CN109911977A - A kind of iridium zinc oxide electrode and its preparation method and application - Google Patents
A kind of iridium zinc oxide electrode and its preparation method and application Download PDFInfo
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- CN109911977A CN109911977A CN201910268395.6A CN201910268395A CN109911977A CN 109911977 A CN109911977 A CN 109911977A CN 201910268395 A CN201910268395 A CN 201910268395A CN 109911977 A CN109911977 A CN 109911977A
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Abstract
The invention belongs to the technical fields of photoelectrocatalysioxidization oxidization degradation of organic waste water, and in particular to a kind of iridium zinc oxide electrode and its preparation method and application.The preparation method of iridium zinc oxide electrode is specifically includes the following steps: chloro-iridic acid and zinc chloride are dissolved in dehydrated alcohol by (1) by certain metal ion molar ratio；(2) it takes the masking liquid of appropriate above-mentioned preparation to carry out single side brushing to titanium plate, obtains IrO2- ZnO/Ti composite oxides electrode；The present invention is by being added iridium, greatly improve the PhotoelectrocatalytiPerformance Performance of electrode, PhotoelectrocatalytiPerformance Performance is much larger than the summation of electro-catalysis and photocatalysis performance, has reached synergistic effect, and electrode is better than rhodamine B and methyl orange solution to the photoelectrocatalysis effect of Congo red solution.
Description
Technical field
The invention belongs to the technical fields of photoelectrocatalysioxidization oxidization degradation of organic waste water, and in particular to one kind is in iridium zinc oxide
Electrode and its preparation method and application.
Background technique
With being constantly progressive for modern industry, environmental pollution is increasingly valued by people, wherein the kind of organic wastewater
Class is many and diverse, endangers water body very big.Traditional physics, chemistry and bioremediation has been unable to satisfy ring higher and higher at present
Guaranteed request.It is a kind of ideal, free of contamination environmental pollution treatment technology by the photocatalysis of catalyst of conductor oxidate, in recent years
Come, is paid close attention to by people.Electrocatalysis high-grade oxidized technology is also a kind of very promising high concentration, toxic, difficult to degrade organic
Wastewater processing technology.The present invention is complementary with photocatalysis technology fusion by electro-catalysis technology, and then carries out corresponding electrocatalysis material
With the application foundation Journal of Sex Research of catalysis material and magnanimity technology of preparing.ZnO has excellent property, such as biggish forbidden bandwidth
(3.37 eV), big exciton bind energy (60 meV), high photocatalysis efficiency etc..This makes nano-ZnO in the organic object space of light degradation
Face has broad application prospects.IrO2Type anode has good analysis oxygen analysis chlorine activity, is excellent electro catalytic activity electrode, Ir
Addition can effectively improve the electric conductivity of electrode.Therefore combination electrode is prepared using both the above material, electro-catalysis and light is urged
Change technology is merged.
Summary of the invention
The purpose of the present invention is to provide a kind of iridium zinc oxide electrodes and its preparation method and application, by the way that iridium is added,
The PhotoelectrocatalytiPerformance Performance of electrode is greatly improved, PhotoelectrocatalytiPerformance Performance is much larger than the summation of electro-catalysis and photocatalysis performance, reaches
Synergistic effect is arrived, electrode is better than the photoelectrocatalysis effect of rhodamine B and methyl orange to Congo red photoelectrocatalysis effect.
To achieve the above object, the present invention takes following technical scheme:
A kind of preparation method of iridium zinc oxide electrode, comprising the following steps:
(1) after etching in sulfuric acid, washing drying is placed in spare in dehydrated alcohol technical pure titanium board TA1.
(2) by chloro-iridic acid (H2IrCl6·6H2The mass fraction 35% of O iridium) and zinc chloride press a complexing metal ion molar ratio
It is dissolved in dehydrated alcohol, ultrasonic vibration, is uniformly mixed to obtain masking liquid.
(3) masking liquid of step (2) is taken to brush the titanium plate of step (1), it is to be coated uniformly after titanium plate is placed on it is infrared
10 min are dried under lamp, is placed in Muffle furnace and pre-oxidizes, and above-mentioned coating-pre-oxidation-process air cooler is repeated after air-cooled until masking liquid
It is exhausted, is finally annealed to obtain iridium zinc oxide electrode.
