CN106868540A - A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver - Google Patents
A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver Download PDFInfo
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- CN106868540A CN106868540A CN201710079014.0A CN201710079014A CN106868540A CN 106868540 A CN106868540 A CN 106868540A CN 201710079014 A CN201710079014 A CN 201710079014A CN 106868540 A CN106868540 A CN 106868540A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
Abstract
The invention discloses a kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver, specifically implement according to following steps：Step 1, prepares Cu2O films；Step 2, the Cu that will be prepared in step 12Reacted in O films immersion silver nitrate solution, obtained the nanometer Cu of metal modified by silver2O catalysis materials.The nanometer Cu containing metal modified by silver prepared using a kind of preparation method of nano cuprous oxide catalysis material based on modified by silver of the invention2O films, its stability is higher, and recycling rate of waterused is also high.
Description
Technical field
The invention belongs to catalysis material preparation method technical field, it is related to a kind of nano cuprous oxide based on modified by silver
The preparation method of catalysis material.
Background technology
Nanometer Cu2The energy gap of O is about 2.1eV, is that rare can be also by the semi-conducting material of excited by visible light
A kind of p-type semiconductor material for having a Metal-vacancy, can effectively absorb the light of wavelength in visible-range, so as to produce photoproduction electricity
Son and hole.When with energy be more than Cu2When the light of O band gap widths is excited, electronics and hole will be in semiconductor surface and inside
Various organic-inorganic contaminant degradations are CO to aoxidize or reduce surface adsorbate by rapid transfer2And H2O, and without secondary
Pollution, therefore Cu2O has wide application prospect in environmental protection, decontamination field.But simple nanometer Cu2The electronics of O and answering for hole
Conjunction rate is high, and the efficiency of light energy utilization is low, and photocatalysis effect is poor, and its conversion efficiency to sunshine is also undesirable.Existing improved method is
By Cu2O is coupled as a kind of sensitized semiconductor with another gap semiconductor, forms the p-n junction with catalytic efficiency high.
But the method complex operation, is not apparent from improving the photoelectric transformation efficiency and electron-hole recombination rate problem high of semi-conducting material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver, energy
Prepare the photocatalysis effect Cu that preferably Ag containing metal is modified2O films.
The technical solution adopted in the present invention is, a kind of preparation of the nano cuprous oxide catalysis material based on modified by silver
Method, specifically implements according to following steps：
Step 1, prepares Cu2O films；
Step 2, the Cu that will be prepared in step 12Reacted in O films immersion silver nitrate solution, obtained metal modified by silver
Nanometer Cu2O catalysis materials.
The features of the present invention is also resided in,
The step 1 is specifically implemented according to following steps：
Step 1.1, ITO electro-conductive glass is cleaned by ultrasonic in Ultrasound Instrument with solvent, by the ITO conduction glass after cleaning
Glass is respectively calomel electrode and platinum electrode as working electrode, reference electrode and to electrode；
Step 1.2, configures electrolyte, using the mixed solution of copper-bath and lactic acid solution as electrolyte；
Step 1.3, is 10.0~11.5 to NaOH solution regulation pH is added in the electrolyte configured in step 1.2；
Step 1.4, will regulate the electrolyte of pH under certain deposition voltage and mixing speed in step 1.3, and
40~60min is deposited in electrochemical workstation, Cu is obtained2O films.
The step 2 is specifically implemented according to following steps：
Step 2.1, by gained Cu in step 12The immersion of O films contains Ag+Silver nitrate solution in reacted, keep it is thin
Film location 10s~30s is motionless, obtains the Cu containing modified by silver2O films；
Step 2.2, the Cu containing modified by silver of gained after being reacted through step 2.12O films are cleaned with distilled water, natural
Dry, obtain the nanometer Cu of metal modified by silver2O catalysis materials.
ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in the step 1.1.
