CN105063723B - A kind of method that differential arc oxidation directly prepares iron-silicon-sulphur codope titanium dioxide thin film - Google Patents
A kind of method that differential arc oxidation directly prepares iron-silicon-sulphur codope titanium dioxide thin film Download PDFInfo
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Abstract
The present invention provides a kind of methods that differential arc oxidation directly prepares iron silicon sulphur codope titanium dioxide thin film, and carrying out the conventional surfaces such as deoiling cleaning to steel material surface first cleans；It using steel material as anode, is placed in electrolyte solution, carries out differential arc oxidation processing；There is the steel sample of micro-arc oxidation films to be cleaned and be dried surface, obtained steel sample, as target sample.To realize that the purpose of steel surface differential arc oxidation film layer, electrolyte solution at least should include silicate, dihydric phosphate, sulfate, the component of four kinds of concentration of titania powder.Prepared oxidation Fe2O3 doping two-phase titanium deoxid film is used for visible light photocatalytic degradation methylene blue, there is good degradation effect, can reach 83% degradation rate.The process stabilizing of the present invention is reliable, and the equipment of use is simple, and reaction carries out at normal temperatures, easy to operate, is easy to grasp, and electrolyte solution is environment-friendly type solution, meets environment protection emission requirement.
Description
Technical field
The present invention relates to differential arc oxidization techniques, refer in particular to one kind and directly preparing iron-silicon-sulphur multielement codope in steel surface
The method of titanium dioxide thin film catalyst, the iron-silicon-prepared by this method sulphur codope titanium dioxide thin film can be used for can
Light-exposed catalytic field is used especially for visible light photocatalytic degradation methylene blue.
Background technology
As energy and environment problem becomes increasingly conspicuous, photocatalysis field receives more and more attention.Titanium-dioxide photo is urged
Agent is always the research hotspot of photocatalysis field.Pure titanium dioxide has preferable ultraviolet catalytic, by organic or nothing
After machine element doping, visible light activity can be obtained.Studies have shown that the elements such as multiple element such as iron, silver, sulphur, tungsten, silicon are to improving
The visible light activity of titanium dioxide plays an important roll.Meanwhile containing the mixed structure of a certain proportion of crystalline substance red stone and anatase
With preferable catalytic performance, therefore, it is titania-doped that scientific research personnel using a variety of methods is prepared for iron oxide.
Differential arc oxidization technique is the process for modifying surface to grow up in recent years in anodic oxidation, be chiefly used in Al, Mg, Ti and its
Include the study on the modification for the purpose of improving matrix wear and corrosion behavior and preparation in the surface treatment of the so-called valve metal such as alloy
The research of function film.In recent years, some scholars are gradually in the research for carrying out iron-based material differential arc oxidation.This seminar is to steel
Surface by micro-arc oxidation, which is modified, carries out system research.
It is thin that the present invention first with differential arc oxidation directly prepares iron-silicon-sulphur multielement codope titanium dioxide in steel surface
Film catalyst need not carry out cumbersome pre-treatment and post-processing, and obtain film catalyst and contain brilliant red stone and anatase two
Kind structure crystal form, film have preferable visible light catalytic performance.The present invention is doping type highly efficient titania film catalyst
Preparation provide a kind of new method.
Titanium deoxid film containing ferro element, then by heat treatment, obtaining has brilliant red stone and anatase double structure
The titania-doped film of iron oxide, research shows that the film have higher visible light catalysis activity.
Invention content
The object of the present invention is to provide one kind directly to prepare iron-silicon-sulphur in steel surface by micro-arc oxidation polynary
The method of plain codope titanium dioxide thin film catalyst.It is a new method for preparing catalyst film in steel surface, prepares
Film there is iron-silicon-sulphur multielement codope titanium dioxide, and contain brilliant red stone and two kinds of structure crystal forms of anatase, film
With preferable visible light catalytic performance.Method provided by the invention, be both to differential arc oxidation in-depth research, expand application,
Simultaneously also a kind of new cheap steel attachment load is provided for iron-silicon-sulphur multielement codope titanium dioxide thin film catalyst
Body.The present invention is suitable for various carbon steels, steel alloy etc. in addition to stainless steel.
