CN105126855B - ZnO/ZnFe2O4/ C nano structure hollow ball and preparation method thereof - Google Patents
ZnO/ZnFe2O4/ C nano structure hollow ball and preparation method thereof Download PDFInfo
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- CN105126855B CN105126855B CN201510412673.2A CN201510412673A CN105126855B CN 105126855 B CN105126855 B CN 105126855B CN 201510412673 A CN201510412673 A CN 201510412673A CN 105126855 B CN105126855 B CN 105126855B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A kind of ZnO/ZnFe disclosed by the invention2O4/ C nano structure hollow ball, the spherical shell of the hollow ball are followed successively by ZnO/ZnFe from inside to outside2O4Layer and C layer, often layer thickness at 10 nanometers or less.The present invention utilize template adsorption method, by stepwise adsorption and subsequent hydro-thermal and annealing and etc. ZnO/ZnFe is prepared2O4/ C nano hollow ball structure.ZnO/ZnFe prepared by the present invention2O4/ C nano hollow ball structure nucleocapsid is regular, and can regulate and control per layer thickness, ZnO and ZnFe2O4Crystallite dimension at 6 ~ 10 nanometers, crystal property is good, and specific surface area be more than 200 m2/g.Method of the invention is simple, cost is relatively low, is conducive to industrialized production, has good application in lithium ion battery, ultracapacitor, gas sensing and photocatalytic hydrogen production by water decomposition etc..
Description
Technical field
The present invention relates to a kind of nano-hollow ball and preparation method thereof more particularly to a kind of ZnO/ZnFe2O4/ C nano structure
Hollow ball and preparation method thereof.
Background technology
The increasingly exhausted crisis of the energy such as facing mankind coal, oil, finds new alternative energy source and has obtained the weight of various countries
Depending on.Solar energy is inexhaustible, the nexhaustible energy, scientists also for solar energy be transformed into storable electric energy,
Chemical energy and effort.Photocatalytic hydrogen production by water decomposition is the preferred approach of solar energy chemical conversion, because Hydrogen Energy is as secondary energy
Source has the advantages that other energy such as cleaning, safe efficient are incomparable.Climate change, fuel cell technology and increasingly prominent
The environmental problem gone out has pushed the generation of " hydrogen economy ", replaces existing energy supply that will become people with hydrogen substitution or part
The direction that class is made great efforts.Currently, fossil fuel hydrogen manufacturing is industrial main path, it is by changing that, which there is 95% or more hydrogen in the whole world,
Stone fuel making.Although fossil resource hydrogen manufacturing prior art is ripe, production cost is relatively low, and resource is limited and can not be again
It is raw, while obtaining hydrogen, a large amount of GHG carbon dioxide is discharged into air, and resource will be faced with fossil resource hydrogen manufacturing
The two fold problem of shortage and environmental degradation.In the long run, this needs for not meeting sustainable development.Therefore, using can be again
Raw energy hydrogen manufacturing from non-fossil fuel, including biological hydrogen production, solar energy photocatalytic decomposing hydrogen-production and renewable energy power generation electricity
Water hydrogen manufacturing is solved, is one of the effective way for solving national energy security and environmental problem, wherein being decomposed using solar energy photocatalytic
Water hydrogen manufacturing has caused the extensive attention of countries in the world in recent years.