Wherein step (1) in order to make active coating in conjunction with Titanium base it is more secured, increase and electrode surface area and slow down
Titanium base surface passivation, it usually needs Titanium base is pre-processed, greasy dirt, the cleaning surface oxygen that may be present on surface are removed
Compound.
The metal ion molar ratio of iridium and zinc is (1 ~ 10) in step (2): 32.
Single side brushing described in step (3) specially takes 3 μ L/cm every time2Masking liquid to titanium plate carry out single side brushing,
Pre-oxidation is specially in 500 DEG C of 10 min of pre-oxidation in Muffle furnace, and the annealing is specifically kept the temperature under 500 DEG C of annealing temperature
1 h。
A kind of application of the iridium zinc oxide electrode in photoelectric catalysis degrading organic, specifically: it prepares certain dense
Degree is with Na2SO4As the rhodamine B of electrolyte, methyl orange and Congo red solution, then using the electrode of above-mentioned preparation as work
Make electrode, photoelectrocatalysis is carried out to the solution of preparation respectively, sample interval is 20 min.The rhodamine B, methyl orange and
Congo red solution concentration is 20 mg/L, Na2SO4Concentration is 0.1 mol/L.
Remarkable advantage of the invention is:
The present invention in semiconductor ZnO by being added a small amount of IrO2Prepare IrO2- ZnO/Ti composite oxides electrode, makes electrode not
Only there is excellent photocatalytic activity, while also there is extraordinary electro catalytic activity.Ir4+As activated centre, it is easy to adsorb
Organic molecule, IrO are decomposed in organic molecule, the hole for having extremely strong oxidisability for being conducive to ZnO generation2In vacant Ir3+It is easy to catch
It obtains photoelectron and generates Ir4+, promote electron-hole separation；Ir, which is added, not only makes ZnO introduce impurity energy level, is conducive to capture electronics,
And forbidden band radius is reduced, make longer wavelengths of light wave that can also excite electronics, expands the utilization scope of spectrum, and then improve light quantity
Suboutput；So the effect of photoelectrocatalysis is greater than the sum of photocatalysis and electro-catalysis.Also, combination electrode urges Congo red photoelectricity
Change effect and is better than rose-red and methyl orange.
Detailed description of the invention
Fig. 1 is ultraviolet-ray visible absorbing light of the electrode made from embodiment 1 using different catalysis process to Congo red degradation
Spectrum, (a) electro-catalysis;(b) photocatalysis;(c) photoelectrocatalysis;
Fig. 2 is that electrode made from embodiment 1 uses different catalysis process to Congo red removal rate；
Fig. 3 is the uv-visible absorption spectra that electrode made from embodiment 1 degrades to different organic solutions, (a) rose-red;
(b) methyl orange;(c) Congo red；
Fig. 4 is removal rate comparison diagram of the electrode made from embodiment 1 to different organic solutions.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, below with reference to concrete mode to technology of the present invention
Scheme is described further, but the present invention is not limited only to this.
Embodiment 1
(1) select with a thickness of 1 mm technical pure titanium board TA1 be substrate, it is clipped obtain size be 20 mm × 20mm ×
The titanium plate of 1mm, etches 2h in the 0.5 mol/L concentrated sulfuric acid, and washing drying is placed on spare in dehydrated alcohol.
(2) by chloro-iridic acid (H2IrCl6·6H2The mass fraction 35% of O iridium) and zinc chloride press a complexing metal ion molar ratio
It is dissolved in dehydrated alcohol, 30 min of solution ultrasonic vibration is uniformly mixed.
(3) every time take the masking liquid of 3 μ L/cm2 to titanium plate carry out single side brushing, it is to be coated uniformly after titanium plate is placed on it is red
10 min are dried under outer lamp, is placed in 500 DEG C of Muffle furnace and pre-oxidizes 10 min, above-mentioned coating procedure are repeated after air-cooled 6 times, most
Afterwards sample is kept the temperature into 1 h under 500 DEG C of annealing temperature, obtains iridium, the IrO that zinc metal ion molar ratio is 3:322-ZnO/Ti
Composite oxides electrode.
