CN105129778A - Preparation method of nano ZnO/graphene composite material - Google Patents
Preparation method of nano ZnO/graphene composite material Download PDFInfo
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- CN105129778A CN105129778A CN201510434140.4A CN201510434140A CN105129778A CN 105129778 A CN105129778 A CN 105129778A CN 201510434140 A CN201510434140 A CN 201510434140A CN 105129778 A CN105129778 A CN 105129778A
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Abstract
The invention relates to a preparation method of a nano ZnO/graphene composite material. The preparation method includes following steps: (1) mixing a nano zinc oxide water solution with a chemically-reduced graphene oxide solution uniformly to prepare a mixture solution, wherein the mass ratio of nano zinc oxide to chemically-reduced graphene oxide is 1-100:1; (2) performing an ultrasound reaction to the mixture solution in an ultrasound instrument to obtain a reaction product; and (3) separating and washing the reaction product to obtain the nano ZnO/graphene composite material. The nano ZnO/graphene composite material is uniform in structure, is excellent in ultraviolet absorption performance, is simple in preparation method and device and is easy to achieve large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of nano composite material, especially relate to a kind of preparation method of nano-ZnO-graphene composite material.
Background technology
Within 2004, by since British scientist Geim reported first Graphene, become rapidly domestic and international study hotspot.The multifunctional semiconductor material of the most a kind of broad-band gap of zinc oxide, it not only has excellent chemistry and physical properties, also there is other many-sided excellent performances, show that zinc oxide has the aspects such as good electromechanical coupling performance, chemical stability and thermostability.The advantage that Graphene zinc oxide composite may have Graphene and nano zine oxide concurrently, as having the photoelectric conversion rate and electric transmission rate etc. of excellent translucidus, electroconductibility and colleges and universities, has wide practical use in fields such as electrochemistry, electrooptical device, battery or electrical condensers.
Current researchist mainly finds to adopt ultrasonic spray pyrolysis, and the Graphene-zinc oxide electrode material successfully prepared has good application prospect in super capacitor apparatus field.Adopt Metalorganic chemical vapor deposition method successfully to prepare Graphene-zinc oxide multifunctional conductor material, it compares mutually with Graphene, and it has excellent translucidus and electroconductibility, and remains the intrinsic advantageous property of zinc oxide.Obtain Graphene-nano zinc oxide material by Both Plasma Chemical Vapor enhanced deposition legal system is standby, confirmed it is a kind of raw material of very good manufacture Flied emission equipment.In addition, zinc salt and chemical reduction graphene oxide also can be adopted to have prepared Graphene-zinc oxide nanometer composite material by hydrothermal method, solvent-thermal method or microwave heating etc.But adopt above-mentioned various method apparatus expensive, process is complicated, and energy consumption is higher, and experimental cost is expensive, limits a large amount of synthesis of nano-ZnO-graphene composite material and the popularization of application thereof.
Chinese patent 201310350139.4 discloses a kind of short-cut method preparing Graphene-zinc-oxide nano rod composite material in ultrasonic wave.First utilize roll extrusion vibration mill for subsequent use sealing after common for 150g zinc powder grinding 5h in argon shield, by 50 order crystalline flake graphites and concentrated nitric acid in mass ratio 1:3 mix, and 10min is stirred at 30 DEG C, repeatedly after cleaning and filtering, 60 DEG C of dryings obtain expansible black lead, then in retort furnace, 900 DEG C of process 30s obtain expanded graphite, seal for subsequent use; Take ground zinc powder and expanded graphite in proportion in distilled water, then add dehydrated alcohol and stir, continuous ultrasound 6 ~ 10 hours in ultrasonic wave, leave standstill and extract upper part suspended substance and centrifugation after ten minutes, last 60 DEG C of vacuum-dryings obtain graphene-based nano-zinc oxide composite material.Although this patent technique is simple, the Stability Analysis of Structures of obtained graphene-based nano-zinc oxide composite material, its reaction times is longer, and productive rate is relatively low.
Summary of the invention
Object of the present invention is exactly provide a kind of preparation method of nano-ZnO-graphene composite material to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for nano-ZnO-graphene composite material, comprises the following steps:
(1) the nano zine oxide aqueous solution and chemical reduction graphene oxide solution are mixed, obtained mixing solutions, wherein, the mass ratio of nano zine oxide and chemical reduction graphene oxide is 1 ~ 100:1;
(2) mixing solutions that step (1) is obtained is put into ultrasonic instrument and carry out ultrasonic reaction, obtain reaction product;
(3) by after reaction product separation, washing, nano-ZnO-graphene composite material is namely obtained.
The concentration of the described nano zine oxide aqueous solution is 0.01mg/mL ~ 5mg/mL.
The concentration of described chemical reduction graphene oxide solution is 0.01mg/mL ~ 0.5mg/mL.
In step (2), the frequency of ultrasonic instrument is 40KHz, and power is 40 ~ 200W, and the time of ultrasonic reaction is 1 ~ 4h.
In step (1), the mass ratio of nano zine oxide and chemical reduction graphene oxide is 5 ~ 15:1.
