CN105148925B - A kind of adjustable three-dimensional ordered macroporous ZnO Cu of Lacking oxygen2O‑TiO2Composite oxides, preparation method and applications - Google Patents
A kind of adjustable three-dimensional ordered macroporous ZnO Cu of Lacking oxygen2O‑TiO2Composite oxides, preparation method and applications Download PDFInfo
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Abstract
The invention provides a kind of adjustable three-dimensional ordered macroporous ZnO Cu of Lacking oxygen2O‑TiO2Composite oxides, preparation method and applications.Compared with prior art, the present invention is used as solvent by ethylene glycol, can effectively control the synthesis speed of the colloid, without adding any soda acid adjusting control agent, just can realize the regulation and control of plastic speed and three-dimensional ordered macroporous ZnO Cu2O‑TiO2The preparation of composite oxides.Meanwhile, there is variable valence according to copper ion, and form copper ion and zinc ion and take oxygen situation by force jointly, therefore the regulation of the ratio between the amount of substance of copper nitrate, zinc nitrate is taken, it just can conveniently realize ZnO Cu2O‑TiO2The modulation of oxygen vacancy concentration in composite oxides, so as to improve its photocatalysis performance.
Description
Technical field
The invention belongs to Photocatalysis Function Material field, and in particular to a kind of adjustable three-dimensional ordered macroporous ZnO- of Lacking oxygen
Cu2O-TiO2Composite oxides, preparation method and applications.
Background technology
Semi-conducting material, because it has special electronic structure, significant development is illustrated in fields such as the energy, environment latent
Power, is received significant attention.Among numerous semi-conducting materials, titanium oxide has green non-poisonous, cheap, property steady because of it
The characteristic such as fixed, is one of semi-conducting material of greatest concern.
It is well known that titanium dioxide has special performance in terms of light, electricity, magnetic, particularly in new energy, photocatalysis
The fields such as the depollution of environment, sensing are used widely, therefore it has immeasurable research and development value and market application.
As catalysis material, the influence of its chemical composition, microstructure to its catalytic performance is very notable.Grind recently
Study carefully display, doped chemical introduced in a semiconductor material, the generation of its Lacking oxygen being had a significant impact to photocatalysis can be promoted,
The Lacking oxygen of semiconductor catalysis material influences very notable (Science, 2011,331 (6018) on its catalytic performance:746-
750) often, there are more excellent physical and chemical properties compared with its one-component semi-conducting material.
At present, construct and use high temperature reduction or quenching technology more Lacking oxygen, not only complicated but also cost is high for operating process.Though
So having relevant report in recent years takes doping method to realize that Lacking oxygen is constructed, but due to high-temperature roasting condition, to TiO2's
Doping is often more to be existed in cupric (CuO) form, it is clear that divalent copper oxides (CuO) do not have notable photoresponse effect, right
Photocatalysis is obviously unfavorable.From current report, using monovalence cuprous oxide (Cu2) and zinc oxide (ZnO) codope in situ O
ZnO-Cu2O-TiO2Composite oxides are prepared and had not been reported.Meanwhile, porous TiO more prevailing at present2Preparation method is mostly logical
Cross the sol-gel process of pH regulation and control.But, when introducing multicomponent in the colloid preparation process, because of the multicomponent member of addition
There is objective difference in plain ionic charge attribute, the formation of colloid and the preparation of three ordered big holes is become very difficult.
The content of the invention
It is an object of the invention to provide a kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Combined oxidation
Thing, is a kind of continuous orderly, the Lacking oxygen adjustable ZnO and Cu in duct2O two-components doping ZnO-Cu2O-TiO2Combined oxidation
Thing.
Present invention also offers a kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The system of composite oxides
Preparation Method, by controlling copper source, the amount ratio in zinc source and titanium source, reaction time and temperature, realizes the modulation of Lacking oxygen, is prepared into
To ZnO-Cu2O-TiO2Composite oxides.
Present invention also offers a kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Composite oxides should
With the application in terms of photocatalytic degradation.
