CN101884938A - Method for preparing nitrogen-doped TiO2 photocatalytic film - Google Patents
Method for preparing nitrogen-doped TiO2 photocatalytic film Download PDFInfo
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Abstract
The invention provides a method for preparing a nitrogen-doped titanium dioxide (TiO2) photocatalytic film, which comprises: firstly, performing nitriding treatment on a metal titanium or titanium alloy surface by using a ion nitriding process; and secondly, growing a TiO2 thin film in situ on the metal titanium or titanium alloy substrate obtained after the nitriding treatment by using a microarc oxidation technique. The method is used in the field of photocatalytic purification. Compared with a TiO2 thin film which is not doped with nitrogen, the nitrogen doped TiO2 photocatalytic film prepared by the method has the advantages that: the ultraviolet light and visible light absorption efficiency is improved obviously; the intensity of light generated current is improved obviously; and the organic material degradation efficiency is improved obviously.
Description
Technical field
The present invention relates to a kind of preparation nitrogen-doped titanium dioxide (TiO
2) method and the purposes of photocatalysis film.
Background technology
Titanium dioxide is a kind of wide bandgap semiconductor, and its energy gap is 3.2eV (anatase), only just can show photocatalytic activity under the exciting of ultraviolet light.Can utilize visible lights a large amount of in the solar energy partly is research TiO
2An important goal of photochemical catalyst.Anion doped TiO
2Because it has caused the concern of numerous researchers in the photocatalytic activity of visible region and the defective that overcome metal ion mixing.Wherein nitrogen mixes and to be considered to one of effective method.
In general, TiO
2The nitrogen of catalysis material mixes and is divided into two kinds of clearance-type and displaced types, and the clearance-type nitrogen-atoms is present in TiO
2In the space of lattice, unstable and come off easily; And the doping of displaced type nitrogen is the process that the oxygen atom substituted nitrogen atom enters lattice, and a small amount of not oxidized nitrogen-atoms still is in the titanium lattice, can obtain the higher TiO of nitrogen doping
2TiO
2The nitrogen of catalysis material mixes and mainly realizes by technology such as chemical vapour deposition (CVD), sol-gel, thermal oxide magnetron sputtering, anodic oxidations, no matter but what obtain is clearance-type or displaced type nitrogen-atoms, the subject matter of existence is to be difficult to obtain the higher TiO of nitrogen doping
2Thereby, improve limited to its photocatalysis efficiency.
Glow discharge nitriding claims the aura nitriding again, utilize the glow discharge principle to carry out, concrete technology is: metal works is put into as negative electrode be connected with the negative-pressure container that contains nitrogen medium, nitrogen, hydrogen atom in the medium of energising back are ionized, and form ion plasma between anode and cathode.Under the effect of ion plasma highfield, to the surface of the work bombardment, surface of the work produces atom sputtering to the cation of nitrogen and hydrogen with at a high speed.Because absorption and diffusion, nitrogen infiltrates surface of the work then.Glow discharge nitriding has characteristics such as the nitriding cycle is short, temperature required low, and process is controlled.
(Micro-arc oxidation, MAO) technology is a kind of new technology at non-ferrous metal surface in situ growth porous, dense ceramic membrane to differential arc oxidation, and combine tight between rete and matrix.Detailed process is that valve metals such as Ti, Al, Mg, Zr, Ta, Nb or its alloy are placed electrolyte aqueous solution, utilize electrochemical method, in the surface micropore of this material, produce the spark discharge spot, under heat chemistry, plasma chemistry and electrochemical acting in conjunction, generate ceramic film.Utilize the MAO technology to prepare TiO at titanium or titanium alloy surface " original position "
2Photocatalysis film.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provides a kind of nitrogen doping higher TiO
2The preparation method of film.
The technical scheme that the present invention provides for solving the problems of the technologies described above is: at first adopt glow discharge nitriding technology that Titanium or titanium alloy surface are carried out the nitriding processing, adopt differential arc oxidization technique growth in situ nitrogen doped Ti O on Titanium after the nitriding or titanium alloy-based surface afterwards again
2Film.
