CN106946222A - A kind of FTO/CuO nano wires and its preparation method and application - Google Patents
A kind of FTO/CuO nano wires and its preparation method and application Download PDFInfo
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- CN106946222A CN106946222A CN201710109271.4A CN201710109271A CN106946222A CN 106946222 A CN106946222 A CN 106946222A CN 201710109271 A CN201710109271 A CN 201710109271A CN 106946222 A CN106946222 A CN 106946222A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/228—Other specific oxides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/71—Photocatalytic coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
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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
The present invention provides the preparation method of FTO/CuO nano wires, comprises the following steps：（1）Electro-conductive glass is cleaned up and dried up；（2）PVP is dissolved in deionized water, stirred to clarify, urea, sodium tartrate is sequentially added, adds copper sulphate, mixed solution is stirred to obtain, by mixed solution and step（1）Obtained electro-conductive glass is transferred to polytetrafluoroethyl-ne alkene reaction liner, is reacted 24 hours under conditions of 120 DEG C, is subsequently cooled to after room temperature, washing and drying, obtains solid membrane sample；（3）By step（2）Obtained solid membrane sample is calcined 3 hours at 550 DEG C, obtains FTO/CuO nano wires.The present invention also provides the FTO/CuO nano wires prepared using this method and application.The present invention is successfully prepared for CuO nano wires, improves the surface area and carrier concentration of CuO nano wires, and maintains the uniformity of material morphology before and after annealing, and the material is expected to be used for photolysis water hydrogen.
Description
Technical field
The present invention relates to a kind of preparation of the semi-conducting material of doping, more particularly to a kind of FTO/CuO nano wires and its system
Preparation Method and application.
Background technology
Nanostructured, is all the master that scholars further investigate all the time due to its interesting characteristic and unique application
Topic.Nanometer CuO is a kind of multifunctional material.When CuO particle sizes are small arrives nanoscale (1-100nm), its surface atom number, ratio
Surface area and surface can etc. sharply increased with the reduction of particle diameter so that show small-size effect, quantum size effect,
The features such as skin effect and macro quanta tunnel effect, with good optical property, magnetic, catalytic performance etc..But at present
The requirement expanded day by day can not have been met in many fields to the research with different-shape and the CuO materials of size and application
.In order to expand CuO performance, method that is modified or being doped with other elements is that the one kind for synthesizing CuO composites has
Effect approach, the especially doping with metallic element.Many CuO composites, CuO composites are being synthesized nearly ten years
The new chemical and physical features not available for single material can be shown, this may produce new in the application of many technologies
The performance of grain husk.In the composite, the CuO adulterated to metallic element research and applying has widely in photoelectrocatalysis field
Using.
Composite semiconductor nano material with undoped with or unmodified material compared with, due to its electricity, optics, calorifics and
Significant in mechanical property, and attracted extensive concern.With the further development of nanometer science and technology, half is combined
Conductor nano material is also extensively using the research of photoelectrochemical behaviour.
The content of the invention
The invention provides a kind of FTO/CuO nano wires and its preparation method and application, the material is expected to be used for photocatalytic water
Hydrogen manufacturing.
First purpose of the present invention is to provide the preparation method of FTO/CuO nano wires, comprises the following steps：
（1）Electro-conductive glass is cleaned up and dried up；
（2）PVP is dissolved in deionized water, stirred to clarify, urea, sodium tartrate is sequentially added, copper sulphate is added, stirred
Mixed solution is obtained, by mixed solution and step（1）Obtained electro-conductive glass is transferred to polytetrafluoroethyl-ne alkene reaction liner, at 120 DEG C
Under conditions of react 24 hours, be subsequently cooled to after room temperature, washing and drying, obtain solid membrane sample；
（3）By step（2）Obtained solid membrane sample is calcined 3 hours at 550 DEG C, obtains FTO/CuO nano wires.
Preferably, step（2）The amount ratio of middle each component is：PVP：Urea：Sodium tartrate：Copper sulphate=0.001-
0.002mol：0.03-0.04 mol：0.03-0.04 mol：0.01-0.03 mol.
As further preferred：Step（2）The amount ratio of middle each component is：PVP：Urea：Sodium tartrate：Copper sulphate=
0.002mol：0.03mol：0.03 mol：0.01 mol.
Preferably, step（2）Described in drying be 80 DEG C dry 10 hours.
Second object of the present invention is to provide a kind of FTO/CuO nano wires, is prepared using any of the above-described described method.
Third object of the present invention is to provide application of the FTO/CuO nano wires in photocatalytic water liberation of hydrogen.
Preferably, be by FTO/CuO nano wires in the electrolytic solution, using LSV technologies, in the irradiation of simulated solar irradiation
Under, carry out photocatalytic water.