In semi-conducting material photocatalytic system, zinc oxide（ZnO）Because of the high, electron transfer rate with photocatalytic activity
Soon, the advantages that nontoxic, cheap is considered as very promising catalysis material.But due to zinc oxide（ZnO）It is interior
Portion's defect and intrinsic compound reason so that photo-generate electron-hole after generation, has the photo-generate electron-hole close to 90% directly to exist
Inside semiconductor and surface pairings are compound, rather than are acted on water and pollutant.Which results in most of photoproduction electricity
The waste in sub- hole greatly limits the utilization to solar energy.Therefore, the separation for promoting light induced electron and hole inhibits it multiple
It closes, to improve quantum efficiency, to make full use of solar energy, the stability for improving photochemical catalyst is modern photocatalysis field
Key problem.Currently, there is the modification technology of several common semiconductor light-catalysts, include mainly doped transition metal ions and
Semiconductor light-catalyst it is compound etc..First two is due to the use of many yttriums among this, so receiving cost
With the limitation of resource reserve.It is because of composite material that composite photocatalyst material has excellent performance than single catalysis material
Hetero-junctions can generally be formed.Hetero-junctions is usually combined by two different semi-conducting materials by heteroepitaxial growth, because
Its internal generation can promote the built in field that electron hole detaches, so having uniqueness on promoting photo-generate electron-hole separation
Physicochemical property.Zinc ferrite（ZnFe2O4）With quality fine paper bottom and excellent photocatalytic activity, can be formed with zinc oxide very well
Type-Heterojunction structure can effectively realize efficiently separating for photo-generate electron-hole, to improve photocatalysis efficiency.
In addition, in recent years the study found that by amorphous carbon with catalysis material is compound can effectively improve photocatalysis material
The photocatalysis efficiency of material under visible light.
But up to the present, the ZnO/ZnFe that prepared by people2O4Hetero-junctions is in micron level, although can improve
The separation of light induced electron vacancy pair, but due to being far smaller than the size of the material, most of light with the size of hetero-junctions
Raw electronics vacancy pair still can be compound in vivo, therefore we need the urgent hetero-junctions for preparing nano-scale, especially
Hetero-junctions less than 10 nanometers further increases the separation of light induced electron vacancy pair.
Invention content
The object of the present invention is to provide a kind of large specific surface area, photocatalysis efficiency height and the simple ZnO/ of preparation method
ZnFe2O4/ C nano structure hollow ball and preparation method thereof.
The ZnO/ZnFe of the present invention2O4/ C nano structure hollow ball, the spherical shell of the hollow ball are followed successively by ZnO/ from inside to outside
ZnFe2O4Layer and amorphous carbon layer, per layer thickness at 10 nanometers or less；ZnO/ZnFe2O4ZnO crystal grain and ZnFe in layer2O4It is brilliant
Nano heterojunction, ZnO and ZnFe are formed between grain2O4Crystallite dimension at 6 ~ 10 nanometers, the hollow ball a diameter of 80~
600 nanometers.
Prepare above-mentioned ZnO/ZnFe2O4The method of/C nano structure hollow ball, includes the following steps：
1）Adsorb Zn ions：Zinc nitrate is added to DMF（N,N-dimethylformamide）In, preparing Zn ion concentrations is
Surface there is the spherical template of carboxyl and hydroxyl to be added in above-mentioned solution, makes ball by the Zn ionic adsorption liquid of 0.01~0.1M
Shape template content is 5g/L ~ 50g/L, and ultrasonic 0.5h ~ 1h keeps spherical template fully dispersed, filtered after 12 ~ 36h of stirring and adsorbing, and
It is washed with ethyl alcohol, the sample of acquisition is placed in 50~90 DEG C of baking ovens later, dry 6~for 24 hours；Spherical template described above is
Carbon ball, PS balls or SiO2Ball；
2）Adsorb Fe ions：Ferric nitrate is added in DMF, the Fe ions that Fe ion concentrations are 0.001~0.01M are prepared
Adsorption liquid, by step 1）Sample after middle drying is added in Fe ionic adsorption liquid, and ultrasonic 0.5h ~ 1h keeps its fully dispersed, stirs
It is centrifuged after mixing 4 ~ 12h of absorption, ethyl alcohol is used in combination to wash, the sample of acquisition is placed in 50~90 DEG C of baking ovens later, dry 6~for 24 hours；
3）Remove removing template：By step 2）Sample after middle drying is heat-treated 6~48h at 400~600 DEG C in air,
To remove carbon ball template or PS ball templates, ZnO/ZnFe is obtained2O4Nanostructure hollow ball；Or by step 2）In be dried to obtain
Sample be heat-treated 6~48h in air at 400~600 DEG C after, then immerse a concentration of 1~20M's at 60~100 DEG C
In NaOH solution keep 1~for 24 hours, to remove SiO2Ball template obtains ZnO/ZnFe2O4Two layers of nanostructure hollow ball；
4）Add amorphous carbon layer：By 10 ~ 50mg steps 3）Obtained ZnO/ZnFe2O4Nanostructure hollow ball is added
Into the glucose solution of a concentration of 0.01 ~ 0.5M of 10 ~ 30mL, ultrasonic 0.5h ~ 1h keeps its fully dispersed, is heated to 60 later
~ 100 DEG C, under stirring conditions, water is volatilized dry, obtained product is heated to 400~600 under the protection of inert gas
DEG C, and 6~48h is kept the temperature, obtain ZnO/ZnFe2O4/ C nano structure hollow ball.