Technique scheme specifically comprises the steps:
1, glow discharge nitriding: Titanium or titanium alloy after the selection polishing are put into the ion-nitriding furnace that is connected with ammonia, and furnace chamber keeps negative pressure; Titanium or titanium alloy are as cathode material, and body of heater applies voltage and produces the glow discharge effect as anode material between anode and cathode, 700～900 ℃ of control temperature, and constant temperature time 5～15h forms a nitriding layer at Titanium or titanium alloy surface;
2, differential arc oxidation: Titanium after surface carburization handled or titanium alloy are as anode, and corrosion resistant plate places electrolyte as cathode material, and electrolyte temperature is controlled at below 40 ℃; Under 200～400V pulse voltage, act on 5～60min, generate nitrogen doped Ti O at Titanium or titanium alloy-based surface
2Film.
In the described glow discharge nitriding step, treat that temperature drops to 100～180 ℃ and takes out titanium or titanium alloy again.
In the described differential arc oxidation step, described electrolyte is the mixed solution of natrium carbonicum calcinatum and nine water sodium metasilicate, and wherein the mass concentration of natrium carbonicum calcinatum is 15～30g/L, and the mass concentration of nine water sodium metasilicate is 5～15g/L.
The nitrogen doped Ti O that the inventive method is prepared
2Film can be used for the light catalytic purifying field.
The inventive method at first utilizes glow discharge nitriding technology to form the nitriding layer with higher concentration at titanium or titanium alloy surface, and then it is carried out MAO handle, and has obtained " displaced type " nitrogen doped Ti O of high concentration
2Film, thus photocatalysis performance improved.With the TiO that does not carry out the nitrogen doping
2Film is compared, and the absorption efficiency of ultraviolet light and visible light is obviously improved, and have obvious red shift phenomenon, and this is with to adopt glow discharge nitriding technology to introduce 10% left and right sides displaced type nitrogen-atoms in conjunction with differential arc oxidation (MAO) technology in the lattice of Titanium relevant.Photogenerated current intensity obviously strengthens, and the degradation efficiency of degraded organic contamination significantly improves.The inventive method technology is simple in addition, and preparation process is easy to control, the production efficiency height, and environmental pollution is little.In a word, the present invention has useful effect.
Description of drawings
Fig. 1 is the nitrogen doped Ti O of embodiment 1 preparation
2The ESEM of film (SEM) figure;
Fig. 2 is the nitrogen doped Ti O of embodiment 2 preparations
2The x-ray photoelectron spectroscopy of film (XPS) figure;
Fig. 3 is the TiO of Comparative Examples and embodiment 5 preparations
2The X-ray diffraction of film (XRD) comparison diagram;
Fig. 4 is the TiO of Comparative Examples and embodiment 5 preparations
2The ultraviolet-visible of film (UV-Vis) absorption spectrum comparison diagram;
Fig. 5 is the TiO of Comparative Examples and embodiment 5 preparations
2The photogenerated current of film (Photo-Current) intensity contrast figure;
Fig. 6 is the TiO of Comparative Examples and embodiment 5 preparations
2Film is to the degradation effect comparison diagram of methylene blue solution.
The specific embodiment
Nitrogen doped Ti O provided by the invention
2The photocatalysis film preparation method is as follows:
At first adopt glow discharge nitriding technology that Titanium or titanium alloy surface are carried out the nitriding processing, adopt differential arc oxidization technique growth in situ nitrogen doped Ti O on Titanium after the nitriding or titanium alloy-based surface afterwards again
2Photocatalysis film.
