CN104857945A - Preparation method of zinc oxide/carbon micro-sphere composite material - Google Patents
Preparation method of zinc oxide/carbon micro-sphere composite material Download PDFInfo
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- CN104857945A CN104857945A CN201510216404.9A CN201510216404A CN104857945A CN 104857945 A CN104857945 A CN 104857945A CN 201510216404 A CN201510216404 A CN 201510216404A CN 104857945 A CN104857945 A CN 104857945A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of a zinc oxide/carbon micro-sphere composite material. The preparation method comprises the following steps that sucrose dissolves in water, and then the solution is transmitted to a stainless steel reaction kettle to conduct a hydrothermal reaction, so that a brownish black mixed solution is obtained; the obtained brownish black mixed solution is processed through extraction filtration and drying, so that dried black substances are carbon micro-spheres; the carbon micro-spheres are dispersed in water, Zn(Ac)2.2H2O dissolves in the mixed solution with the dispersed carbon micro-spheres, then the mixed solution is stirred, ammonia water is dropwise added to the mixed solution, and finally, a dark gray substrate is obtained and processed through high-temperature annealing, so that a zinc oxide/carbon micro-sphere compound is obtained. According to the prepared zinc oxide/carbon micro-sphere composite material, zinc oxide nano-particles uniformly wrap the carbon micro-spheres, the micro-spheres of the composite product is uniform in size, the diameter of each micro-sphere is 5-6 micrometers, and the zinc oxide/carbon micro-sphere composite material can be applied to the fields of photocatalysis, electrochemical sensing and supercapacitors.
Description
Technical field
The invention belongs to material science, be specifically related to the preparation method of a kind of zinc oxide/carbon micro-spheres composite.
Technical field
After the New Type of Carbon functional materials such as fullerene, CNT, Graphene are found and successfully prepare, the research overbearing tide of material with carbon element did not at all just disappear.Because the particularity of carbon self structure determines the diversity of material with carbon element in application aspect.In the preparation method of numerous carbon micro-spheres, hydro-thermal method is the effective synthetic method of a kind of simple and fast.Recently, the carbosphere with superior chemical stability and good electric conductivity causes the extensive concern of people gradually in electrochemical research field, but the limitation performance of carbosphere electric conductivity limits its application; Along with the compound that deeply it is found that some heavy metal, metal oxide and carbosphere material of research, positive effect is served to its utilization rate of raising, but the uniformity of the particle that heavy metal, metal oxide and carbosphere material are prepared from and coated uniformity all poor, comparatively serious to the performance impact of the material be prepared into.Zinc oxide is a kind of Multifunctional straight tape splicing gap semiconductor material, have nontoxic, synthesis technique is simple, pattern is easily controlled, cheap, good chemical stability and heat endurance, have a wide range of applications in photocatalysis, sensing and Flied emission etc.
Summary of the invention
The object of the invention is to adopt simple mechanical agitation that zinc hydroxide is loaded to carbon micro-spheres surface, then annealed temperature prepares zinc oxide/carbon micro-spheres composite that Zinc oxide nanoparticle evenly wraps up.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for zinc oxide/carbon micro-spheres composite, comprises the steps:
Step one, by 1-6g sucrose dissolved in the deionized water of 40ml, is then transferred to 50ml and carries out hydro-thermal reaction containing in teflon-lined stainless steel cauldron, reaction temperature is 150-190 DEG C, time is 5-24h, finally naturally cools to room temperature, obtains brownish black mixed solution;
Step 2, brownish black mixed solution step one be obtained by reacting is 0.22-0.45 μm of filter membrane suction filtration with aperture in glass sand core funnel, then deionized water, absolute ethyl alcohol cyclic washing at least twice is used respectively, finally dry filtering the atrament obtained in the temperature of 50-80 DEG C, the atrament after oven dry is carbon micro-spheres;
Step 3,0.05-0.5g carbon micro-spheres step 2 prepared is dispersed in 50ml deionized water, 0.5-5g Zn (Ac)
22H
2o is dissolved in and is dispersed with in the mixed solution of carbon micro-spheres, then stir and dropwise add the ammoniacal liquor that 1-3mL mass fraction is 37%, the stirring reaction time is 1-8h, afterwards by the centrifugation under the rotating speed of 5000-10000 rev/min of product supercentrifuge, the lower floor's material obtained after separation is used deionized water and absolute ethyl alcohol eccentric cleaning respectively, finally obtains dark-grey material;
Step 4, dark-grey material tube furnace step 3 eccentric cleaning obtained carries out vacuum annealing at 400-800 DEG C, naturally cools to room temperature, namely obtain zinc oxide/carbon micro-spheres compound after keeping 1-3h.