Using: 1, it prepares with the Na of 0.1 mol/L2SO4The rhodamine B solution of 20 mg/L as electrolyte, is then adopted
It uses the electrode of above-mentioned preparation as working electrode, electro-catalysis, photocatalysis and photoelectric catalysis degrading is carried out to mixed solution respectively
80min, sample interval are 20 min；2, it prepares with the Na of 0.1 mol/L2SO4The methyl of 20 mg/L as electrolyte
Then orange solution is used as working electrode using the electrode of above-mentioned preparation, to solution progress photoelectric catalysis degrading 60min, when sampling
Between between be divided into 20 min；3, it prepares with the Na of 0.1 mol/L2SO4The Congo red solution of 20 mg/L as electrolyte, then
Using the electrode of above-mentioned preparation as working electrode, photoelectric catalysis degrading 40min, sample interval 20 are carried out to solution
min。
Embodiment 2
(1) select with a thickness of 1 mm technical pure titanium board TA1 be substrate, it is clipped obtain size be 20 mm × 20mm ×
The titanium plate of 1mm, etches 2h in the 0.5 mol/L concentrated sulfuric acid, and washing drying is placed on spare in dehydrated alcohol.
(2) by chloro-iridic acid (H2IrCl6·6H2The mass fraction 35% of O iridium) and zinc chloride press a complexing metal ion molar ratio
It is dissolved in dehydrated alcohol, 30 min of solution ultrasonic vibration is uniformly mixed.
(3) every time take the masking liquid of 3 μ L/cm2 to titanium plate carry out single side brushing, it is to be coated uniformly after titanium plate is placed on it is red
10 min are dried under outer lamp, is placed in 500 DEG C of Muffle furnace and pre-oxidizes 10 min, above-mentioned coating procedure are repeated after air-cooled 6 times, most
Afterwards sample is kept the temperature into 1 h under 500 DEG C of annealing temperature, obtains iridium, the IrO that zinc metal ion molar ratio is 1:322-ZnO/Ti
Composite oxides electrode.
Embodiment 3
(1) select with a thickness of 1 mm technical pure titanium board TA1 be substrate, it is clipped obtain size be 20 mm × 20mm ×
The titanium plate of 1mm, etches 2h in the 0.5 mol/L concentrated sulfuric acid, and washing drying is placed on spare in dehydrated alcohol.
(2) by chloro-iridic acid (H2IrCl6·6H2The mass fraction 35% of O iridium) and zinc chloride press a complexing metal ion molar ratio
It is dissolved in dehydrated alcohol, 30 min of solution ultrasonic vibration is uniformly mixed.
(3) every time take the masking liquid of 3 μ L/cm2 to titanium plate carry out single side brushing, it is to be coated uniformly after titanium plate is placed on it is red
10 min are dried under outer lamp, is placed in 500 DEG C of Muffle furnace and pre-oxidizes 10 min, above-mentioned coating procedure are repeated after air-cooled 6 times, most
Afterwards sample is kept the temperature into 1 h under 500 DEG C of annealing temperature, obtains iridium, the IrO that zinc metal ion molar ratio is 10:322-ZnO/
Ti composite oxides electrode.
Fig. 1 illustrates ratio photocatalysis and the electrocatalysis of electrode absorbance decline Congo red under photoelectrocatalysis effect
Fast down, it is good that electrode photo electrocatalysis removes Congo red effect.
Fig. 2 illustrates that electrode removal rate Congo red under photoelectrocatalysis effect is better than photocatalysis and electro-catalysis, electrode
Photoelectrocatalysis effect is best.
Fig. 3 illustrates what the rhodamine B of absorbance decline Congo red under electrode photo electrocatalysis effect and methyl orange declined
Fastly, it is good to remove Congo red effect for electrode photo electrocatalysis.
Fig. 4 illustrates that electrode removal rate Congo red under photoelectrocatalysis effect is better than rhodamine B and methyl orange, electrode
It is best that photoelectrocatalysis removes Congo red effect.