Specifically comprise the steps:
1, glow discharge nitriding: Titanium or titanium alloy after the selection polishing are put into the ion-nitriding furnace that is connected with ammonia, and furnace chamber keeps negative pressure; Titanium or titanium alloy are as cathode material, and body of heater applies voltage and produces the glow discharge effect as anode material between anode and cathode, 700～900 ℃ of control temperature, and constant temperature time 5～15h forms a nitriding layer at Titanium or titanium alloy surface;
2, differential arc oxidation: Titanium after surface carburization handled or titanium alloy are as anode, and corrosion resistant plate places electrolyte as cathode material, and electrolyte temperature is controlled at below 40 ℃; Under 200～400V pulse voltage, act on 5～60min, generate nitrogen doped Ti O at Titanium or titanium alloy-based surface
2Film.
Below in conjunction with drawings and Examples the present invention is further set forth, but therefore do not limit the present invention within the described scope of embodiments.
Embodiment 1: Titanium after the polishing or titanium alloy are put into the LD-70 type ion-nitriding furnace that is connected with ammonia and furnace chamber maintenance negative pressure, Titanium or titanium alloy are as cathode material, body of heater is as anode material, between anode and cathode, apply voltage and produce the glow discharge effect, 700 ℃ of control temperature, constant temperature time 15h; Treat from ion-nitriding furnace, to take out when temperature drops to 150 ℃ sample; Weighing 20g natrium carbonicum calcinatum, 5g nine water sodium metasilicate add the 1000ml deionized water dissolving and are placed in the reactive tank, as electrolyte; Utilize the effect of electric blender stirring and circulating condensing water that the temperature of whole system in the reactive tank is controlled in 40 ℃; As anode, corrosion resistant plate slowly increases pulse voltage to 300V, stopping reaction 10min as cathode material between two electrodes the Titanium after the nitrogenize or titanium alloy; Reaction is taken off anode material and is cleaned with ultrasonic wave after finishing.
The nitrogen doped Ti O of embodiment 1 preparation
2The ESEM of film (SEM) as shown in Figure 1, as can be seen from Figure: the film that makes is the porous compact shape;
Embodiment 2: Titanium after the polishing or titanium alloy are put into the LD-70 type ion-nitriding furnace that is connected with ammonia and furnace chamber maintenance negative pressure, Titanium or titanium alloy are as cathode material, body of heater is as anode material, between anode and cathode, apply voltage and produce the glow discharge effect, 900 ℃ of control temperature, constant temperature time 10h; Treat from ion-nitriding furnace, to take out when temperature drops to 100 ℃ sample; Weighing 15g natrium carbonicum calcinatum, 10g nine water sodium metasilicate add the 1000ml deionized water dissolving and are placed in the reactive tank, as electrolyte; Utilize the effect of electric blender stirring and circulating condensing water that the temperature of whole system in the reactive tank is controlled in 40 ℃; As anode, corrosion resistant plate slowly increases pulse voltage to 400V, stopping reaction 5min as cathode material between two electrodes the Titanium after the nitrogenize or titanium alloy; Reaction is taken off anode material and is cleaned with ultrasonic wave after finishing.
Nitrogen doped Ti O by embodiment 2 preparations
2Film x-ray photoelectron spectroscopy (XPS) therefrom can draw as shown in Figure 2: nitrogen-atoms has entered TiO really
2Lattice, and be that " displaced type " mixes, the doping of nitrogen reaches 11%, far above the nitrogen doping (3%-5%) of commonsense method;
Embodiment 3: Titanium after the polishing or titanium alloy are put into the LD-70 type ion-nitriding furnace that is connected with ammonia and furnace chamber maintenance negative pressure, Titanium or titanium alloy are as cathode material, body of heater is as anode material, between anode and cathode, apply voltage and produce the glow discharge effect, 850 ℃ of control temperature, constant temperature time 5h; Treat from ion-nitriding furnace, to take out when temperature drops to 180 ℃ sample; Weighing 25g natrium carbonicum calcinatum, 15g nine water sodium metasilicate add the 1000ml deionized water dissolving and are placed in the reactive tank, as electrolyte; Utilize the effect of electric blender stirring and circulating condensing water that the temperature of whole system in the reactive tank is controlled in 40 ℃; As anode, corrosion resistant plate slowly increases pulse voltage to 200V, stopping reaction 30min as cathode material between two electrodes the Titanium after the nitrogenize or titanium alloy; Reaction is taken off anode material and is cleaned with ultrasonic wave after finishing.
