CN104076073A - Short-bar-shaped nano-zinc oxide/graphene compound and preparation method thereof - Google Patents
Short-bar-shaped nano-zinc oxide/graphene compound and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a short-bar-shaped nano-zinc oxide/graphene compound and a preparation method thereof. Nano-zinc oxide in the compound is uniformly supported on the surface of a graphene sheet layer and shaped as a short bar. The preparation method of the compound comprises the following steps: dispersing a graphene oxide aqueous solution in absolute ethyl alcohol, and subsequently carrying out ultrasonic treatment to obtain a uniform dispersion liquid; adding a surface surfactant, namely polyethylene glycol 400, into the dispersion liquid to obtain a mixed liquid; dissolving Zn(NO3)2.6H2O in the absolute ethyl alcohol, and then adding to the mixed liquid; and adjusting pH of the mixed liquid to 9-10, then carrying out constant-temperature reaction in a sealed reaction kettle, and washing and drying a product after the reaction is ended to obtain a target product. The preparation method of the compound is a soft chemical method which is simple to operate, can be used for preparing the target product with excellent gas-sensitive property, and is good in application prospect in the field of gas-sensitive sensors.
Description
Technical field
The present invention relates to a kind of nano-complex and preparation method thereof, particularly a kind of corynebacterium nano zine oxide/graphene complex and preparation method thereof.
Background technology
Zinc paste is a kind of important semiconductor material, due to its unique electricity, optical characteristics, has caused in recent years very big concern.As everyone knows, the pattern of air-sensitive performance and material, especially relevant with material surface area.Nano zinc oxide material have specific surface area large, be easy to prepare the features such as compound substance, in fields such as gas sensors, have wide practical use.Such as nano level zinc paste, the gas meters such as alcohol are revealed to higher sensitivity, the sensor that utilizes this characteristic to prepare can be used for the detection of alcohol concentration in expiration, prevents from drivining a car under the influence of alcohol, and reduces traffic hazard.But the detection sensitivity of zinc paste is on the low side at present, and working temperature is higher, and therefore, we need to be compound by zinc paste and other materials, improves its gas sensitization performance.
Graphene is the allotrope of the carbon that discovered in recent years is new, is a kind of two-dimensional nano material of uniqueness.Graphene has unique electronic structure, huge specific surface area and minimum band gap etc., makes the interaction between Graphene and gas molecule can show many distinctive phenomenons.The inorganic oxide and the Graphene that are used as gas sensitive is compound, can increase its dispersiveness because of the existence of Graphene, for its research at the microelectric techniques such as gas sensor and device provides new approaches and new direction.
Document 1 (Bie L J, Yan X N, Yin J, et al.Nanopillar ZnO gas sensor for hydrogen and ethanol[J] .Sensors and Actuators B:Chemical, 2007,126 (2): the preparation method who 604-608.) has reported a kind of columnar nanometer zinc paste as ethanol sensor.The columnar nanometer zinc paste obtaining by two step solwution methods is about 44 to the sensitivity of 1000ppm alcohol gas at 350 ℃.
Document 2 (Jiaqiang X, Yuping C, Daoyong C, et al.Hydrothermal synthesis and gas sensing characters of ZnO nanorods[J] .Sensors and Actuators B:Chemical, 2006,113 (1): 526-531.) reported that an a kind of step solvent-thermal method prepares the method for rod-like nano-zinc oxide.Zinc powder and cetyl trimethyl ammonium bromide are scattered in and in deionized water, form suspending liquid, then 182 ℃ of reaction 24h in closed reactor.Reaction finishes afterproduct and obtains rod-like nano-zinc oxide through washing, being dried, and at 332 ℃, the sensitivity of 1000ppm alcohol gas is about 52.