In described step one, in aqueous sucrose solution, the content of sucrose is 2g/40ml.
In described step 2 and step 4, the aperture of miillpore filter is 0.22 μm.
In described step 3, the carbon micro-spheres amount joined in deionized water is divided into 0.1g/50ml, Zn (Ac)
22H
2the O amount joined in deionized water is 1.355g/50ml.
This preparation method's technique is tight, simple, be easy to realize industrialization, zinc oxide/carbon micro-spheres the composite prepared through the present invention is that Zinc oxide nanoparticle is wrapped in carbon micro-spheres surface uniformly, the micron ball size of combination product is even, diameter is at 5-6 μm, and zinc oxide/carbon micro-spheres composite can be applicable to the fields such as photocatalysis, electrochemical sensing, super capacitor.
Accompanying drawing explanation
The XRD collection of illustrative plates of the zinc oxide/carbon micro-spheres of Fig. 1 zinc hydroxide/carbon micro-spheres and 400 DEG C of annealing in process.
The SEM picture of Fig. 2 carbon micro-spheres.
The SEM picture of Fig. 3 zinc hydroxide/carbon micro-spheres composite.
Zinc oxide/the carbon micro-spheres of Fig. 4 400 DEG C of annealing in process SEM picture.
Detailed description of the invention
embodiment 1
A preparation method for zinc oxide/carbon micro-spheres composite, comprises the steps:
Step one, by 1-6g sucrose dissolved in the deionized water of 40ml, is then transferred to 50ml and carries out hydro-thermal reaction containing in teflon-lined stainless steel cauldron, reaction temperature is 150-190 DEG C, time is 5-24h, finally naturally cools to room temperature, obtains brownish black mixed solution;
Step 2, brownish black mixed solution step one be obtained by reacting is 0.22-0.45 μm of filter membrane suction filtration with aperture in glass sand core funnel, then deionized water, absolute ethyl alcohol cyclic washing at least twice is used respectively, finally dry filtering the atrament obtained in the temperature of 50-80 DEG C, the atrament after oven dry is carbon micro-spheres;
Step 3,0.05-0.5g carbon micro-spheres step 2 prepared is dispersed in 50ml deionized water, 0.5-5g Zn (Ac)
22H
2o is dissolved in and is dispersed with in the mixed solution of carbon micro-spheres, then stir and dropwise add the ammoniacal liquor that 1-3mL mass fraction is 37%, the stirring reaction time is 1-8h, afterwards by the centrifugation under the rotating speed of 5000-10000 rev/min of product supercentrifuge, the lower floor's material obtained after separation is used deionized water and absolute ethyl alcohol eccentric cleaning respectively, finally obtains dark-grey material;
Step 4, dark-grey material tube furnace step 3 eccentric cleaning obtained carries out vacuum annealing at 400-800 DEG C, naturally cools to room temperature, namely obtain zinc oxide/carbon micro-spheres compound after keeping 1-3h.
In described step one, in aqueous sucrose solution, the content of sucrose is 2g/40ml.
In described step 2 and step 4, the aperture of miillpore filter is 0.22 μm.
In described step 3, the carbon micro-spheres amount joined in deionized water is divided into 0.1g/50ml, Zn (Ac)
22H
2the O amount joined in deionized water is 1.355g/50ml.