In the present invention, there is the preparation method of the spherical template of carboxyl and hydroxyl can refer to Sun, X. on the surface;
Li, Y., Angewandte Chemie International Edition 2004,43 (29), 3827-3831、Lou,
X. W.; Archer, L. A.; Yang, Z., Advanced Materials 2008,20(21), 3987-4019 with
And Wang, D.; Hisatomi, T.; Takata, T.; Pan, C.; Katayama, M.; Kubota, J.;
Domen, K., Angewandte Chemie International Edition 2013,52 (43), 11252-11256.
In the present invention, using template, Zn ions are first adsorbed, adsorb Fe ions again later, removing template is removed in heat treatment
Meanwhile zinc oxide and iron oxide can generate zinc ferrite, and the zinc ferrite for reacting remaining zinc oxide and generation be formed it is heterogeneous
Knot.Later again in ZnO/ZnFe2O4The surface of nanostructure hollow ball deposits one layer of glucose, under the protection of inert gas, heat
Processing glucose will become amorphous carbon, to obtain ZnO/ZnFe2O4/ C nano structure hollow ball.
The beneficial effects of the present invention are：The ZnO/ZnFe of the present invention2O4/ C nano structure hollow ball, by ZnO/ZnFe2O4
Layer and C layers of close composition, every layer of thickness is all at 10 nanometers hereinafter, a diameter of 80~600 nanometers of hollow ball, ZnO and ZnFe2O4
Crystallite dimension at 6 ~ 10 nanometers, amorphous carbon layer can be used as electron transfer layer and protective layer, hollow ball crystallinity of the invention
Can be good, and specific surface area is more than 200 m2/g.Method of the invention is simple, cost is relatively low, realizes ZnO, ZnFe2O4With having for C
It imitates compound, avoids the compound of light induced electron and hole, be conducive to the separation in light induced electron and hole, to improve the light of material
Catalytic performance.Meanwhile the material can be additionally used in lithium ion battery, gas catalysis and gas sensing, and it is correspondingly improved its property
Energy.
Description of the drawings
Fig. 1 is ZnO/ZnFe2O4The XRD diffraction pictures of nanostructure hollow ball.
Fig. 2 is ZnO/ZnFe2O4The SEM pictures of/C nano structure hollow ball.
Fig. 3 is ZnO/ZnFe2O4The TEM pictures of/C nano structure hollow ball.
Fig. 4 is ZnO/ZnFe2O4The N of/C nano structure hollow ball2Adsorption-desorption curve.
Fig. 5 is ZnO/ZnFe2O4The photocatalysis performance figure of/C nano structure hollow ball.