In step (3), reaction product obtains nano-ZnO-graphene composite material after centrifugation, washing.
Nano-ZnO solution used in the present invention is by according to document (Zhang, Y.; Wu, H.; Huang, X.; Zhang, J.; Guo, S., NanoscaleRes.Lett.2011,6,450) making ZnO nano particle, and obtained ZnO nano Granular composite is formed in deionized water; Chemical reduction graphene oxide solution is according to document (Zhang, J.; Yang, H.; Shen, G.; Cheng, P.; Zhang, J.; Guo, S., Chem.Commun.2010,46,1112-1114.) prepare.
First the zinc oxide that the present invention adds and chemical reduction graphene oxide can be combined by electrostatic interaction, then under the high temperature and high pressure environment produced at ultrasonic cavitation, there is provided energy by ultrasonic wave and make zinc oxide and Graphene further combined with forming matrix material, and obtaining the nano-ZnO-graphene composite material of the three-dimensional micropore structure forming similar pod-like by the control time of ultrasonic reaction and the frequency of ultrasonic instrument.
Compared with prior art, simply, the reaction times is short, and productive rate is high, is convenient to scale of mass production, and obtained nano-ZnO-graphene composite material even structure is stablized, and has good uv absorption property for preparation method of the present invention and experimental installation.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of nano-ZnO-graphene composite material obtained in the embodiment of the present invention 1;
Fig. 2 is the uv-visible absorption spectroscopy figure of nano-ZnO-graphene composite material obtained in the embodiment of the present invention 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.The present embodiment is implemented premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
CRGO (chemical reduction graphene oxide solution) Homogeneous phase mixing of to be the nano-ZnO solution of 1mg/mL and 10mL concentration by 10mL concentration be 0.1mg/mL.Then mixed solution being put into ultrasonic instrument is 40KHz in frequency, and power is under the condition of 150W, ultrasonic reaction 2 hours.After reaction, product is centrifugal, washing after obtain nano-ZnO-graphene composite material.
Carry out scanning electron microscope to obtained nano-ZnO-graphene composite material, as shown in Figure 1, find that this matrix material forms three-dimensional micropore shape, nano ZnO particles is coated on Graphene inside to its result, defines the shape of similar pea pod.
Carry out uv-visible absorption spectroscopy sign to matrix material, as shown in Figure 2, compared with the CRGO finding this matrix material and simple same concentrations and nano ZnO particles, within the scope of 200-400nm, uv-absorbing obviously strengthens its result.
Embodiment 2
The CRGO Homogeneous phase mixing of to be the nano-ZnO solution of 5mg/mL and 10mL concentration by 10mL concentration be 1mg/mL.Then mixed solution being put into ultrasonic instrument is 40KHz in frequency, and power is under the condition of 200W, ultrasonic reaction 1 hour.After reaction, product is centrifugal, washing after obtain matrix material.
Embodiment 3
The CRGO Homogeneous phase mixing of to be 0.02mg/mL nano ZnO particles solution and 10mL concentration by 10mL concentration be 0.01mg/mL.Then under mixed solution to be put into ultrasonic instrument be 40KHz power be the condition of 40W in frequency, ultrasonic reaction 4 hours.After reaction, product is centrifugal, washing after obtain matrix material.
Embodiment 4
A preparation method for nano-ZnO-graphene composite material, comprises the following steps:
(1) the chemical reduction graphene oxide solution of to be the nano zine oxide aqueous solution of 0.01mg/mL and 10mL concentration by 10mL concentration be 0.01mg/mL mixes, obtained mixing solutions;
(2) mixing solutions that step (1) is obtained is put into ultrasonic instrument, be 40KHz in ultrasonic instrument frequency, power is ultrasonic reaction 2h under 100W condition, obtains reaction product;
(3) by after reaction product centrifugation, washing, nano-ZnO-graphene composite material is namely obtained.
Embodiment 5
A preparation method for nano-ZnO-graphene composite material, comprises the following steps:
(1) the chemical reduction graphene oxide solution of to be the nano zine oxide aqueous solution of 0.1mg/mL and 10mL concentration by 10mL concentration be 0.01mg/mL mixes, obtained mixing solutions;
(2) mixing solutions obtained for step (1) is put into ultrasonic instrument, ultrasonic reaction 1h under be 40KHz power being 200W condition in ultrasonic instrument frequency, obtains reaction product;
(3) by after reaction product centrifugation, washing, nano-ZnO-graphene composite material is namely obtained.
Embodiment 6
A preparation method for nano-ZnO-graphene composite material, comprises the following steps:
(1) the chemical reduction graphene oxide solution of to be the nano zine oxide aqueous solution of 5mg/mL and 10mL concentration by 10mL concentration be 0.05mg/mL mixes, obtained mixing solutions;
(2) mixing solutions obtained for step (1) is put into ultrasonic instrument, ultrasonic instrument frequency be 40KHz, power be 40W condition under ultrasonic reaction 4h, obtain reaction product;
(3) by after reaction product centrifugation, washing, nano-ZnO-graphene composite material is namely obtained.