Embodiment 2
A preparation method for zinc oxide/carbon micro-spheres composite, comprises the steps:
Step one, by 2g sucrose dissolved in 40ml deionized water, then the sucrose solution of achromaticity and clarification is transferred to 50ml containing in teflon-lined stainless steel cauldron, with air dry oven at 180 DEG C of Water Under thermal response 12h, then naturally cools to room temperature and obtain brownish black mixed solution;
Step 2, brownish black mixed solution step one be obtained by reacting filter membrane suction filtration in glass sand core funnel of 0.22 μm, then rinses number secondary repeatedly with deionized water, absolute ethyl alcohol, will filter the atrament 60 DEG C oven dry obtained;
Step 3,0.1g carbon micro-spheres step 2 prepared is dispersed in 50ml deionized water, 1.355g Zn (Ac)
22H
2o is dissolved in and is dispersed with in the dark solution of carbon micro-spheres, then stir and dropwise add the ammoniacal liquor that 2.5mL mass fraction is 37%, the stirring reaction time is 4h, obtain the mixed solution of Dark grey, afterwards by the centrifugation under the rotating speed of 7000 revs/min of product supercentrifuge, the lower floor's material obtained after separation is used deionized water and absolute ethyl alcohol eccentric cleaning respectively, finally obtains dark-grey material;
Step 4, dark-grey material tube furnace step 3 eccentric cleaning obtained carries out vacuum annealing at 400 DEG C, naturally cools to room temperature, namely obtain zinc oxide/carbon micro-spheres compound after keeping 2h
Embodiment 3
A preparation method for zinc oxide/carbon micro-spheres composite, comprises the steps:
Step one, by 6g sucrose dissolved in 40ml deionized water, then the sucrose solution of achromaticity and clarification is transferred to 50ml containing in teflon-lined stainless steel cauldron, with air dry oven at 180 DEG C of Water Under thermal response 12h, then naturally cools to room temperature and obtain brownish black mixed solution;
Step 2, brownish black mixed solution step one be obtained by reacting filter membrane suction filtration in glass sand core funnel of 0.22 μm, then rinses number secondary repeatedly with deionized water, absolute ethyl alcohol, will filter the atrament 60 DEG C oven dry obtained;
Step 3,0.3g carbon micro-spheres step 2 prepared is dispersed in 50ml deionized water, 4g Zn (Ac)
22H
2o is dissolved in and is dispersed with in the dark solution of carbon micro-spheres, then stir and dropwise add the ammoniacal liquor that 1-3mL mass fraction is 37%, the stirring reaction time is 4h, obtain the mixed solution of Dark grey, afterwards by the centrifugation under the rotating speed of 10000 revs/min of product supercentrifuge, the lower floor's material obtained after separation is used deionized water and absolute ethyl alcohol eccentric cleaning respectively, finally obtains dark-grey material;
Step 4, dark-grey material tube furnace step 3 eccentric cleaning obtained carries out vacuum annealing at 400 DEG C, naturally cools to room temperature, namely obtain zinc oxide/carbon micro-spheres compound after keeping 3h
Embodiment 4-13
Concrete implementation step as embodiment 2, concrete technological parameter and amount of substance as shown in table 1:
Test result:
The sample that this test adopts is that embodiment 2 is prepared from, and the model of the ESEM of employing is: Hitachi S-4800, and the model of X-ray diffractometer is: D8/ADVANCE of science.
Its test case and result as follows:
X-ray diffraction is tested: Fig. 1 is the XRD collection of illustrative plates of zinc hydroxide/carbon micro-spheres and 400 DEG C of zinc oxide/carbon micro-spheres, on collection of illustrative plates, a display is the diffraction maximum of zinc hydroxide, b display be the diffraction maximum of zinc oxide, because the XRD diffracted intensity of carbon is lower, easily covered with other material compound tense, so its diffraction maximum can not be shown.
Scanning electron microscope test: Fig. 2,3,4 is the scanning electron microscope diagram sheet of zinc oxide/carbon micro-spheres of carbon micro-spheres, zinc hydroxide/carbon micro-spheres composite, 400 DEG C of annealing in process respectively, no matter zinc hydroxide/carbon micro-spheres can be found out in figure, or the particle diameter of zinc oxide/carbon micro-spheres is compared with carbon micro-spheres, increases all to some extent.