The present invention is successfully prepared for CuO nano wires, improves the surface area and carrier concentration of CuO nano wires, and protect
The uniformity of the front and rear material morphology of annealing is held, the material is expected to be used for photolysis water hydrogen.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, the reality with the present invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
It for embodiment 1 is scanning electron microscope diagram of the obtained FTO/CuO nano wires of the present invention before annealing that Fig. 1, which is,；
It for embodiment 1 is the scanning electron microscope diagram of the obtained FTO/CuO nano wires of the present invention after annealing that Fig. 2, which is,；
Fig. 3 is the XRD diffraction patterns for the FTO/CuO nano wires that embodiment 1 is the present invention；
Fig. 4 is the application drawing of the photocatalytic water for the FTO/CuO nano wires that embodiment 1 is the present invention.
Embodiment
Following embodiment facilitates a better understanding of the present invention, but does not limit the present invention.Experiment in following embodiments
Method, unless otherwise specified, is conventional method.Test material used, unless otherwise specified, is city in following embodiments
Sell.
The step of preparation FTO/CuO nano wires of the present invention, is as follows：
（1）First by electro-conductive glass（FTO）The square of the cm of 2.5 cm × 1.5 size is cut into, three times are first washed with detergent, often
Secondary 20 min ultrasonic in ultrasonic wave, removes surface and oil contaminant, then respectively with distilled water and deionized water ultrasound three times, every time 20
min.Finally washed three times, dried up afterwards with nitrogen, sealing preserve is standby with absolute ethyl alcohol ultrasound.
（2）0.001-0.002mol PVP (polyvinylpyrrolidone) are dissolved in 140mL deionized waters, this solution is stirred
Mix to clarification, sequentially add 0.03-0.04 mol urea, 0.03-0.04 mol sodium tartrates, it is then slow to add 0.01-
0.03 mol copper sulphate is followed by stirring for 1 hour, then by this mixed solution and a piece of step to above solution（1）Obtained FTO
Polytetrafluoroethyl-ne alkene reaction liner is fully transferred to, is reacted 24 hours under conditions of 120 DEG C, is subsequently cooled to room temperature, deionization
After water cyclic washing, in 80 DEG C of drying in oven 10 hours, solid membrane sample is finally given.
PVP is used as a kind of synthesizing water-solubility high-molecular compound, the general aspects with water-soluble high-molecular compound, glue
Body protective effect, film forming, caking property, hygroscopicity, solubilising or cohesion.
Urea is precipitating reagent.
Sodium tartrate loses the crystallization water at 120 DEG C, and reheating is then decomposed.The smell of sugar burning is given out during calcination, its
Residue (ash content) is in strong basicity, meets acid and produces foam.
Because copper sulphate is highly soluble in water, therefore easily ionizable goes out copper ion, and due to there are alkaline gas in solution, therefore
It there occurs Cu2+ + 2NH3·H2O = Cu(OH)2↓ + 2NH4 +Then, due to being reacted 24 hours under conditions of 120 DEG C, because
This, Kocide SD dehydration ultimately produces FTO/CuO presomas.
（3）The solid membrane sample prepared is calcined 3 hours at 550 DEG C, FTO/CuO nano wires are finally given.
（4）By obtained FTO/CuO nano wires electrolyte be 0.5M Na2SO4In solution, using LSV technologies,
Under the irradiation of simulated solar irradiation, photocatalytic water is carried out.
Embodiment 1
The step of preparation FTO/CuO nano wires of the present invention, is as follows：
（1）First by electro-conductive glass（FTO）The square of the cm of 2.5 cm × 1.5 size is cut into, three times are first washed with detergent, often
Secondary 20 min ultrasonic in ultrasonic wave, removes surface and oil contaminant, then respectively with distilled water and deionized water ultrasound three times, every time 20
min.Finally washed three times, dried up afterwards with nitrogen, sealing preserve is standby with absolute ethyl alcohol ultrasound.
（2）0.002mol PVP are dissolved in 140mL deionized waters, this solution is stirred to clarify, 0.03 is added according to this
Mol urea, 0.03 mol sodium tartrates, then slowly add 0.01 mol copper sulphate to above solution, are followed by stirring for 1 small
When, then by this mixed solution and a piece of step（1）It is small that obtained FTO is fully transferred to the reaction 24 of polytetrafluoroethyl-ne alkene reaction liner
When, under conditions of 120 DEG C, it is subsequently cooled to after room temperature, deionized water cyclic washing, in 80 DEG C of drying in oven 10 hours,
Finally give solid membrane sample.Obtained solid membrane sample is scanned with SEM, Fig. 1 is as a result seen.