Embodiment 7
A preparation method for nano-ZnO-graphene composite material, comprises the following steps:
(1) the chemical reduction graphene oxide solution of to be the nano zine oxide aqueous solution of 0.8mg/mL and 10mL concentration by 10mL concentration be 0.1mg/mL mixes, obtained mixing solutions;
(2) mixing solutions obtained for step (1) is put into ultrasonic instrument, ultrasonic instrument frequency be 40KHz, power be 40W condition under ultrasonic reaction 4h, obtain reaction product;
(3) by after reaction product centrifugation, washing, nano-ZnO-graphene composite material is namely obtained.
Embodiment 8
A preparation method for nano-ZnO-graphene composite material, comprises the following steps:
(1) the chemical reduction graphene oxide solution of to be the nano zine oxide aqueous solution of 1.5mg/mL and 10mL concentration by 10mL concentration be 0.1mg/mL mixes, obtained mixing solutions;
(2) mixing solutions obtained for step (1) is put into ultrasonic instrument, ultrasonic instrument frequency be 40KHz, power be 40W condition under ultrasonic reaction 4h, obtain reaction product;
(3) by after reaction product centrifugation, washing, nano-ZnO-graphene composite material is namely obtained.
The productive rate (taking zinc oxide as benchmark) of the nano-ZnO-graphene composite material of following table obtained by above-described embodiment.
Claims (6)
1. a preparation method for nano-ZnO-graphene composite material, is characterized in that, comprises the following steps:
(1) the nano zine oxide aqueous solution and chemical reduction graphene oxide solution are mixed, obtained mixing solutions, wherein, the mass ratio of nano zine oxide and chemical reduction graphene oxide is 1 ~ 100:1;
(2) mixing solutions that step (1) is obtained is put into ultrasonic instrument and carry out ultrasonic reaction, obtain reaction product;
(3) by after reaction product separation, washing, nano-ZnO-graphene composite material is namely obtained.
2. the preparation method of a kind of nano-ZnO-graphene composite material according to claim 1, is characterized in that, the concentration of the described nano zine oxide aqueous solution is 0.01mg/mL ~ 5mg/mL.
3. the preparation method of a kind of nano-ZnO-graphene composite material according to claim 1, is characterized in that, the concentration of described chemical reduction graphene oxide solution is 0.01mg/mL ~ 0.5mg/mL.
4. the preparation method of a kind of nano-ZnO-graphene composite material according to claim 1, is characterized in that, in step (2), the frequency of ultrasonic instrument is 40KHz, and the power of ultrasonic instrument is 40 ~ 200W, and the time of ultrasonic reaction is 1 ~ 4h.
5. the preparation method of a kind of nano-ZnO-graphene composite material according to claim 1, is characterized in that, in step (1), the mass ratio of nano zine oxide and chemical reduction graphene oxide is 5 ~ 15:1.
6. the preparation method of a kind of nano-ZnO-graphene composite material according to claim 1, is characterized in that, in step (3), reaction product obtains nano-ZnO-graphene composite material after centrifugation, washing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108168613A (en) * | 2017-12-29 | 2018-06-15 | 李文清 | The air-quality monitoring system to cooperate with unmanned plane |
| CN108627554A (en) * | 2018-05-09 | 2018-10-09 | 东莞理工学院 | Glucose sensor modified electrode and preparation method thereof |
| CN113443646A (en) * | 2021-06-30 | 2021-09-28 | 华南师范大学 | Composite material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102430401A (en) * | 2011-09-20 | 2012-05-02 | 上海大学 | Nanometer ZnO/graphene photo-catalyst and preparation method thereof |
| CN102654474A (en) * | 2011-03-02 | 2012-09-05 | 中国科学院微电子研究所 | Making method of nano film of graphene doped zinc oxide |
| CN103449504A (en) * | 2013-06-26 | 2013-12-18 | 中山大学 | Zinc oxide nanodisk/graphene composite material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102654474A (en) * | 2011-03-02 | 2012-09-05 | 中国科学院微电子研究所 | Making method of nano film of graphene doped zinc oxide |
| CN102430401A (en) * | 2011-09-20 | 2012-05-02 | 上海大学 | Nanometer ZnO/graphene photo-catalyst and preparation method thereof |
| CN103449504A (en) * | 2013-06-26 | 2013-12-18 | 中山大学 | Zinc oxide nanodisk/graphene composite material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108168613A (en) * | 2017-12-29 | 2018-06-15 | 李文清 | The air-quality monitoring system to cooperate with unmanned plane |
| CN108627554A (en) * | 2018-05-09 | 2018-10-09 | 东莞理工学院 | Glucose sensor modified electrode and preparation method thereof |
| CN113443646A (en) * | 2021-06-30 | 2021-09-28 | 华南师范大学 | Composite material and preparation method and application thereof |
| WO2023272887A1 (en) * | 2021-06-30 | 2023-01-05 | 华南师范大学 | Composite material, preparation method therefor and application thereof |
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