CN101713092A - Method for preparing titanium dioxide photoelectrodes - Google Patents

Method for preparing titanium dioxide photoelectrodes Download PDF

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Publication number
CN101713092A
CN101713092A CN200910305364A CN200910305364A CN101713092A CN 101713092 A CN101713092 A CN 101713092A CN 200910305364 A CN200910305364 A CN 200910305364A CN 200910305364 A CN200910305364 A CN 200910305364A CN 101713092 A CN101713092 A CN 101713092A
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titanium dioxide
preparation
electrolyte solution
photoelectrodes
titanium
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CN101713092B (en
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刘惠玲
钱程
李宣东
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention provides a method for preparing titanium dioxide photoelectrodes, which relates to a method for preparing photoelectrodes. The invention solves the problems of low catalytic activity of catalysts on the surfaces of titanium dioxide photoelectrodes prepared by the prior method under visible light, complicated preparation process and the like. The method comprises the following steps: 1, using cleanser to roughly wash titanium plates and then using ethanol and acetone in turn for cleaning; 2, performing micro-plasma oxidation; and 3, rinsing with distilled water, drying the obtained product and obtaining the titanium dioxide photoelectrodes. The method has the advantages of high catalytic activity of the catalysts on electrode surfaces and simple preparation process. Under visible light, the removal rate of photoelectrocatalysis rhodamine B of the photoelectrode s prepared by the method is raised by over 35 percent.