Embodiment 4: Titanium after the polishing or titanium alloy are put into the LD-70 type ion-nitriding furnace that is connected with ammonia and furnace chamber maintenance negative pressure, Titanium or titanium alloy are as cathode material, body of heater is as anode material, between anode and cathode, apply voltage and produce the glow discharge effect, 850 ℃ of control temperature, constant temperature time 8h; Treat from ion-nitriding furnace, to take out when temperature drops to 150 ℃ sample; Weighing 30g natrium carbonicum calcinatum, 12g nine water sodium metasilicate add the 1000ml deionized water dissolving and are placed in the reactive tank, as electrolyte; Utilize the effect of electric blender stirring and circulating condensing water that the temperature of whole system in the reactive tank is controlled in 40 ℃; As anode, corrosion resistant plate slowly increases pulse voltage to 250V, stopping reaction 60min as cathode material between two electrodes the Titanium after the nitrogenize or titanium alloy; Reaction is taken off anode material and is cleaned with ultrasonic wave after finishing.
Embodiment 5: get a Titanium or a titanium alloy after the polishing and put into the LD-70 type ion-nitriding furnace that is connected with ammonia and furnace chamber maintenance negative pressure, Titanium or titanium alloy are as cathode material, body of heater is as anode material, between anode and cathode, apply voltage and produce the glow discharge effect, 800 ℃ of control temperature, constant temperature time 10h; Treat from ion-nitriding furnace, to take out when temperature drops to 150 ℃ sample; Weighing 20g natrium carbonicum calcinatum, 8g nine water sodium metasilicate add the 1000ml deionized water dissolving and are placed in the reactive tank, as electrolyte; Utilize the effect of electric blender stirring and circulating condensing water that the temperature of whole system in the reactive tank is controlled in 40 ℃; As anode, corrosion resistant plate slowly increases pulse voltage to 350V, stopping reaction 10min as cathode material between two electrodes the Titanium after the nitrogenize or titanium alloy; After reaction finishes anode material is taken off and clean, promptly obtain nitrogen doped Ti O with ultrasonic wave
2Film.
Comparative Examples: weighing 20g natrium carbonicum calcinatum, 8g nine water sodium metasilicate add the 1000ml deionized water dissolving and are placed in the reactive tank, as electrolyte; Utilize the effect of electric blender stirring and circulating condensing water that the temperature of whole system in the reactive tank is controlled in 40 ℃; Titanium after the selection polishing or titanium alloy are as anode material, and corrosion resistant plate slowly increases pulse voltage to 350V, stopping reaction 10min as cathode material between two electrodes; Reaction is cleaned the Titanium anode after finishing with ultrasonic wave, nitrogen TiO is not promptly mixed
2Film sample.
Figure 3 shows that the nitrogen doped Ti O of embodiment 5 preparations
2The not nitrogen doped Ti O of film and Comparative Examples preparation
2The X-ray diffraction of film (XRD) comparison diagram, therefrom can draw: the doping of nitrogen can increase the ratio of film surface anatase phase constituent.
Figure 4 shows that the nitrogen doped Ti O of embodiment 5 preparations
2The not nitrogen doped Ti O of film and Comparative Examples preparation
2The ultraviolet-visible of film (UV-Vis) absorption spectrum comparison diagram, therefrom as can be seen: the nitrogen doped Ti O of embodiment 5 preparations
2Film improves the absorption intensity of ultraviolet and visible light wave range, and obvious red shift phenomenon has taken place.
Figure 5 shows that the nitrogen doped Ti O of embodiment 5 preparations
2The not nitrogen doped Ti O of film and Comparative Examples preparation
2The photogenerated current of film (Photo-Current) intensity contrast figure, therefrom as can be seen: the nitrogen doped Ti O of embodiment 5 preparations
2The photogenerated current intensity of film significantly improves.