Fig. 1 is scanning electron microscope diagram of the obtained FTO/CuO nano wires of embodiment 1 before annealing, i.e. step 2 is obtained
The scanning electron microscope diagram of the solid membrane sample obtained.By figure we can see that one layer of uniform nano wire is grown in
FTO surface, and the size uniformity of the nano wire.
（3）The solid membrane sample prepared is calcined 3 hours at 550 DEG C, FTO/CuO nano wires are finally given.
Obtained FTO/CuO nano wires are scanned with SEM, Fig. 2 is as a result seen.
Fig. 2 is the scanning electron microscope diagram of the obtained FTO/CuO nano wires of embodiment 1 after annealing, i.e. step 3 is obtained
FTO/CuO nano wires scanning electron microscope diagram.Change is there is no for pattern before and after Tu Ke get, annealing, and
And the nanowire surface is smooth.
Fig. 3 is the XRD diffraction patterns of the FTO/CuO nano wires of embodiment 1, and its appearance and document are consistent, belong to standard
The JCPDS (801917) of card.
（4）By obtained FTO/CuO nano wires electrolyte be 0.5M Na2SO4In solution, using LSV technologies,
Under the irradiation of simulated solar irradiation, photocatalytic water is carried out.
Fig. 4 is the application drawing of the photocatalytic water of the FTO/CuO nano wires of embodiment 1, as seen from the figure, in simulated solar irradiation
Irradiation under, material oxidation copper has carried out photocatalytic water generation hydrogen and oxygen well, and thus figure can be seen that, this material can be with
Applied to photocatalytic water, this is also advantageous for utilizing solar energy, meanwhile, produce Hydrogen Energy, environmental protection and energy saving.
Embodiment 2
The step of preparation FTO/CuO nano wires of the present invention, is as follows：
（1）First by electro-conductive glass（FTO）The square of the cm of 2.5 cm × 1.5 size is cut into, three times are first washed with detergent, often
Secondary 20 min ultrasonic in ultrasonic wave, removes surface and oil contaminant, then respectively with distilled water and deionized water ultrasound three times, every time 20
min.Finally washed three times, dried up afterwards with nitrogen, sealing preserve is standby with absolute ethyl alcohol ultrasound.
（2）0.001mol PVP are dissolved in 140mL deionized waters, this solution is stirred to clarify, added according to this
0.04mol urea, 0.03 mol sodium tartrates, then slowly add 0.01 mol copper sulphate to above solution, are followed by stirring for 1
Hour, then by this mixed solution and a piece of step（1）Obtained FTO is fully transferred to polytetrafluoroethyl-ne alkene reaction liner reaction 24
Hour, under conditions of 120 DEG C, it is subsequently cooled to after room temperature, deionized water cyclic washing, it is small in 80 DEG C of drying in oven 10
When, finally give solid membrane sample.
（3）The solid membrane sample prepared is calcined 3 hours at 550 DEG C, FTO/CuO nano wires are finally given.
（4）By obtained FTO/CuO nano wires electrolyte be 0.5M Na2SO4In solution, using LSV technologies,
Under the irradiation of simulated solar irradiation, photocatalytic water is carried out.
Embodiment 3
The step of preparation FTO/CuO nano wires of the present invention, is as follows：
（1）First by electro-conductive glass（FTO）The square of the cm of 2.5 cm × 1.5 size is cut into, three times are first washed with detergent, often
Secondary 20 min ultrasonic in ultrasonic wave, removes surface and oil contaminant, then respectively with distilled water and deionized water ultrasound three times, every time 20
min.Finally washed three times, dried up afterwards with nitrogen, sealing preserve is standby with absolute ethyl alcohol ultrasound.
（2）0.001mol PVP are dissolved in 140mL deionized waters, this solution is stirred to clarify, 0.03 is sequentially added
Mol urea, 0.04 mol sodium tartrates, then slowly add 0.01 mol copper sulphate to above solution, are followed by stirring for 1 small
When, then by this mixed solution and a piece of step（1）It is small that obtained FTO is fully transferred to the reaction 24 of polytetrafluoroethyl-ne alkene reaction liner
When, under conditions of 120 DEG C, it is subsequently cooled to after room temperature, deionized water cyclic washing, in 80 DEG C of drying in oven 10 hours,
Finally give solid membrane sample.
（3）The solid membrane sample prepared is calcined 3 hours at 550 DEG C, FTO/CuO nano wires are finally given.
（4）By obtained FTO/CuO nano wires electrolyte be 0.5M Na2SO4In solution, using LSV technologies,
Under the irradiation of simulated solar irradiation, photocatalytic water is carried out.