Specific implementation mode
Embodiment 1
（1）2.97g zinc nitrate hexahydrates are added in the n,N-Dimethylformamide of 100 mL, prepare a concentration of 0.1M
Zn ions solution.5g carbon balls are added in above-mentioned solution, ultrasonic 1h keeps carbon ball fully dispersed, is taken out after stirring and adsorbing 36h
Filter, is used in combination ethyl alcohol to wash twice, the sample of acquisition is placed in 90 DEG C of baking ovens later, and drying is for 24 hours；
（2）Nine water ferric nitrates of 0.404g are added in the n,N-Dimethylformamide of 100 mL, a concentration of 0.01M is prepared
Fe ions solution.By step（1）The sample obtained after middle drying is added in above-mentioned solution, and ultrasonic 1h makes it fully divide
It dissipates, is centrifuged after stirring and adsorbing 12h, ethyl alcohol is used in combination to wash twice, the sample of acquisition is placed in 90 DEG C later, drying is for 24 hours；
（3）By step（2）The sample obtained after middle drying is heat-treated 48h at 600 DEG C in air, to remove carbon ball mould
Plate, while obtaining ZnO/ZnFe2O4Nanostructure hollow ball；Its XRD spectrum is as shown in Figure 1；
（4）By step（3）In the obtained ZnO/ZnFe of 50mg2O4It is a concentration of that nanostructure hollow ball is added to 30mL
In the glucose solution of 0.5M, ultrasonic 1h keeps its fully dispersed, is heated to 100 DEG C later, and under stirring conditions, water is waved
It is dry.Finally obtained product is heated to 600 DEG C under the protection of inert gas, and keeps the temperature 48h, you can obtains ZnO/
ZnFe2O4/ C nano structure hollow ball.
ZnO/ZnFe made from this example2O4/ C nano structure hollow ball is by ZnO/ZnFe2O4Layer and C layers of close composition, it is every
The thickness of layer spherical shell is all at 10 nanometers hereinafter, a diameter of 80~600 nanometers of hollow ball, ZnO and ZnFe2O4Average grain size
In 6 rans, crystal property is good, and SEM and TEM are as shown in Figure 2,3, N2Adsorption-desorption curve is as shown in figure 4, can be with
Find out that the hollow ball specific surface area is more than 200 m2/g.Fig. 5 is the hollow ball structure and pure ZnO, pure ZnFe2O4The light of hollow ball
Catalytic performance comparison diagram, it can be seen that the hollow ball photocatalysis performance of structure of the invention is apparently higher than other two structure.
Embodiment 2
（1）0.297g zinc nitrate hexahydrates are added in the n,N-Dimethylformamide of 100 mL, are prepared a concentration of
The solution of the Zn ions of 0.01M.0.5gPS balls are added in above-mentioned solution, ultrasonic 0.5h keeps PS balls fully dispersed, and stirring is inhaled
It is filtered after attached 12h, ethyl alcohol is used in combination to wash twice, the sample of acquisition is placed in 50 DEG C of baking ovens later, dry 6h；
（2）Nine water ferric nitrates of 0.0404g are added in the n,N-Dimethylformamide of 100 mL, are prepared a concentration of
The solution of the Fe ions of 0.001M.By step（1）The sample obtained after middle drying is added in above-mentioned solution, and ultrasonic 0.5h makes it
It is fully dispersed, it is centrifuged after stirring and adsorbing 4h, ethyl alcohol is used in combination to wash twice, the sample of acquisition is placed in 50 DEG C later, dry 6h；
（3）By step（2）The sample obtained after middle drying is heat-treated 6h at 400 DEG C in air, to remove PS ball moulds
Plate, while obtaining ZnO/ZnFe2O4Nanostructure hollow ball；
（4）By step（3）In the obtained ZnO/ZnFe of 10mg2O4It is a concentration of that nanostructure hollow ball is added to 10mL
In the glucose solution of 0.01M, ultrasonic 0.5h keeps its fully dispersed, is heated to 60 DEG C later, under stirring conditions, by water
Volatilization is dry.Finally obtained product is heated to 400 DEG C under the protection of inert gas, and keeps the temperature 6h, you can obtains ZnO/
ZnFe2O4/ C nano structure hollow ball.