Two samples of embodiment 5 and Comparative Examples are used for the contrast experiment of degradation of methylene blue solution, and the concentration of methylene blue solution is 12 mg/litre in the experiment, and the light source that adopts is a high-pressure sodium lamp.Contrast and experiment can be drawn by Fig. 6 as shown in Figure 6: nitrogen doped Ti O
2Film to the degradation rate of methylene blue solution with respect to nitrogen doped Ti O not
2Film obviously improves.
Claims (5)
1. nitrogen doped Ti O
2The preparation method of photocatalysis film is characterized in that: at first adopt glow discharge nitriding technology that Titanium or titanium alloy surface are carried out the nitriding processing, adopt differential arc oxidization technique growth in situ nitrogen doped Ti O on Titanium after the nitriding or titanium alloy-based surface afterwards again
2Film.
2. preparation method as claimed in claim 1 is characterized in that, specifically comprises the steps:
1) glow discharge nitriding: Titanium or titanium alloy after the selection polishing are put into the ion-nitriding furnace that is connected with ammonia, and furnace chamber keeps negative pressure; Titanium or titanium alloy are as cathode material, and body of heater applies voltage and produces the glow discharge effect as anode material between anode and cathode, 700～900 ℃ of control temperature, and constant temperature time 5～15h forms a nitriding layer at Titanium or titanium alloy surface;
2) differential arc oxidation: Titanium after surface carburization handled or titanium alloy are as anode, and corrosion resistant plate places electrolyte as cathode material, and electrolyte temperature is controlled at below 40 ℃; Under 200～400V pulse voltage, act on 5～60min, generate nitrogen doped Ti O at Titanium or titanium alloy-based surface
2Film.
3. preparation method as claimed in claim 2 is characterized in that: in the glow discharge nitriding step, treat that temperature drops to 100～180 ℃ and takes out titanium or titanium alloy again.
4. preparation method as claimed in claim 2, it is characterized in that: in the differential arc oxidation step, described electrolyte is the mixed solution of natrium carbonicum calcinatum and nine water sodium metasilicate, and wherein the mass concentration of natrium carbonicum calcinatum is 15～30g/L, and the mass concentration of nine water sodium metasilicate is 5～15g/L.
5. each prepared nitrogen doped Ti O of claim 1～4
2Film is used for the light catalytic purifying field.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145294A (en) * | 2011-03-10 | 2011-08-10 | 武汉大学 | Method for preparing ternary TiO2 thin film |
| CN102321902A (en) * | 2011-06-23 | 2012-01-18 | 兰州理工大学 | Preparation method for composite film on titanium alloy surface and solution formula thereof |
| CN103074588A (en) * | 2013-01-15 | 2013-05-01 | 太原理工大学 | Method for preparing boron-nitrogen-doped titanium dioxide thin film |
| CN103230807A (en) * | 2013-04-18 | 2013-08-07 | 武汉大学 | Method for preparing wide-spectral-response titanium dioxide thin film through ion beam doping |
| CN103276393A (en) * | 2013-05-23 | 2013-09-04 | 太原理工大学 | Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) porous film on surface of stainless steel matrix |
| CN103489935A (en) * | 2013-09-26 | 2014-01-01 | 四川农业大学 | Nitrogen-doped titanium dioxide photoelectrode responding to visible light and infrared light and method for preparing same |
| CN104846414A (en) * | 2015-04-17 | 2015-08-19 | 江苏大学 | Micro-arc oxidation preparation method of TiO2 semiconductor photoanode |