Embodiment 4
The step of preparation FTO/CuO nano wires of the present invention, is as follows：
（1）First by electro-conductive glass（FTO）The square of the cm of 2.5 cm × 1.5 size is cut into, three times are first washed with detergent, often
Secondary 20 min ultrasonic in ultrasonic wave, removes surface and oil contaminant, then respectively with distilled water and deionized water ultrasound three times, every time 20
min.Finally washed three times, dried up afterwards with nitrogen, sealing preserve is standby with absolute ethyl alcohol ultrasound.
（2）0.001mol PVP are dissolved in 140mL deionized waters, this solution is stirred to clarify, sequentially added
0.03mol urea, 0.035 mol sodium tartrates, then slowly add 0.015 mol copper sulphate to above solution, then stir
Mix 1 hour, then by this mixed solution and a piece of step（1）It is anti-that obtained FTO is fully transferred to polytetrafluoroethyl-ne alkene reaction liner
Answer 24 hours, under conditions of 120 DEG C, be subsequently cooled to after room temperature, deionized water cyclic washing, in 80 DEG C of drying in oven 10
Hour, finally give solid membrane sample.
（3）The solid membrane sample prepared is calcined 3 hours at 550 DEG C, FTO/CuO nano wires are finally given.
（4）By obtained FTO/CuO nano wires electrolyte be 0.5M Na2SO4In solution, using LSV technologies,
Under the irradiation of simulated solar irradiation, photocatalytic water is carried out.
Embodiment 5
The step of preparation FTO/CuO nano wires of the present invention, is as follows：
（1）First by electro-conductive glass（FTO）The square of the cm of 2.5 cm × 1.5 size is cut into, three times are first washed with detergent, often
Secondary 20 min ultrasonic in ultrasonic wave, removes surface and oil contaminant, then respectively with distilled water and deionized water ultrasound three times, every time 20
min.Finally washed three times, dried up afterwards with nitrogen, sealing preserve is standby with absolute ethyl alcohol ultrasound.
（2）0.0015mol PVP are dissolved in 140mL deionized waters, this solution is stirred to clarify, added according to this
0.035mol urea, 0.03 mol sodium tartrates, then slowly add 0.03 mol copper sulphate to above solution, are followed by stirring for
1 hour, then by this mixed solution and a piece of step（1）Obtained FTO is fully transferred to the reaction of polytetrafluoroethyl-ne alkene reaction liner
24 hours, under conditions of 120 DEG C, it is subsequently cooled to after room temperature, deionized water cyclic washing, it is small in 80 DEG C of drying in oven 10
When, finally give solid membrane sample.
（3）The solid membrane sample prepared is calcined 3 hours at 550 DEG C, FTO/CuO nano wires are finally given.
（4）By obtained FTO/CuO nano wires electrolyte be 0.5M Na2SO4In solution, using LSV technologies,
Under the irradiation of simulated solar irradiation, photocatalytic water is carried out.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or to which part technical characteristic progress equivalent.
Within the spirit and principles of the invention, any modifications, equivalent substitutions and improvements made etc., should be included in the present invention's
Within protection domain.
Claims (7)
- The preparation method of 1.FTO/CuO nano wires, it is characterised in that：Comprise the following steps：（1）Electro-conductive glass is cleaned up and dried up；（2）PVP is dissolved in deionized water, stirred to clarify, urea, sodium tartrate is sequentially added, copper sulphate is added, stirred Mixed solution is obtained, by mixed solution and step（1）Obtained electro-conductive glass is transferred to polytetrafluoroethyl-ne alkene reaction liner, at 120 DEG C Under conditions of react 24 hours, be subsequently cooled to after room temperature, washing and drying, obtain solid membrane sample；（3）By step（2）Obtained solid membrane sample is calcined 3 hours at 550 DEG C, obtains FTO/CuO nano wires.
- 2. according to the method described in claim 1, it is characterised in that：Step（2）The amount ratio of middle each component is：PVP：Urea： Sodium tartrate：Copper sulphate=0.001-0.002mol：0.03-0.04 mol：0.03-0.04 mol：0.01-0.03 mol.
- 3. method according to claim 2, it is characterised in that：Step（2）The amount ratio of middle each component is：PVP：Urea： Sodium tartrate：Copper sulphate=0.002mol：0.03mol：0.03 mol：0.01 mol.
- 4. according to the method described in claim 1, it is characterised in that：Step（2）Described in drying be 80 DEG C dry 10 hours.
- 5.FTO/CuO nano wires, it is characterised in that：Usage right requires prepared by any described methods of 1-4.
- 6. application of the FTO/CuO nano wires in photocatalytic water liberation of hydrogen described in claim 5.
- 7. application according to claim 6, it is characterised in that：Be by FTO/CuO nano wires in the electrolytic solution, utilize LSV Technology, under the irradiation of simulated solar irradiation, carries out photocatalytic water.
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