The step 1.2 is specifically implemented according to following steps：
Step 1.2.1, configuration concentration is the copper-bath of 0.01mol/L~0.1mol/L；
Step 1.2.2, configuration concentration is the lactic acid solution of 0.1mol/L~1.0mol/L；
Step 1.2.3, the copper-bath that will have been configured is 2~3 according to volume ratio with lactic acid solution：1 ratio is super
Mix under the conditions of sound, stand 5~10min, obtain preparing Cu2The electrolyte of O.
NaOH solution concentration described in step 1.3 is 4~5mol/L.
Deposition voltage in step 1.4 is -0.55V~-0.40V, and mixing speed is 100rpm~200rpm, sedimentation time
It is 40~60min.
The concentration of the silver nitrate in step 2.1 is 0.01mol/L~0.05mol/L.
Ultrasound condition in step 1.2.3 is that ultrasonic electrical power is 300~500W, and working frequency is 40~60KHz.
The beneficial effects of the invention are as follows a kind of system of the nano cuprous oxide catalysis material based on modified by silver of the invention
Preparation Method is simple to operate, can more accurately control the pattern of made catalysis material；The stability of catalysis material is effectively increased,
Recycling rate of waterused is also high；Overcome existing modified Nano Cu2The technical barrier of O films；Largely improve Cu2The photocatalysis of O
Activity, makes photochemical catalyst obtain further genralrlization application, more operability and application in real life, production.
Brief description of the drawings
Fig. 1 is Cu2The nanometer Cu of O films and metal modified by silver2The XRD diffracting spectrums of O films；
Fig. 2 is the nanometer Cu of metal modified by silver2The SEM figures of O films；
Fig. 3 is Cu2The nanometer Cu of O films and metal modified by silver2The dynamic process figure of O film degradation methylene blues.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver of the present invention, specifically according to following step
It is rapid to implement：
Step 1, prepares Cu2O films；
Step 2, the Cu that will be prepared in step 12Reacted in O films immersion silver nitrate solution, obtained metal modified by silver
Nanometer Cu2O catalysis materials.
The features of the present invention is also resided in,
Step 1 is specifically implemented according to following steps：
Step 1.1, ITO electro-conductive glass is cleaned by ultrasonic in Ultrasound Instrument with solvent, by the ITO conduction glass after cleaning
Glass is respectively calomel electrode and platinum electrode as working electrode, reference electrode and to electrode；
Step 1.2, configures electrolyte, using the mixed solution of copper-bath and lactic acid solution as electrolyte；
Step 1.3, is 10.0~11.5 to NaOH solution regulation pH is added in the electrolyte configured in step 1.2；
Step 1.4, will regulate the electrolyte of pH under certain deposition voltage and mixing speed in step 1.3, and
40~60min is deposited in electrochemical workstation, Cu is obtained2O films.
Step 2 is specifically implemented according to following steps：
Step 2.1, by gained Cu in step 12The immersion of O films contains Ag+Silver nitrate solution in reacted, keep it is thin
Film location 10s~30s is motionless, obtains the Cu containing modified by silver2O films；
Step 2.2, the Cu containing modified by silver of gained after being reacted through step 2.12O films are cleaned with distilled water, natural
Dry, obtain the nanometer Cu of metal modified by silver2O catalysis materials.
ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in step 1.1.
Step 1.2 is specifically implemented according to following steps：
Step 1.2.1, configuration concentration is the copper-bath of 0.01mol/L~0.1mol/L；
Step 1.2.2, configuration concentration is the lactic acid solution of 0.1mol/L~1.0mol/L；
Step 1.2.3, the copper-bath that will have been configured is 2~3 according to volume ratio with lactic acid solution：1 ratio is super
Mix under the conditions of sound, stand 5~10min, obtain preparing Cu2The electrolyte of O.
NaOH solution concentration in step 1.3 is 4~5mol/L.