Embodiment 3
（1）1.485g zinc nitrate hexahydrates are added in the n,N-Dimethylformamide of 100 mL, are prepared a concentration of
The solution of the Zn ions of 0.05M.By 3g SiO2Ball is added in above-mentioned solution, and ultrasonic 0.75h makes SiO2Ball is fully dispersed, stirring
Absorption filters afterwards for 24 hours, is used in combination ethyl alcohol to wash twice, the sample of acquisition is placed in 70 DEG C of baking ovens later, dry 18h；
（2）Nine water ferric nitrates of 0.202g are added in the n,N-Dimethylformamide of 100 mL, are prepared a concentration of
The solution of the Fe ions of 0.005M.By step（1）The sample obtained after middle drying is added in above-mentioned solution, and ultrasonic 0.75h makes
Its is fully dispersed, is centrifuged after stirring and adsorbing 8h, ethyl alcohol is used in combination to wash twice, and the sample of acquisition is placed in 70 DEG C later, drying
18h；
（3）By step（2）The sample obtained after middle drying is heat-treated 28h at 500 DEG C in air, immerses again later dense
12h is kept in the NaOH solution that degree is 10M, to remove SiO2Ball template, while obtaining ZnO/ZnFe2O4Nanostructure hollow ball；
（4）By step（3）In the obtained ZnO/ZnFe of 30mg2O4It is a concentration of that nanostructure hollow ball is added to 20mL
In the glucose solution of 0.2M, ultrasonic 0.75h keeps its fully dispersed, is heated to 80 DEG C later, under stirring conditions, by water
Volatilization is dry.Finally obtained product is heated to 500 DEG C under the protection of inert gas, and keeps the temperature 12h, you can obtains ZnO/
ZnFe2O4/ C nano structure hollow ball.
Claims (3)
1. a kind of ZnO/ZnFe2O4/ C nano structure hollow ball, it is characterised in that the spherical shell of the hollow ball is followed successively by from inside to outside
ZnO/ZnFe2O4Layer and amorphous carbon layer, per layer thickness at 10 nanometers or less；ZnO/ZnFe2O4Layer in ZnO crystal grain with
ZnFe2O4Nano heterojunction, ZnO and ZnFe are formed between crystal grain2O4Crystallite dimension at 6 ~ 10 nanometers, the hollow ball
A diameter of 80~600 nanometers；The hollow ball is made with the following method：Using template, first adsorb Zn ions, then adsorb Fe from
Son, while removing template is removed in heat treatment, zinc oxide and iron oxide generate zinc ferrite, react remaining zinc oxide and the iron of generation
Sour zinc forms hetero-junctions；Again in ZnO/ZnFe2O4Hetero-junctions surface deposits one layer of glucose, under the protection of inert gas, at heat
It manages glucose and forms amorphous carbon, to obtain ZnO/ZnFe2O4/ C nano structure hollow ball.
2. preparing ZnO/ZnFe as described in claim 12O4The method of/C nano structure hollow ball, it is characterised in that including such as
Lower step：
1）Adsorb Zn ions：Zinc nitrate is added in DMF, the Zn ionic adsorptions that Zn ion concentrations are 0.01~0.1M are prepared
Surface there is the spherical template of carboxyl and hydroxyl to be added in above-mentioned solution by liquid, and it is 5g/L ~ 50g/L to make spherical template content,
Ultrasonic 0.5h ~ 1h keeps spherical template fully dispersed, is filtered after 12 ~ 36h of stirring and adsorbing, ethyl alcohol is used in combination to wash, later by acquisition
Sample is placed in 50~90 DEG C of baking ovens, dry 6~for 24 hours；Spherical template described above is carbon ball, PS balls or SiO2Ball；
2）Adsorb Fe ions：Ferric nitrate is added in DMF, the Fe ionic adsorptions that Fe ion concentrations are 0.001~0.01M are prepared