The adjustable three-dimensional ordered macroporous ZnO-Cu of a kind of Lacking oxygen that the present invention is provided2O-TiO2Composite oxides, are ZnO
And Cu2The composite oxides of O two-components doping, three-dimensional ordered macroporous structure, duct is continuously orderly, and macropore diameter is 150nm.
The adjustable three-dimensional ordered macroporous ZnO-Cu of a kind of Lacking oxygen that the present invention is provided2O-TiO2The preparation of composite oxides
Method, comprises the following steps：
A, at 25 DEG C, using ethylene glycol as solvent, add after copper source and zinc source, stirring and dissolving, add titanium source, sealing is stirred
Mix, obtain mixed solution；
B, by after mixed solution heat ageing obtained by step a, immerse polystyrene colloid crystal template, obtain mixture, do
Dry, roasting, obtains the adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Composite oxides.
In step a, copper source is Cu (NO3)2·3H2O, the zinc source is Zn (NO3)2·6H2O, the titanium source is titanium
Acid butyl ester.
Cu (NO in step a3)2·3H2O、Zn(NO3)2·6H2O molar concentrations in ethylene glycol are respectively 0.010~
0.029mol/L and 0.010~0.029mol/L, the volume for adding butyl titanate is the 25-40% of ethylene glycol volume.
Added in step a after butyl titanate, 3-5h is stirred in sealing.
Heat ageing described in step b, be specifically：In 30-50 DEG C of aging 3-5h.
In step b, immersed at 25 DEG C after polystyrene colloid crystal template 12-24h, obtain mixture.
In step b, the amount ratio of solution and Colloidal crystals is：0.39g colloid crystal templates are added per 3mL mixed solutions.
The preparation method of polystyrene colloid crystal template is described in step b：Particle diameter is synthesized about by emulsion polymerization
150nm polystyrene microsphere.It is specific as follows：Take 6mL styrene to be added to separatory funnel, washed with 5% sodium hydroxide until
Liquid is without pink, then it is 7 to be washed to Ph with distillation；Washed styrene is poured into three-necked flask, plus 54ml water, leads to nitrogen,
And the 70 DEG C of heating of digital display thermostat water bath are placed on, react 12 hours；The white emulsion of generation is poured into centrifuge tube after the completion of reaction
Centrifugation 12 hours, then centrifuges 12h, subsequent drying at room temperature 12-24h in centrifuge by this microballoon with 2500rpm rotating speed,
Just polystyrene colloid crystal template can be obtained.
In step b, the drying, condition is progress 12-24h dryings at 50-70 DEG C.
In step b, the roasting, condition is 500-600 DEG C of roasting temperature 3-5h.
The adjustable three-dimensional ordered macroporous ZnO-Cu of a kind of Lacking oxygen that the present invention is provided2O-TiO2The application of composite oxides,
Application in terms of photocatalytic degradation, the application especially in terms of photocatalytic degradation of methylene blue.
First, ethylene glycol is introduced as solvent, reduces titanium source contact with copper ion and zinc ion in butyl titanate
Speed, can effectively control the synthesis speed of the colloid, therefore need not introduce the regulation and control that soda acid adjusting control agent carries out plastic speed to it.Its
TiO that is secondary, being adulterated for two-component2, there is copper ion and zinc ion and take oxygen situation by force jointly, when the copper nitrate and zinc nitrate of introducing
The ratio between when changing, be used as the just respective change of the Cu oxide oxygen content with variable valence.In the process, with Cu2+/
Zn2+The change of concentration ratio, the concentration of Lacking oxygen also respective change, as a result such as the O of O 1XPS in Fig. 3 DadsContent and OlattContent
The ratio between shown in.In addition, with Cu2+/Zn2+The change of concentration ratio, closely related bandwidth is also significantly affected with semiconductor,
As a result as shown in Figure 4 B.
Compared with prior art, the present invention is used as solvent by ethylene glycol, can effectively control the synthesis speed of the colloid, nothing
Any soda acid adjusting control agent need to be added, the regulation and control of plastic speed and three-dimensional ordered macroporous ZnO-Cu just can be realized2O-TiO2Combined oxidation
The preparation of thing.Meanwhile, there is variable valence according to copper ion, and form copper ion and zinc ion and take oxygen situation by force jointly, therefore take
The regulation of the ratio between copper nitrate, the amount of substance of zinc nitrate, just can easily realize ZnO-Cu2O-TiO2Lacking oxygen in composite oxides
The modulation of concentration, so as to improve its photocatalysis performance.
