2023-05-30 | 河南科技大学 | Preparation method of ZnO micro-nano structural material constructed by cross growth of nano sheets |
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