Liquid, by step 1）Sample after middle drying is added in Fe ionic adsorption liquid, and ultrasonic 0.5h ~ 1h keeps its fully dispersed, and stirring is inhaled
It is centrifuged after attached 4 ~ 12h, ethyl alcohol is used in combination to wash, the sample of acquisition is placed in 50~90 DEG C of baking ovens later, dry 6~for 24 hours；
3）Remove removing template：By step 2）Sample after middle drying is heat-treated 6~48h at 400~600 DEG C in air, to go
Except carbon ball template or PS ball templates, ZnO/ZnFe is obtained2O4Nanostructure hollow ball；Or by step 2）In the sample that is dried to obtain
After product are heat-treated 6~48h at 400~600 DEG C in air, then immerse at 60~100 DEG C the NaOH of a concentration of 1~20M
In solution keep 1~for 24 hours, to remove SiO2Ball template obtains ZnO/ZnFe2O4Two layers of nanostructure hollow ball；
4）Add amorphous carbon layer：By 10 ~ 50mg steps 3）Obtained ZnO/ZnFe2O4Nanostructure hollow ball is added to 10 ~
In the glucose solution of a concentration of 0.01 ~ 0.5M of 30mL, ultrasonic 0.5h ~ 1h keeps its fully dispersed, is heated to 60 ~ 100 later
DEG C, under stirring conditions, water is volatilized dry, obtained product is heated to 400~600 DEG C under the protection of inert gas,
And 6~48h is kept the temperature, obtain ZnO/ZnFe2O4/ C nano structure hollow ball.
3. a kind of ZnO/ZnFe as described in claim 12O4The purposes of/C nano structure hollow ball, it is characterised in that the nanometer
Hollow ball can be used for lithium ion battery, gas catalysis, photocatalytic hydrogen production by water decomposition, photocatalytic pollutant degradation or gas sensing
In.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105664950B (en) * | 2016-01-04 | 2018-05-15 | 南京林业大学 | A kind of porous nano ZnFe2O4Preparation method |
| CN105712393B (en) * | 2016-03-21 | 2017-04-19 | 西北工业大学 | Method for preparing zinc-oxide/simple-substance-carbon core-shell structure |
| CN106311248B (en) * | 2016-08-15 | 2019-02-22 | 浙江师范大学 | A kind of zinc ferrite/carbon/zinc oxide nanometer composite material and its method of preparation |
| CN107224972A (en) * | 2017-07-26 | 2017-10-03 | 齐齐哈尔大学 | Flower ball-shaped structure ZnO/ZnWO4The synthetic method of photochemical catalyst |
| CN109399725B (en) * | 2017-08-15 | 2021-04-13 | 中国石油化工股份有限公司 | Preparation method and application of zinc ferrite-containing nano-structure array |
| CN108598414B (en) * | 2018-04-23 | 2021-02-26 | 复旦大学 | Amorphous zinc oxide/carbon composite lithium ion battery cathode material and preparation method thereof |
| CN108772095A (en) * | 2018-07-13 | 2018-11-09 | 中国计量大学 | A kind of preparation method of efficient degradation antibiotic visible light catalytic composite material |
| CN111847526B (en) * | 2020-07-29 | 2021-04-23 | 十堰浩达新能源科技有限公司 | High-capacity super capacitor |
| CN116328777B (en) * | 2023-03-17 | 2024-04-19 | 西安交通大学 | Preparation method of magnetic zinc oxide@zinc ferrite photocatalyst |
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| CN101759146A (en) * | 2010-01-20 | 2010-06-30 | 浙江师范大学 | Method for preparing ZnO/ZnFe2O4 compound nano hollow sphere |
| CN102208637A (en) * | 2010-11-09 | 2011-10-05 | 广州市香港科大***研究院 | ZnFe2O4/C composite cathode material with hollow sphere structure and one-step preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101759146A (en) * | 2010-01-20 | 2010-06-30 | 浙江师范大学 | Method for preparing ZnO/ZnFe2O4 compound nano hollow sphere |
| CN102208637A (en) * | 2010-11-09 | 2011-10-05 | 广州市香港科大***研究院 | ZnFe2O4/C composite cathode material with hollow sphere structure and one-step preparation method thereof |
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