Document 3 (Fu D, Han G, Chang Y, et al.The synthesis and properties of ZnO-graphene nano hybrid for photodegradation of organic pollutant in water[J] .Materials Chemistry and Physics, 2012,132 (2): 673-681.) reported a kind of preparation method of nano zine oxide/graphene complex, and be applied to water pollution processing aspect.Graphite oxide aqueous solution is scattered in absolute ethyl alcohol, adds LiOHH
2o obtains mixed liquor; By Zn (CH
3cOO)
22H
2o is dissolved in absolute ethyl alcohol, continues at 80 ℃ to stir after 20min, is cooled to 50 ℃, and above-mentioned mixed liquor is added, and continues to stir 40min.After cooling, add hexane storage overnight at 4 ℃, filter by washing, the dry nano zine oxide/graphene complex that obtains.
There is following defect in above-mentioned preparation method: 1, complicated operation is not suitable for practical application; 2, nano zine oxide has higher chemical activity, show obvious surface effect, easily generation is assembled and is reached steady state (SS), thereby reunite, occurs, reduced and gas between interaction, cause for the sensitivity of the nano zine oxide of gas sensor on the low side.
Summary of the invention
The object of the present invention is to provide a kind of corynebacterium nano zine oxide/graphene complex and preparation method thereof, is that nano zine oxide is mutually compound with Graphene, is applied to gas sensor.
The technical solution that realizes the object of the invention is:
Corynebacterium nano zine oxide/graphene complex, in described compound, nano zine oxide uniform load, on graphene sheet layer surface, is corynebacterium; Described corynebacterium nano zine oxide/graphene complex is prepared by the following method:
Step 1: graphite oxide aqueous solution is scattered in absolute ethyl alcohol, then carries out ultrasonic processing, obtain uniform dispersion liquid;
Step 2: surfactant polyethylene 400 is joined in the dispersion liquid that step 1 obtains, obtain mixed liquor;
Step 3: by Zn (NO
3)
26H
2o is dissolved in absolute ethyl alcohol, then joins in the mixed liquor of step 2;
Step 4: regulate pH of mixed to 9～10, then isothermal reaction in closed reactor, reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
Above-mentioned reaction is carried out under lasting stirring condition.
In step 1, the concentration of graphite oxide aqueous solution is 5～30mg/g, and ultrasonic time is 10～120min;
Zn (NO in graphite oxide aqueous solution and step 3 in step 1
3)
26H
2the mass ratio of O is 1:33～1:3650.
In step 2, in PEG400 and system, the volume ratio of absolute ethyl alcohol is 1:70～1:10.
In step 4, select NaOH aqueous solution to regulate pH of mixed value, the concentration of NaOH aqueous solution is 0.5～10mol/L.
In step 4, reaction kettle for reaction temperature is 120～180 ℃, and the reaction time is 12～48h.
Principle explanation:
Graphene oxide surface band negative charge, as Zn (NO
3)
26H
2when O and graphene oxide mix, the Zn of positively charged
2+because the effect of electrostatic force is adsorbed onto graphene oxide surface, add after NaOH solution, original position forms Zn (OH)
2.In follow-up heat treatment process, it can be used as nuclear particle and grows by your moral slaking of Oswald, corynebacterium nano zine oxide in load.Meanwhile, when corynebacterium nano zine oxide forms, graphene oxide is reduced into Graphene by ethanol, and due to the adsorption of corynebacterium nano zine oxide, graphene sheet layer can not be brought together.Surfactant polyethylene 400 has played very important effect, appreciable impact pattern and the structure of material, for by nano zine oxide uniform load on graphene sheet layer surface, prepare corynebacterium nano zine oxide/graphene complex.
The present invention compared with prior art, has following remarkable advantage:
(1) described preparation method is prepared by a step solvent-thermal method, simple to operate.
(2) adopting PEG400 is surfactant, for by nano zine oxide uniform load on graphene sheet layer surface, appreciable impact pattern and the structure of material.
(3) due to the adsorption of corynebacterium nano zine oxide, prevent the reunion of graphene sheet layer, for giving full play to its excellent properties, established solid foundation.
(4) Graphene has unique electronic structure, huge specific surface area and minimum band gap etc., make the interaction between Graphene and gas molecule can show many distinctive phenomenons, make the interaction between Graphene and gas molecule can show many distinctive phenomenons.
(5) inorganic oxide and the Graphene that are used as gas sensitive is compound, can increase its dispersiveness because of the existence of Graphene, for its research at the microelectric techniques such as gas sensor and device provides new approaches and new direction, gained corynebacterium nano zine oxide/graphene composite material shows excellent air-sensitive performance.