Brief description of the drawings
Figure 1A is ZnO-Cu prepared by embodiment 12O-TiO2The SEM figures of composite oxides；
Figure 1B is ZnO-Cu prepared by embodiment 22O-TiO2The SEM figures of composite oxides；
Fig. 1 C are ZnO-Cu prepared by embodiment 32O-TiO2The SEM figures of composite oxides；
Fig. 2 is ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The XRD of composite oxides；A is the XRD of embodiment 1
Figure；B is the XRD of embodiment 2；C is the XRD of embodiment 3；
Fig. 3 A are ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The Zn 2p XPS figures of composite oxides；Wherein：A is
Sample prepared by embodiment 1；B is sample prepared by embodiment 2；C is sample prepared by embodiment 3；
Fig. 3 B are ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The Cu 2p figures of composite oxides；Wherein：A is implementation
Sample prepared by example 1；B is sample prepared by embodiment 2；C is sample prepared by embodiment 3；
Fig. 3 C are ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The Ti 2P of composite oxides XPS figures；Wherein：a
The sample prepared for embodiment 1；B is sample prepared by embodiment 2；C is sample prepared by embodiment 3；
Fig. 3 D are ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The O 1s of composite oxides XPS figures；Wherein：A is
Sample prepared by embodiment 1；B is sample prepared by embodiment 2；C is sample prepared by embodiment 3；
Fig. 4 A are ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The UV-vis DRS of composite oxides absorbs light
Spectrum is wherein：A is sample prepared by embodiment 1；B is sample prepared by embodiment 2；C is sample prepared by embodiment 3；
Fig. 4 B are ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The bandwidth figure of composite oxides；Wherein：A is embodiment
1 sample prepared；B is sample prepared by embodiment 2；C is sample prepared by embodiment 3；
Fig. 5 is ZnO-Cu prepared by embodiment 1,2 and 32O-TiO2The Photocatalytic Degradation Property figure of composite oxides；A is real
Apply the Photocatalytic Degradation Property figure of example 1；B is the Photocatalytic Degradation Property figure of embodiment 2；C is the photocatalytic degradation of embodiment 3
Performance map；D be undoped with TiO2(preparation method is similar to embodiment 1,2,3) Photocatalytic Degradation Property figure.
Embodiment
Below by embodiment, the invention will be further described.
Embodiment 1
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Cu in composite oxides, middle preparation process
(NO3)2·3H2O and Zn (NO3)2·6H2O molar concentrations in ethylene glycol are respectively 0.010mol/L, 0.029mol/L.
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The preparation method of composite oxides, including it is following
Step：
A, at 25 DEG C, 0.207mmol Cu (NO are added in 20mL ethylene glycol3)2·3H2O and 0.571mmol Zn
(NO3)2·6H2O magnetic agitations dissolve, and are subsequently added 6.8mL butyl titanates and continue to stir 5h with preservative film sealing；
B and then resulting solution is moved into 40 DEG C of water-bath carry out aging 3h, subsequent polystyrene colloid crystal template leaching
Enter in this solution, after 24h, 12h dryings are carried out at 70 DEG C to the mixture；Then to it in 600 DEG C of roasting temperature 3h,
Three-dimensional ordered macroporous ZnO-Cu can be obtained2O-TiO2Composite oxides.
The SEM of synthesized compound is characterized as shown in Figure 1A；As the XRD crystal formations shown in a in Fig. 2 and Fig. 3 A XPS
A is understood in a in figure, Fig. 3 B XPS figures, and synthesized product is ZnO-Cu2O-TiO2Composite oxides；The a institutes in Fig. 3 DXPS figures
Show that O1s XPS analysis understand that synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.15), correspondence compared with
Low oxygen vacancy concentration.