Description

A kind of preparation method of titanium dioxide photoelectrode
Technical field
The present invention relates to a kind of preparation method of optoelectronic pole.
Background technology
Photoactivation titanium dioxide (TiO 2) photohole on the semi-conductor valence band, has very strong oxidation capacity, the electronics that can capture in the water molecules generates hydroxyl radical free radical (OH), and OH is that reactive behavior is the strongest in the oxygenant that exists in the water, its oxidation object does not almost have selectivity, so can make multiple inorganicization of organic pollutant that is difficult to degrade, comprising pollutents such as aliphatics, aromatic series, washing composition, dyestuff, agricultural chemicals, weedicide and soil ulmin, and organic in the water " three cause thing " (carcinogenic, teratogenesis, mutagenic matter).TiO 2Have good chemistry and biology inertia, can guarantee the safety of water quality and cheap and easy to get.So TiO 2Photochemical catalytic oxidation has become the current research focus of advanced water treatment process field both at home and abroad as a kind of brand-new water technology.
Nineteen eighty-two, Ward etc. are first with surface coverage TiO 2Platinum electrode (the TiO of film 2/ Pt) handle organic waste water with the photoelectrocatalysioxidization oxidization method, the concurrent existing degradation rate of organism in the photoelectrocatalysis process is than its degradation rate height in corresponding photocatalytic process.Vinodgopal in 1993 etc. studies confirm that: extra electric field can promote the separation of photo-generated carrier, and photoelectric current is significantly improved, thereby has improved the degradation efficiency of organism in photocatalytic process.Utilize this method to the separation in electronics, hole not only simply but also effective, therefore many investigators think that utilizing photoelectrocatalysioxidization oxidization to improve light-catalysed efficient is a up-and-coming research direction.And the core of photoelectrocatalysioxidization oxidization technology is exactly the preparation of highly efficient titania photochemical catalyst electrode.
Existing method prepares problems such as titanium dioxide photoelectrode exists catalyzer catalytic activity under visible light of electrode surface lower, complicated process of preparation.
Description
The objective of the invention is to prepare problems such as titanium dioxide photoelectrode exists catalyzer catalytic activity under visible light of electrode surface lower, complicated process of preparation in order to solve existing method; And provide a kind of preparation method of titanium dioxide photoelectrode.
The preparation method of titanium dioxide photoelectrode of the present invention is undertaken by following step: the preparation method of titanium dioxide photoelectrode is undertaken by following step: one, slightly wash the titanium plate with scrubbing powder earlier, clean with ethanol, clean with acetone then; Two, titanium plate that will be after step 1 is handled is made negative electrode as anode with stainless steel plate, puts into electrolyte solution, and holding current is constant, is 100mA/cm in current density 2, electrolyte solution temperature remain under 20~30 ℃ of conditions and carry out micro-plasma oxidation 60min, electrolyte solution is the aqueous solution of sulfuric acid and cerous nitrate, H in the electrolyte solution 2SO 4Concentration be 0.5mol/L, Ce (NO in the electrolyte solution 3) 3Concentration be 920mg/L; Three, titanium plate that will be after step 2 is handled takes out use distilled water flushing, again at 105 ± 2 ℃ of drying 0.4~0.6h down; Obtain titanium dioxide photoelectrode.
The present invention uses the preparation by micro-plasma oxidation titanium dioxide photoelectrode to simplify preparation technology, and it is even to be prepared into catalyst distribution.Optoelectronic pole photocatalytic activity height under visible light of the inventive method preparation.Under visible light, the clearance of the optoelectronic pole photoelectrocatalysis rhodamine B of the present invention's preparation has improved more than 35%.The optoelectronic pole of the inventive method preparation is used for the treating water Persistent organic pollutants.
Description of drawings
Fig. 1 is the removal graphic representation of optoelectronic pole photoelectrocatalysioxidization oxidization rhodamine B under visible light, among the figure-△-the removal curve of the prepared optoelectronic pole photoelectrocatalysioxidization oxidization rhodamine B under visible light of expression embodiment seven ,--expression optoelectronic pole TiO 2The removal curve of/Ti photoelectrocatalysioxidization oxidization rhodamine B under visible light; Fig. 2 is scanning electronic microscope (SEM) figure on the prepared optoelectronic pole surface of embodiment seven.
Embodiment
Embodiment one: the preparation method of titanium dioxide photoelectrode is undertaken by following step: one, slightly wash the titanium plate with scrubbing powder earlier, clean with ethanol, clean with acetone then; Two, titanium plate that will be after step 1 is handled is made negative electrode as anode with stainless steel plate, puts into electrolyte solution, and holding current is constant, is 100mA/cm in current density 2, electrolyte solution temperature remain on and carry out micro-plasma oxidation 60min under 20~30 ℃ of conditions (impressed voltage reaches 300~400V), and electrolyte solution is the aqueous solution of sulfuric acid and cerous nitrate, H in the electrolyte solution 2SO 4Concentration be 0.5mol/L, Ce (NO in the electrolyte solution 3) 3Concentration be 920mg/L; Three, titanium plate that will be after step 2 is handled takes out use distilled water flushing, again at 105 ± 2 ℃ of drying 0.4~0.6h down; Obtain titanium dioxide photoelectrode.
The rete that the titanium dioxide photoelectrode surface of present embodiment preparation has dense structure, the rete component is Ce-TiO 2, catalyst distribution is even.The clearance of the optoelectronic pole photoelectrocatalysis rhodamine B of present embodiment preparation has improved more than 35%.
Embodiment two: what present embodiment and embodiment one were different is: be in the step 1 with the ethanol scavenging period to be 8~12min.Other step is identical with embodiment one with parameter.
Embodiment three: what present embodiment and embodiment one were different is: be 10min with the ethanol scavenging period in the step 1.Other step is identical with embodiment one with parameter.
Embodiment four: what present embodiment and embodiment one, two or three were different is: be 8~12min with the acetone scavenging period in the step 1.Other step is identical with embodiment one, two or three with parameter.
Embodiment five: what present embodiment and embodiment one, two or three were different is: be 10min with the acetone scavenging period in the step 1.Other step is identical with embodiment one, two or three with parameter.
Embodiment six: what present embodiment and embodiment one to five were different is: be 0.5h time of drying in the step 3.Other step is identical with embodiment one to five with parameter.
Embodiment seven: the preparation method of titanium dioxide photoelectrode is undertaken by following step in the present embodiment: one, slightly wash the titanium plate with scrubbing powder earlier, clean 10min with ethanol again, clean 10min with acetone then; Two, titanium plate that will be after step 1 is handled is made negative electrode as anode with stainless steel plate, puts into electrolyte solution, and holding current is constant, is 100mA/cm in current density 2, electrolyte solution temperature remain on and carry out micro-plasma oxidation 60min under 20~30 ℃ of conditions (impressed voltage reaches 300~400V), and electrolyte solution is the aqueous solution of sulfuric acid and cerous nitrate, H in the electrolyte solution 2SO 4Concentration be 0.5mol/L, Ce (NO in the electrolyte solution 3) 3Concentration be 920mg/L; Three, titanium plate that will be after step 2 is handled takes out use distilled water flushing, again at 105 ± 2 ℃ times dry 0.5h; Obtain titanium dioxide photoelectrode.
The rete that the titanium dioxide photoelectrode surface of present embodiment preparation has dense structure, the rete component is Ce-TiO 2, it is even to prepare catalyst distribution, referring to Fig. 2.Optoelectronic pole photocatalytic activity height under visible light of present embodiment preparation.Optoelectronic pole degradation of dye rhodamine B (the rhodamine B starting point concentration is HID xenon lamp, the applying bias 1.0V of 5mg/L, 35W) under visible light of present embodiment preparation, the result as shown in Figure 1, the clearance of rhodamine B has improved about 35~50% as shown in Figure 1.