(6) in corynebacterium nano zine oxide/graphene complex that the present invention prepares, nano zine oxide uniform load, on graphene sheet layer surface, is corynebacterium form, has excellent air-sensitive performance, in gas sensor field, has good application prospect.
Accompanying drawing explanation
Fig. 1 is the preparation method's of corynebacterium nano zine oxide/graphene complex of the present invention schematic flow sheet.
Fig. 2 presses transmission electron microscope (TEM) figure of embodiment 1 reaction conditions gained corynebacterium nano zine oxide/graphene complex under different amplification.
Fig. 3 presses embodiment 1 reaction conditions gained corynebacterium nano zine oxide/graphene complex air-sensitive performance response recovery curve figure to the nano zine oxide of response recovery curve figure (a) load 3% Graphene of different concentration ethanol at 400 ℃, (b) air-sensitive performance of nano zine oxide response recovery curve figure.
Fig. 4 presses embodiment 1 reaction conditions gained corynebacterium nano zine oxide/graphene complex sensitivity map to 100ppm gas with various at 370 ℃.
Fig. 5 (a) is by transmission electron microscope (TEM) figure of comparative example 1 reaction conditions gained corynebacterium nano zine oxide/graphene complex, (b) by transmission electron microscope (TEM) figure of comparative example 2 reaction conditions gained corynebacterium nano zine oxide/graphene complexes.
Embodiment
In conjunction with Fig. 1, the preparation method of a kind of corynebacterium nano zine oxide/graphene complex of the present invention, described method adopts surfactant polyethylene 400 for nano zine oxide uniform load is surperficial at graphene sheet layer, specifically comprises the following steps:
Step 1: graphite oxide aqueous solution is scattered in absolute ethyl alcohol, then carries out ultrasonic processing, obtain uniform dispersion liquid; The concentration of graphite oxide aqueous solution is 5～30mg/g, and ultrasonic time is 10～120min;
Step 2: surfactant polyethylene 400 is joined in the dispersion liquid that step 1 obtains, obtain mixed liquor; In PEG400 and system, the volume ratio of absolute ethyl alcohol is 1:70～1:10;
Step 3: by Zn (NO
3)
26H
2o is dissolved in absolute ethyl alcohol, then joins in the mixed liquor of step 2; Zn (NO in graphite oxide aqueous solution and step 3 in step 1
3)
26H
2the mass ratio of O is 1:33～1:3650;
Step 4: NaOH aqueous solution regulates pH of mixed to 9～10, then isothermal reaction in closed reactor, temperature of reaction is 120～180 ℃, and the reaction time is 12～48h, and reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains; The concentration of NaOH aqueous solution is 0.5～10mol/L.
Above-mentioned reaction is carried out under lasting stirring condition.
Below in conjunction with embodiment, comparative example and accompanying drawing, the present invention is further detailed explanation:
Embodiment 1:
Step 1: 0.7550g graphite oxide aqueous solution (20mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 30min, obtain uniform dispersion liquid;
Step 2: 2mL PEG400 is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 1.7849gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min, then joins in the mixed liquor of step 2, stirs 20～60min;
Step 4: the NaOH aqueous solution of 2.5mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 180 ℃ of temperature of reaction, the reaction time is 12h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
As shown in Figure 2, corynebacterium nano zine oxide loads on graphene sheet layer surface to the photo of products therefrom uniformly, without extensive agglomeration, produces.The spacing of lattice that shows the corynebacterium nano zine oxide/graphene composite material of preparation in Fig. 2 (d) is 0.258nm, has good crystal formation.In Fig. 3, display material is relevant with tested gas concentration to the susceptibility of tested gas, and air-sensitive performance improves along with the rising of concentration of alcohol.At 400 ℃, the nano zine oxide of load 3% Graphene is 505 to the sensitivity of the ethanol of 1000ppm, and the sensitivity of nano zine oxide is 103, is 5 times of nano zine oxide sensitivity, and this shows the high sensitivity of graphene-supported corynebacterium nano zine oxide.Fig. 4 is the ZnO composite nano materials element of the 3% Graphene sensitivity to 100ppm gas with various of adulterating at 370 ℃, from sensitivity coordinate (horizontal ordinate), analyze: this element is especially outstanding to the sensitivity of ethanol, show it and be similar in drunk driving test and there is unique prospect, there is good gas-selectively.