Deposition voltage in step 1.4 is -0.55V~-0.40V, and mixing speed is 100rpm~200rpm, sedimentation time
It is 40~60min.
The concentration of the silver nitrate in step 2.1 is 0.01mol/L~0.05mol/L.
Ultrasound condition in step 1.2.3 is that ultrasonic electrical power is 300~500W, and working frequency is 40~60KHz.
Fig. 1 is the Cu before metal Ag modifications2The nanometer Cu of O films and metal modified by silver2The XRD diffracting spectrums of O films, from
Fig. 1 can be seen that the Cu modified through metal Ag2Strong silver-colored phase character peak is occurred in that on O film samples, with standard card
(JCPDSNo.87-720) it is consistent.And it can be found that strong and sharp Cu2O diffraction maximums appear in 2 θ for 29.55 °,
36.42 °, 42.30 °, 61.34 °, 73.53 ° of position, i.e., corresponding to Cu2(110) of O, (111), (200), (220), (311)
Crystal face, matches with JCPDSNo.05-0667 standard cards, and does not occur other peaks, illustrating metal Ag between diffraction maximum
Gained Cu after modification2The purity of O films is higher.
Fig. 2 is the nanometer Cu of metal modified by silver2The SEM figures of O films, figure it is seen that after being modified through metal Ag
Cu2O nanostructured surfaces grow into layer structure that is continuous, smooth but having obvious taper.
Fig. 3 is the Cu before metal Ag modifications2The nanometer Cu of O films and metal modified by silver2O film degradation methylene blues it is dynamic
Mechanical process figure, from figure 3, it can be seen that compared to simple Cu2O films, modified Cu2O films have to methylene blue degradation rate
Obvious to improve, degradation rate is lifted to 93% or so, illustrates Cu after metal Ag modifications2O films have more preferable photocatalysis effect.
Embodiment 1
A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver of the present invention, specifically according to following step
It is rapid to implement：
Step 1, prepares Cu2O films；
ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in Ultrasound Instrument, the ITO after cleaning is conductive
Glass is respectively calomel electrode and platinum electrode as working electrode, reference electrode and to electrode；Configuration electrolyte, is respectively configured dense
Spend for the copper-bath and configuration concentration of 0.01mol/L are the lactic acid solution of 0.1mol/L, measure the copper sulphate for having configured molten
Liquid 100mL, measures the lactic acid solution 50mL for having configured, by two solution ultrasonic electrical power be 300W, working frequency is 40KHz
Ultrasound condition under mix, stand 10min, obtain prepare Cu2The electrolyte of O；To the Cu for preparing2Concentration is added in the electrolyte of O
For the NaOH solution regulation pH of 4mol/L is 10.0；It is that -0.40V, mixing speed are that the electrolyte of pH is regulated in deposition voltage
100rpm, and 40min is deposited in electrochemical workstation.Obtain Cu2O films.
Step 2, by gained Cu in step 12O films immerse concentration to be reacted in the silver nitrate solution of 0.01mol/L,
Keep film position 10s motionless, obtain the Cu containing modified by silver2O films；By through the Cu containing modified by silver of gained2O films are used
Distilled water is cleaned, and is dried naturally, obtains the nanometer Cu of metal modified by silver2O catalysis materials.
Embodiment 2
A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver of the present invention, specifically according to following step
It is rapid to implement：
Step 1, prepares Cu2O films；
ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in Ultrasound Instrument, the ITO after cleaning is conductive
Glass is respectively calomel electrode and platinum electrode as working electrode, reference electrode and to electrode；Configuration electrolyte, is respectively configured dense
Spend for the copper-bath and configuration concentration of 0.03mol/L are the lactic acid solution of 0.7mol/L, measure the copper sulphate for having configured molten
Liquid 100mL, measures the lactic acid solution 40mL for having configured, by two solution ultrasonic electrical power be 400W, working frequency is 50KHz
Ultrasound condition under mix, stand 5min, obtain prepare Cu2The electrolyte of O；To the Cu for preparing2Concentration is added in the electrolyte of O
For the NaOH solution regulation pH of 4.5mol/L is 10.5；The electrolyte for regulating pH is -0.50V, mixing speed in deposition voltage
It is 150rpm, and 50min is deposited in electrochemical workstation.Obtain Cu2O films.