Claims (4)
1. a preparation method for zinc oxide/carbon micro-spheres composite, is characterized in that comprising the steps:
Step one, by 1-6g sucrose dissolved in the deionized water of 40ml, is then transferred to 50ml and carries out hydro-thermal reaction containing in teflon-lined stainless steel cauldron, reaction temperature is 150-190 DEG C, time is 5-24h, finally naturally cools to room temperature, obtains brownish black mixed solution;
Step 2, brownish black mixed solution step one be obtained by reacting is 0.22-0.45 μm of filter membrane suction filtration with aperture in glass sand core funnel, then deionized water, absolute ethyl alcohol cyclic washing at least twice is used respectively, finally dry filtering the atrament obtained in the temperature of 50-80 DEG C, the atrament after oven dry is carbon micro-spheres;
Step 3,0.05-0.5g carbon micro-spheres step 2 prepared is dispersed in 50ml deionized water, 0.5-5g Zn (Ac)
22H
2o is dissolved in and is dispersed with in the mixed solution of carbon micro-spheres, then stir and dropwise add the ammoniacal liquor that 1-3mL mass fraction is 37%, the stirring reaction time is 1-8h, afterwards by the centrifugation under the rotating speed of 5000-10000 rev/min of product supercentrifuge, the lower floor's material obtained after separation is used deionized water and absolute ethyl alcohol eccentric cleaning respectively, finally obtains dark-grey material;
Step 4, dark-grey material tube furnace step 3 eccentric cleaning obtained carries out vacuum annealing at 400-800 DEG C, naturally cools to room temperature, namely obtain zinc oxide/carbon micro-spheres compound after keeping 1-3h.
2. the preparation method of zinc oxide according to claim 1/carbon micro-spheres composite, is characterized in that: in described step one, in aqueous sucrose solution, the content of sucrose is 2g/40ml.
3. the preparation method of zinc oxide according to claim 2/carbon micro-spheres composite, is characterized in that: in described step 2 and step 4, the aperture of miillpore filter is 0.22 μm.
4. the preparation method of zinc oxide according to claim 3/carbon micro-spheres composite, is characterized in that: in described step 3, the carbon micro-spheres amount joined in deionized water is divided into 0.1g/50ml, Zn (Ac)
22H
2the O amount joined in deionized water is 1.355g/50ml.
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Cited By (8)
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| CN105552334A (en) * | 2016-01-11 | 2016-05-04 | 杭州电子科技大学 | Preparation method for carbon-film-coated zinc oxide hollow sphere |
| CN107552034A (en) * | 2017-08-21 | 2018-01-09 | 信阳师范学院 | A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet |
| CN107958995A (en) * | 2017-12-22 | 2018-04-24 | 湖南工业大学 | A kind of dried persimmon shape core shell structure C/ZnO lithium-ion negative pole electrode piece preparation methods and its fastening lithium ionic cell |
| CN108054372A (en) * | 2017-12-22 | 2018-05-18 | 湖南工业大学 | A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof |
| CN108987720A (en) * | 2018-08-01 | 2018-12-11 | 吉林大学 | Carbon/zinc oxide composite and its preparation method and application |
| CN109499563A (en) * | 2017-09-15 | 2019-03-22 | 张家港市沐和新材料技术开发有限公司 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
| US20210296648A1 (en) * | 2016-01-14 | 2021-09-23 | Agency For Science, Technology And Research | Free-standing mof-derived hybrid porous carbon nanofiber mats |
| CN114989641A (en) * | 2022-06-23 | 2022-09-02 | 四川轻化工大学 | Modified carbon microsphere/zinc oxide hybrid and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105552334A (en) * | 2016-01-11 | 2016-05-04 | 杭州电子科技大学 | Preparation method for carbon-film-coated zinc oxide hollow sphere |
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| US20210296648A1 (en) * | 2016-01-14 | 2021-09-23 | Agency For Science, Technology And Research | Free-standing mof-derived hybrid porous carbon nanofiber mats |
| US11646418B2 (en) * | 2016-01-14 | 2023-05-09 | Agency For Science, Technology And Research | Free-standing MOF-derived hybrid porous carbon nanofiber mats |
| CN107552034A (en) * | 2017-08-21 | 2018-01-09 | 信阳师范学院 | A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet |
| CN109499563A (en) * | 2017-09-15 | 2019-03-22 | 张家港市沐和新材料技术开发有限公司 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
| CN107958995A (en) * | 2017-12-22 | 2018-04-24 | 湖南工业大学 | A kind of dried persimmon shape core shell structure C/ZnO lithium-ion negative pole electrode piece preparation methods and its fastening lithium ionic cell |
| CN108054372A (en) * | 2017-12-22 | 2018-05-18 | 湖南工业大学 | A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof |
| CN108987720A (en) * | 2018-08-01 | 2018-12-11 | 吉林大学 | Carbon/zinc oxide composite and its preparation method and application |
| CN114989641A (en) * | 2022-06-23 | 2022-09-02 | 四川轻化工大学 | Modified carbon microsphere/zinc oxide hybrid and preparation method and application thereof |
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Application publication date: 20150826 |