Embodiment 2:
Step 1: 0.8221g graphite oxide aqueous solution (10mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 30min, obtain uniform dispersion liquid;
Step 2: 2mL PEG400 is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 2.9749gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min, then joins in the mixed liquor of step 2, stirs 20～60min;
Step 4: the NaOH aqueous solution of 5mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 180 ℃ of temperature of reaction, the reaction time is 24h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
By air-sensitive measuring and calculation, corynebacterium nano zine oxide/graphene composite material sensitivity that this example obtains is 312.
Embodiment 3:
Step 1: 0.1631g graphite oxide aqueous solution (5mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 10min, obtain uniform dispersion liquid;
Step 2: 1mL PEG400 is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 2.9749gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min, then joins in the mixed liquor of step 2, stirs 20～60min;
Step 4: the NaOH aqueous solution of 10mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 180 ℃ of temperature of reaction, the reaction time is 48h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
By air-sensitive measuring and calculation, corynebacterium nano zine oxide/graphene composite material sensitivity that this example obtains is 283.
Embodiment 4:
Step 1: 0.6783g graphite oxide aqueous solution (25mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 90min, obtain uniform dispersion liquid;
Step 2: 5mL PEG400 is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 1.4875gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min, then joins in the mixed liquor of step 2, stirs 20～60min;
Step 4: the NaOH aqueous solution of 2.5mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 160 ℃ of temperature of reaction, the reaction time is 24h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
By air-sensitive measuring and calculation, corynebacterium nano zine oxide/graphene composite material sensitivity that this example obtains is 164.
Embodiment 5:
Step 1: 0.9015g graphite oxide aqueous solution (30mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 120min, obtain uniform dispersion liquid;
Step 2: 7mL PEG400 is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 0.8925gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min; Then join in the mixed liquor of step 2, stir 20～60min;
Step 4: the NaOH aqueous solution of 0.5mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 120 ℃ of temperature of reaction, the reaction time is 24h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
By air-sensitive measuring and calculation, corynebacterium nano zine oxide/graphene composite material sensitivity that this example obtains is 116.
Comparative example 1:
Step 1: 0.7550g graphite oxide aqueous solution (20mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 30min, obtain uniform dispersion liquid;
Step 2: 0.1g cetyl trimethyl ammonium bromide is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 1.7849gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min, then joins in the mixed liquor of step 2, stirs 20～60min;
Step 4: the NaOH aqueous solution of 2.5mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 180 ℃ of temperature of reaction, the reaction time is 12h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
By air-sensitive measuring and calculation, corynebacterium nano zine oxide/graphene composite material sensitivity that this example obtains is 105.
Comparative example 2:
Step 1: 0.7550g graphite oxide aqueous solution (20mg/g) is scattered in 60mL absolute ethyl alcohol, stirs 20～60min, then carry out ultrasonic processing 30min, obtain uniform dispersion liquid;
Step 2: 2mL Macrogol 4000 is joined in the dispersion liquid that step 1 obtains, stir 20～60min, obtain mixed liquor;
Step 3: by 1.7849gZn (NO
3)
26H
2o is dissolved in 10mL absolute ethyl alcohol, stirs 20～60min, then joins in the mixed liquor of step 2, stirs 20～60min;
Step 4: the NaOH aqueous solution of 2.5mol/L is joined in step 3, regulate pH to 9～10, then isothermal reaction in closed reactor, 180 ℃ of temperature of reaction, the reaction time is 12h; Reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
By air-sensitive measuring and calculation, corynebacterium nano zine oxide/graphene composite material sensitivity that this example obtains is 132.