| CN104959159A (en) * | 2015-05-21 | 2015-10-07 | 浙江大学 | Nitrogen-doped titanium dioxide film, and preparation method and applications thereof |
| CN107502939A (en) * | 2017-06-26 | 2017-12-22 | 安徽雷萨重工机械有限公司 | A kind of anti-friction bearing rolling element |
| CN107723778A (en) * | 2017-09-06 | 2018-02-23 | 太原理工大学 | A kind of method for preparing Ni Ti O richness Ni nano-pores in NiTi alloy surfaces |
| CN109092347A (en) * | 2017-06-21 | 2018-12-28 | 神华集团有限责任公司 | Hydrogenation catalyst and its preparation method and application |
| CN110180020A (en) * | 2019-05-29 | 2019-08-30 | 中国科学院上海硅酸盐研究所 | A kind of N doping titanium oxide coating and its preparation method and application |
| CN111424236A (en) * | 2020-04-29 | 2020-07-17 | 缙云县太极科技有限公司 | Preparation method of antibacterial titanium product |
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| CN102145294A (en) * | 2011-03-10 | 2011-08-10 | 武汉大学 | Method for preparing ternary TiO2 thin film |
| CN102321902A (en) * | 2011-06-23 | 2012-01-18 | 兰州理工大学 | Preparation method for composite film on titanium alloy surface and solution formula thereof |
| CN103074588A (en) * | 2013-01-15 | 2013-05-01 | 太原理工大学 | Method for preparing boron-nitrogen-doped titanium dioxide thin film |
| CN103074588B (en) * | 2013-01-15 | 2015-11-18 | 太原民丰金属表面处理科技有限公司 | A kind of preparation method of boron nitrogen co-doped titanium dioxide film |
| CN103230807A (en) * | 2013-04-18 | 2013-08-07 | 武汉大学 | Method for preparing wide-spectral-response titanium dioxide thin film through ion beam doping |
| CN103230807B (en) * | 2013-04-18 | 2015-03-25 | 武汉大学 | Method for preparing wide-spectral-response titanium dioxide thin film through ion beam doping |
| CN103276393A (en) * | 2013-05-23 | 2013-09-04 | 太原理工大学 | Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) porous film on surface of stainless steel matrix |
| CN103489935B (en) * | 2013-09-26 | 2016-01-20 | 四川农业大学 | Nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light and preparation method thereof |
| CN103489935A (en) * | 2013-09-26 | 2014-01-01 | 四川农业大学 | Nitrogen-doped titanium dioxide photoelectrode responding to visible light and infrared light and method for preparing same |
| CN104846414A (en) * | 2015-04-17 | 2015-08-19 | 江苏大学 | Micro-arc oxidation preparation method of TiO2 semiconductor photoanode |
| CN104959159A (en) * | 2015-05-21 | 2015-10-07 | 浙江大学 | Nitrogen-doped titanium dioxide film, and preparation method and applications thereof |
| CN109092347A (en) * | 2017-06-21 | 2018-12-28 | 神华集团有限责任公司 | Hydrogenation catalyst and its preparation method and application |
| CN109092347B (en) * | 2017-06-21 | 2022-03-22 | 国家能源投资集团有限责任公司 | Hydrogenation catalyst, preparation method and application thereof |
| CN107502939A (en) * | 2017-06-26 | 2017-12-22 | 安徽雷萨重工机械有限公司 | A kind of anti-friction bearing rolling element |
| CN107502939B (en) * | 2017-06-26 | 2020-12-01 | 阜阳市鼎铭汽车配件制造有限公司 | Wear-resistant bearing rolling body |
| CN107723778A (en) * | 2017-09-06 | 2018-02-23 | 太原理工大学 | A kind of method for preparing Ni Ti O richness Ni nano-pores in NiTi alloy surfaces |
| CN107723778B (en) * | 2017-09-06 | 2020-01-07 | 太原理工大学 | Method for preparing Ni-Ti-O Ni-rich nano-pores on surface of NiTi alloy |
| CN110180020A (en) * | 2019-05-29 | 2019-08-30 | 中国科学院上海硅酸盐研究所 | A kind of N doping titanium oxide coating and its preparation method and application |
| CN111424236A (en) * | 2020-04-29 | 2020-07-17 | 缙云县太极科技有限公司 | Preparation method of antibacterial titanium product |
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Application publication date: 20101117 |