Step 2, by gained Cu in step 12O films immerse concentration to be reacted in the silver nitrate solution of 0.03mol/L,
Keep film position 20s motionless, obtain the Cu containing modified by silver2O films；By through the Cu containing modified by silver of gained2O films are used
Distilled water is cleaned, and is dried naturally, obtains the nanometer Cu of metal modified by silver2O catalysis materials.
Embodiment 3
A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver of the present invention, specifically according to following step
It is rapid to implement：
Step 1, prepares Cu2O films；
ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in Ultrasound Instrument, the ITO after cleaning is conductive
Glass is respectively calomel electrode and platinum electrode as working electrode, reference electrode and to electrode；Configuration electrolyte, is respectively configured dense
Spend for the copper-bath and configuration concentration of 0.05mol/L are the lactic acid solution of 0.8mol/L, measure the copper sulphate for having configured molten
Liquid 100mL, measures the lactic acid solution 38mL for having configured, by two solution ultrasonic electrical power be 500W, working frequency is 50KHz
Ultrasound condition under mix, stand 7.5min, obtain prepare Cu2The electrolyte of O；To the Cu for preparing2Added in the electrolyte of O dense
Spend for the NaOH solution regulation pH of 5mol/L is 11.0；The electrolyte for regulating pH is -0.45V, mixing speed in deposition voltage
It is 150rpm, and 60min is deposited in electrochemical workstation, obtains Cu2O films.
Step 2, by gained Cu in step 12O films immerse concentration to be reacted in the silver nitrate solution of 0.05mol/L,
Keep film position 25s motionless, obtain the Cu containing modified by silver2O films；By through the Cu containing modified by silver of gained2O films are used
Distilled water is cleaned, and is dried naturally, obtains the nanometer Cu of metal modified by silver2O catalysis materials.
Embodiment 4
A kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver of the present invention, specifically according to following step
It is rapid to implement：
Step 1, prepares Cu2O films；
ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in Ultrasound Instrument, the ITO after cleaning is conductive
Glass is respectively calomel electrode and platinum electrode as working electrode, reference electrode and to electrode；Configuration electrolyte, is respectively configured dense
Spend for the copper-bath and configuration concentration of 0.1mol/L are the lactic acid solution of 1.0mol/L, measure the copper-bath for having configured
100mL, measures the lactic acid solution 33mL for having configured, in ultrasonic electrical power be 500W by two solution, and working frequency is for 60KHz
Mix under ultrasound condition, stand 8min, obtain preparing Cu2The electrolyte of O；To the Cu for preparing2Addition concentration is in the electrolyte of O
The NaOH solution regulation pH of 5mol/L is 11.5；It is that -0.55V, mixing speed are that the electrolyte of pH is regulated in deposition voltage
200rpm, and 55min is deposited in electrochemical workstation.Obtain Cu2O films.
Step 2, by gained Cu in step 12O films immerse concentration to be reacted in the silver nitrate solution of 0.05mol/L,
Keep film position 30s motionless, obtain the Cu containing modified by silver2O films；By through the Cu containing modified by silver of gained2O films are used
Distilled water is cleaned, and is dried naturally, obtains the nanometer Cu of metal modified by silver2O catalysis materials.
Claims (9)
1. a kind of preparation method of the nano cuprous oxide catalysis material based on modified by silver, it is characterised in that specifically according to
Lower step is implemented：
Step 1, prepares Cu2O films；
Step 2, the Cu that will be prepared in step 12Reacted in O films immersion silver nitrate solution, obtained the nanometer of metal modified by silver
Cu2O catalysis materials.
2. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 1, its
It is characterised by, the step 1 is specifically implemented according to following steps：
Step 1.1, ITO electro-conductive glass is cleaned by ultrasonic in Ultrasound Instrument with solvent, and the ITO electro-conductive glass after cleaning is made
It is working electrode, reference electrode and calomel electrode and platinum electrode is respectively to electrode；
Step 1.2, configures electrolyte, using the mixed solution of copper-bath and lactic acid solution as electrolyte；
Step 1.3, is 10.0~11.5 to NaOH solution regulation pH is added in the electrolyte configured in step 1.2；
Step 1.4, will regulate the electrolyte of pH under certain deposition voltage and mixing speed, and in electrification in step 1.3
40~60min of deposition in work station is learned, Cu is obtained2O films.
3. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 1, its
It is characterised by, the step 2 is specifically implemented according to following steps：
Step 2.1, by gained Cu in step 12The immersion of O films contains Ag+Silver nitrate solution in reacted, keep film position
Put that 10s~30s is motionless, obtain the Cu containing modified by silver2O films；
Step 2.2, the Cu containing modified by silver of gained after being reacted through step 2.12O films are cleaned with distilled water, are dried naturally,
Obtain the nanometer Cu of metal modified by silver2O catalysis materials.
4. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 2, its
It is characterised by, ITO electro-conductive glass is cleaned by ultrasonic with acetone and ethanol successively in the step 1.1.
5. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 2, its
It is characterised by, the step 1.2 is specifically implemented according to following steps：
Step 1.2.1, configuration concentration is the copper-bath of 0.01mol/L~0.1mol/L；
Step 1.2.2, configuration concentration is the lactic acid solution of 0.1mol/L~1.0mol/L；
Step 1.2.3, the copper-bath that will have been configured is 2~3 according to volume ratio with lactic acid solution：1 ratio is in ultrasonic bar
Mix under part, stand 5~10min, obtain preparing Cu2The electrolyte of O.
6. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 2, its
It is characterised by, the NaOH solution concentration described in step 1.3 is 4~5mol/L.
7. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 2, its
It is characterised by, the deposition voltage described in step 1.4 is -0.55V~-0.40V, mixing speed is 100rpm~200rpm, is sunk
The product time is 40~60min.
8. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 3, its
It is characterised by, the concentration of the silver nitrate described in step 2.1 is 0.01mol/L~0.05mol/L.
9. the preparation method of a kind of nano cuprous oxide catalysis material based on modified by silver according to claim 5, its
It is characterised by, the ultrasound condition described in step 1.2.3 is that ultrasonic electrical power is 300~500W, working frequency is 40~
60KHz。
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Cited By (3)
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| CN108336187A (en) * | 2018-02-13 | 2018-07-27 | 桂林理工大学 | A kind of Ag/Cu2The preparation method of O hetero-junctions nano thin-films |
| CN108823588A (en) * | 2018-06-05 | 2018-11-16 | 青岛科技大学 | A kind of Cu of Ag modification2O nanobelt/foam copper combination electrode and preparation method thereof |
| CN108823598A (en) * | 2018-06-05 | 2018-11-16 | 青岛科技大学 | A kind of Ag modification porous structure Cu3P/ foam copper combination electrode and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108336187A (en) * | 2018-02-13 | 2018-07-27 | 桂林理工大学 | A kind of Ag/Cu2The preparation method of O hetero-junctions nano thin-films |
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| CN108823588A (en) * | 2018-06-05 | 2018-11-16 | 青岛科技大学 | A kind of Cu of Ag modification2O nanobelt/foam copper combination electrode and preparation method thereof |
| CN108823598A (en) * | 2018-06-05 | 2018-11-16 | 青岛科技大学 | A kind of Ag modification porous structure Cu3P/ foam copper combination electrode and preparation method thereof |
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