Claims (7)
1. a kind of preparation method of iridium zinc oxide electrode, it is characterised in that: comprise the steps of:
(1) after sulfuric acid etches, washing drying is placed in spare in dehydrated alcohol technical pure titanium board TA1；
(2) chloro-iridic acid and zinc chloride are dissolved in dehydrated alcohol, ultrasonic vibration by a complexing metal ion molar ratio, are uniformly mixed
Obtain masking liquid；
(3) masking liquid of step (2) is taken to brush the titanium plate of step (1), it is to be coated uniformly after titanium plate is placed under infrared lamp
10 min are dried, are pre-oxidized, above-mentioned coating-pre-oxidation-process air cooler is repeated after air-cooled until masking liquid is exhausted, finally
It is annealed to obtain iridium zinc oxide electrode.
2. preparation method according to claim 1, it is characterised in that: the metal ion molar ratio of iridium and zinc in step (2)
For (1 ~ 10): 32.
3. preparation method according to claim 1, it is characterised in that: the brushing in step (3) specially takes 3 μ L every time
/ cm2Masking liquid to titanium plate carry out single side brushing.
4. preparation method according to claim 1, it is characterised in that: the pre-oxidation in step (3) is specially in Muffle furnace
In 10 min are pre-oxidized at 500 DEG C, annealing is specially that 1 h is kept the temperature at 500 DEG C.
5. a kind of iridium zinc oxide electrode as made from claim 1 ~ 4 described in any item preparation methods.
6. a kind of iridium zinc oxide electrode as claimed in claim 5 is in rhodamine B degradation, methyl orange and Congo red application,
It is characterized by: with Na2SO4Solution is electrolyte, using the iridium zinc oxide electrode carry out rhodamine B, methyl orange and just
The photoelectric catalysis degrading of arnotto.
7. application according to claim 6, it is characterised in that: the Na2SO4Concentration is 0.1 mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113813974A (en) * | 2021-10-13 | 2021-12-21 | 福州大学 | Titanium carbide-Mxene doped modified photoelectrocatalysis electrode and preparation method thereof |
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| JP2005217385A (en) * | 2004-01-31 | 2005-08-11 | National Institute For Materials Science | Metal oxide semiconductor including zinc and its manufacturing method |
| CN102603037A (en) * | 2012-04-01 | 2012-07-25 | 南京工业大学 | Organic wastewater treatment film reactor utilizing sunlight-assisted electro-catalysis |
| CN104894620A (en) * | 2015-06-26 | 2015-09-09 | 厦门理工学院 | Electroplating solution, IrO2/ZnO nano composite-structure film material and preparation method thereof |
| CN107162115A (en) * | 2017-05-19 | 2017-09-15 | 福州大学 | A kind of Ir doped titanium-base stannic oxide electrodes with PhotoelectrocatalytiPerformance Performance |
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2019
- 2019-04-04 CN CN201910268395.6A patent/CN109911977A/en active Pending
Patent Citations (4)
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| JP2005217385A (en) * | 2004-01-31 | 2005-08-11 | National Institute For Materials Science | Metal oxide semiconductor including zinc and its manufacturing method |
| CN102603037A (en) * | 2012-04-01 | 2012-07-25 | 南京工业大学 | Organic wastewater treatment film reactor utilizing sunlight-assisted electro-catalysis |
| CN104894620A (en) * | 2015-06-26 | 2015-09-09 | 厦门理工学院 | Electroplating solution, IrO2/ZnO nano composite-structure film material and preparation method thereof |
| CN107162115A (en) * | 2017-05-19 | 2017-09-15 | 福州大学 | A kind of Ir doped titanium-base stannic oxide electrodes with PhotoelectrocatalytiPerformance Performance |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113813974A (en) * | 2021-10-13 | 2021-12-21 | 福州大学 | Titanium carbide-Mxene doped modified photoelectrocatalysis electrode and preparation method thereof |
| CN113813974B (en) * | 2021-10-13 | 2023-08-11 | 福州大学 | Titanium carbide-Mxene doped modified photoelectrocatalysis electrode and preparation method thereof |
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Application publication date: 20190621 |