Conclusion: in conjunction with transmission electron microscope (TEM) figure of Fig. 2 and Fig. 5, the form of having shown clearly the nano zine oxide/graphene complex forming, when surfactant is cetyl trimethyl ammonium bromide, there is a large amount of particles to be scattered in graphene film outside; When surfactant is Macrogol 4000, adulterate inhomogeneous, fold place is more, and particle is oval; When surfactant is PEG400, be entrained in the nano particle structure homogeneous on Graphene, be bar-shaped.Analyze possible reason, cetyl trimethyl ammonium bromide is cationic surfactant, can occupy Zn
2+growth site, suppress Zn
2+and the electrostatic interaction between the anion active group of graphene oxide; Compared to Macrogol 4000, PEG400 molecular weight, and the coordination ability of zincite crystal is stronger, is conducive to nano zine oxide in the dispersion on graphene sheet layer surface, and cause the change of nano zine oxide pattern.
Claims (8)
1. corynebacterium nano zine oxide/graphene complex, is characterized in that, in described compound, nano zine oxide uniform load, on graphene sheet layer surface, is corynebacterium; Described corynebacterium nano zine oxide/graphene complex is prepared by the following method:
Step 1: graphite oxide aqueous solution is scattered in absolute ethyl alcohol, then carries out ultrasonic processing, obtain uniform dispersion liquid;
Step 2: surfactant polyethylene 400 is joined in the dispersion liquid that step 1 obtains, obtain mixed liquor;
Step 3: by Zn (NO
3)
26H
2o is dissolved in absolute ethyl alcohol, then joins in the mixed liquor of step 2;
Step 4: regulate pH of mixed to 9～10, then isothermal reaction in closed reactor, reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains.
2. corynebacterium nano zine oxide/graphene complex according to claim 1, is characterized in that:
Reaction is carried out under lasting stirring condition.
3. corynebacterium nano zine oxide/graphene complex according to claim 1, is characterized in that:
In step 1, the concentration of graphite oxide aqueous solution is 5～30mg/g, and ultrasonic time is 10～120min; Zn (NO in graphite oxide aqueous solution and step 3 in step 1
3)
26H
2the mass ratio of O is 1:33～1:3650.
4. corynebacterium nano zine oxide/graphene complex according to claim 1, is characterized in that: in step 2, in PEG400 and system, the volume ratio of absolute ethyl alcohol is 1:70～1:10.
5. corynebacterium nano zine oxide/graphene complex according to claim 1, is characterized in that: in step 4, select NaOH aqueous solution to regulate pH of mixed value, the concentration of NaOH aqueous solution is 0.5～10mol/L.
6. corynebacterium nano zine oxide/graphene complex according to claim 1, is characterized in that: in step 4, reaction kettle for reaction temperature is 120～180 ℃, and the reaction time is 12～48h.
7. a preparation method for corynebacterium nano zine oxide/graphene complex, is characterized in that: described method adopt surfactant polyethylene 400 for by nano zine oxide uniform load on graphene sheet layer surface, specifically comprise the following steps:
Step 1: graphite oxide aqueous solution is scattered in absolute ethyl alcohol, then carries out ultrasonic processing, obtain uniform dispersion liquid; The concentration of graphite oxide aqueous solution is 5～30mg/g, and ultrasonic time is 10～120min;
Step 2: surfactant polyethylene 400 is joined in the dispersion liquid that step 1 obtains, obtain mixed liquor; In PEG400 and system, the volume ratio of absolute ethyl alcohol is 1:70～1:10;
Step 3: by Zn (NO
3)
26H
2o is dissolved in absolute ethyl alcohol, then joins in the mixed liquor of step 2; Zn (NO in graphite oxide aqueous solution and step 3 in step 1
3)
26H
2the mass ratio of O is 1:33～1:3650;
Step 4: NaOH aqueous solution regulates pH of mixed to 9～10, then isothermal reaction in closed reactor, temperature of reaction is 120～180 ℃, and the reaction time is 12～48h, and reaction finishes afterproduct through washing, the dry corynebacterium nano zine oxide/graphene complex that obtains; The concentration of NaOH aqueous solution is 0.5～10mol/L.
8. the preparation method of corynebacterium nano zine oxide/graphene complex according to claim 7, is characterized in that: reaction is carried out under lasting stirring condition.
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