Claims (6)

1. the preparation method of a titanium dioxide photoelectrode is characterized in that the preparation method of titanium dioxide photoelectrode is undertaken by following step: one, slightly wash the titanium plate with scrubbing powder earlier, clean with ethanol, clean with acetone then; Two, titanium plate that will be after step 1 is handled is as anode, make negative electrode with stainless steel plate, put into electrolyte solution, holding current is constant, in current density is that the temperature of 100mA/cm2, electrolyte solution remains under 20~30 ℃ of conditions and carries out micro-plasma oxidation 60min, electrolyte solution is the aqueous solution of sulfuric acid and cerous nitrate, and the concentration of H2SO4 is 0.5mol/L in the electrolyte solution, and the concentration of Ce in the electrolyte solution (NO3) 3 is 920mg/L; Three, titanium plate that will be after step 2 is handled takes out use distilled water flushing, again at 105 ± 2 ℃ of drying 0.4~0.6h down; Obtain titanium dioxide photoelectrode.
2. the preparation method of a kind of titanium dioxide photoelectrode according to claim 1 is characterized in that in the step 1 with the ethanol scavenging period being 8~12min.
3. the preparation method of a kind of titanium dioxide photoelectrode according to claim 1 is characterized in that in the step 1 with the ethanol scavenging period being 10min.
4. according to the preparation method of claim 1,2 or 3 described a kind of titanium dioxide photoelectrodes, it is characterized in that in the step 1 with the acetone scavenging period being 8~12min.
5. according to the preparation method of claim 1,2 or 3 described a kind of titanium dioxide photoelectrodes, it is characterized in that in the step 1 with the acetone scavenging period being 10min.
6. according to the preparation method of claim 1,2 or 3 described a kind of titanium dioxide photoelectrodes, it is characterized in that be 0.5h time of drying in the step 3.
CN200910305364XA 2009-08-07 2009-08-07 Method for preparing titanium dioxide photoelectrodes Expired - Fee Related CN101713092B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105597719A (en) * 2015-11-17 2016-05-25 山东大学 Foamed titanium-titanium oxide composite photoelectrocatalytic material and application thereof
CN108118378A (en) * 2017-03-22 2018-06-05 中国科学院金属研究所 A kind of metal oxide nanocatalyst growth in situ and doping modification method
CN114318374A (en) * 2022-01-06 2022-04-12 大连工业大学 Method for degrading hyaluronic acid based on titanium dioxide modified ITO electrode photoelectrocatalysis

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105597719A (en) * 2015-11-17 2016-05-25 山东大学 Foamed titanium-titanium oxide composite photoelectrocatalytic material and application thereof
CN108118378A (en) * 2017-03-22 2018-06-05 中国科学院金属研究所 A kind of metal oxide nanocatalyst growth in situ and doping modification method
CN108118378B (en) * 2017-03-22 2020-08-21 中国科学院金属研究所 In-situ growth and doping modification method of metal oxide nano catalyst
CN114318374A (en) * 2022-01-06 2022-04-12 大连工业大学 Method for degrading hyaluronic acid based on titanium dioxide modified ITO electrode photoelectrocatalysis

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