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The application of composite oxides, in photocatalytic degradation
The application of aspect；
Concrete application method is：
Weigh the ZnO-Cu prepared by embodiment 12O-TiO2Composite oxides 50mg is placed in quartz ampoule, is subsequently added
10mg/L methylene blue solution 100mL, quartz ampoule is moved into darkroom and placed 1 hour, 500W xenon sources are then put in
Light-catalyzed reaction instrument in, to methylene blue carry out photocatalytic degradation, every 1 hour analysis catalytic performance.
A is catalytic performance result in Fig. 5, the visible synthesized ZnO-Cu of a in Fig. 52O-TiO2Composite oxides are small 5
When interior realize the photocatalytic degradation efficiency to methylene blue 69%.
Embodiment 2
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Cu in composite oxides, wherein preparation process
(NO3)2·3H2O and Zn (NO3)2·6H2O molar concentrations in ethylene glycol are respectively 0.019mol/L, 0.018mol/L.
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The preparation method of composite oxides, including it is following
Step：
A, 25 DEG C of addition 0.373mmol Cu (NO in 20mL ethylene glycol3)2·3H2O and 0.369mmol Zn
(NO3)2·6H2O magnetic agitations dissolve, and are subsequently added 6.8mL butyl titanates and continue to stir 5h with preservative film sealing；
B and then resulting solution is moved into aging 5h is carried out in 30 DEG C of water-bath.Subsequent colloid crystal template immerses this solution
In, after 24h, 20h dryings are carried out at 60 DEG C to the mixture.Then to it in 550 DEG C of roasting temperature 5h, you can obtain three-dimensional
Ordered big hole ZnO-Cu2O-TiO2Composite oxides.
The SEM of synthesized compound is characterized as shown in Figure 1B；As the XRD crystal formations shown in b in Fig. 2 and Fig. 3 A XPS
B is understood in b in figure, Fig. 3 B XPS figures, and synthesized product is ZnO-Cu2O-TiO2Composite oxides；The b institutes in Fig. 3 DXPS figures
Show that O1s XPS analysis understand that synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.19), correspondence phase
To high oxygen vacancy concentration.
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The application of composite oxides, in photocatalytic degradation
The application of aspect.
Concrete application method is：
Weigh prepared ZnO-Cu2O-TiO2Composite oxides 50mg is placed in quartz ampoule, is subsequently added 10mg/L methylenes
Base indigo plant solution 100mL, quartz ampoule is moved into darkroom and placed 1 hour, the photocatalysis for being then put in 500W xenon sources is anti-
Ying Yizhong, photocatalytic degradation, the catalytic performance of analysis in every 1 hour are carried out to methylene blue.
B is catalytic performance result in Fig. 5, the visible synthesized ZnO-Cu of b in Fig. 52O-TiO2Composite oxides are small 5
When interior realize the photocatalytic degradation efficiency to methylene blue 97%.
Embodiment 3
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Cu in composite oxides, wherein preparation process
(NO3)2·3H2O and Zn (NO3)2·6H2O molar concentrations in ethylene glycol are respectively 0.029mol/L, 0.010mol/L.
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The preparation method of composite oxides, including it is following
Step：
A, 25 DEG C of addition 0.573mmol Cu (NO in 20mL ethylene glycol3)2·3H2O and 0.204mmol Zn
(NO3)2·6H2O magnetic agitations dissolve, and are subsequently added 6.8mL butyl titanates and continue to stir 5h with preservative film sealing；
B and then resulting solution is moved into aging 3h is carried out in 50 DEG C of water-bath.Subsequent colloid crystal template immerses this solution
In, after 24h, 24h dryings are carried out at 50 DEG C to the mixture.Then to it in 500 DEG C of roasting temperature 3h, you can obtain three-dimensional
Ordered big hole ZnO-Cu2O-TiO2Composite oxides.
The SEM of synthesized compound is characterized as shown in Figure 1 C；As the XRD crystal formations shown in c in Fig. 2 and Fig. 3 A XPS
C is understood in c in figure, Fig. 3 B XPS figures, and synthesized product is ZnO-Cu2O-TiO2Composite oxides；The c in Fig. 3 D XPS figures
Shown O1s XPS analysis understand that synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.27), correspondence
Relatively high oxygen vacancy concentration.
A kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The application of composite oxides, in photocatalytic degradation
The application of aspect.
Concrete application method is：
Weigh the ZnO-Cu prepared by embodiment 32O-TiO2Composite oxides 50mg is placed in quartz ampoule, is subsequently added
10mg/L methylene blue solution 100mL, quartz ampoule is moved into darkroom and placed 1 hour, 500W xenon sources are then put in
Light-catalyzed reaction instrument in, to methylene blue carry out photocatalytic degradation, every 1 hour analysis catalytic performance.
C is catalytic performance result in Fig. 5, the visible synthesized ZnO-Cu of c in Fig. 52O-TiO2Composite oxides are small 5
When interior realize the photocatalytic degradation efficiency to methylene blue 100%.
D is visible in a~c and Fig. 5 in comparison diagram 5, and adulterate ZnO-Cu2O-TiO2Relative to undoped with TiO2, present more
Good catalytic performance.
Claims (7)
1. a kind of adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2The preparation method of composite oxides, its feature exists
In the preparation method comprises the following steps：
A, at 25 DEG C, using ethylene glycol as solvent, add after copper source and zinc source, stirring and dissolving, add titanium source, seal, stirring is obtained
To mixed solution；
B, by after mixed solution heat ageing obtained by step a, immerse polystyrene colloid crystal template, obtain mixture, dry, roasting
Burn, obtain the adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen2O-TiO2Composite oxides;
In step a, copper source is Cu (NO3)2·3H2O, the zinc source is Zn (NO3)2·6H2O, the titanium source is metatitanic acid fourth
Ester;
Cu (NO in step a3)2·3H2O、Zn(NO3)2·6H2O molar concentrations in ethylene glycol are respectively 0.010 ~ 0.029
Mol/L and 0.010 ~ 0.029 mol/L, the volume for adding butyl titanate is the 25-40% of ethylene glycol volume;
The adjustable three-dimensional ordered macroporous ZnO-Cu of prepared Lacking oxygen2O-TiO2Composite oxides are ZnO and Cu2O two-components are mixed
Miscellaneous composite oxides, three-dimensional ordered macroporous structure, duct is continuously orderly, and macropore diameter is 150 nm.
2. preparation method according to claim 1, it is characterised in that added in step a after butyl titanate, is sealed, stirring
3-5h。
3. preparation method according to claim 1, it is characterised in that heat ageing described in step b, is specifically：30-50℃
Aging 3-5h.
4. preparation method according to claim 1, it is characterised in that in step b, immerses polystyrene colloid crystal template
12-24h。
5. preparation method according to claim 1, it is characterised in that in step b, the roasting, condition is 500-600 DEG C
Roasting temperature 3-5h.
6. the adjustable three-dimensional ordered macroporous ZnO-Cu of Lacking oxygen prepared by a kind of any one of claim 1-52O-TiO2Composite oxygen
The application of compound, it is characterised in that the application in terms of photocatalytic degradation.
7. application according to claim 6, it is characterised in that the application in terms of photocatalytic degradation of methylene blue.
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| CN107694559B (en) * | 2017-10-12 | 2020-02-21 | 安徽工程大学 | Zinc-manganese oxide-manganic manganous oxide composite oxide with adjustable oxygen vacancy as well as preparation method and application thereof |
| CN107973339B (en) * | 2017-11-24 | 2020-04-21 | 武汉理工大学 | Three-dimensional ordered macroporous calcium titanate photonic crystal constructed by porous nanosheets and synthetic method thereof |
| CN109395745B (en) * | 2018-12-03 | 2021-10-15 | 安徽工程大学 | Oxygen vacancy adjustable high-energy structure copper sulfide-cuprous oxide compound and preparation method and application thereof |
| CN110102248A (en) * | 2019-06-21 | 2019-08-09 | 清华大学 | A kind of surface oxygen defect porous metal oxide material and its preparation and application |
| CN113540390B (en) * | 2021-06-29 | 2022-04-01 | 哈尔滨工业大学 | Preparation method and application of dynamic interface coating of metal zinc cathode of zinc ion battery |
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