The present invention is achieved by the following scheme：
A kind of method that differential arc oxidation directly prepares iron-silicon-sulphur codope titanium dioxide thin film, includes the following steps：
Step 1 carries out the cleaning of the conventional surfaces such as deoiling cleaning to steel material surface first；
Step 2, using steel material as anode, be placed in electrolyte solution, carry out differential arc oxidation processing；
Surface there is the steel sample of micro-arc oxidation films to be cleaned and be dried by step 3, obtained steel sample, i.e.,
For target sample.
The bi-directionally or uni-directionally pulse power may be used in micro-arc oxidation process in the present invention, and voltage is 400~600V, and electric current is close
Degree is in 2~15A/dm2Between, processing time is 15~50min.
To realize the purpose of steel surface differential arc oxidation film layer, in the step 2, electrolyte solution at least should include such as
The each component of lower concentration：0.1~0.8mol/L silicates, 0.01~0.1mol/L dihydric phosphates, 0.01~0.1mol/L sulphur
Hydrochlorate, 2~60g/L titania powders.
In order to improve adjustment micro-arc oxidation process stability and film layer quality, electrolyte solution also contain phosphate,
At least one of pyrophosphate, ammonium dihydrogen phosphate；The phosphate concn is 0~0.2mol/L, the pyrophosphate concentration
For 0~0.1mol/L, a concentration of 0~0.2mol/L of ammonium dihydrogen phosphate.
The silicate, dihydric phosphate, sulfate, phosphate, pyrophosphate are sodium salt or sylvite.
Further, electrolyte solution contains each component of following concentration：0.1~0.4mol/L sodium metasilicate and 0.01~
0.05mol/L sodium dihydrogen phosphates, 0.01~0.05mol/L sodium sulphate, 5~30g/L titania powders, 0~0.05mol/L phosphorus
Sour sodium.
Further, electrolyte solution contains each component of following concentration：0.4~0.6mol/L sodium metasilicate and 0.05~
0.08mol/L potassium dihydrogen phosphates, 0.05~0.08mol/L sodium sulphate, 2~5g/L titania powders, 0.05~0.1mol/L
Sodium phosphate, 0.03~0.07mol/L sodium pyrophosphates.
Further, electrolyte solution contains each component of following concentration：0.6~0.8mol/L sodium metasilicate and 0.08~
0.1mol/L potassium dihydrogen phosphates, 0.08~0.1mol/L sodium sulphate, 30~60g/L titania powders, 0.1~0.2mol/L phosphorus
Sour sodium, 0.07~0.1mol/L sodium pyrophosphates, 0.1~0.2mol/L ammonium dihydrogen phosphates.
The mechanism of each component and effect：
Differential arc oxidation：By differential arc oxidation, the titanium deoxid film containing iron-silicon-sulphur codope is directly obtained.Above-mentioned
In electrolyte system, steel surface differential arc oxidation is realized, and obtain film layer, one of doped chemical in film layer iron comes from steel-based
Body, other two doped chemical silicon and sulphur come from electrolyte, and the majority crystallographic structure titanium dioxide in film layer comes from electrolyte；Phosphoric acid
Salt, pyrophosphate, ammonium dihydrogen phosphate are optional component, can be added a small amount of or be not added with as needed.
The specific preparation method of electrolyte：
In the case where being stirred continuously, soluble constituent is first dissolved in deionized water, is gone in right amount for example, being packed into large beaker
Ionized water, sequentially add sodium dihydrogen phosphate, sodium sulphate etc. and be stirred continuously, then be separately added into titania powder etc..
The present invention distinctive feature and advantageous effect be：
(1) pulse power and electrolyte system appropriate are utilized, activates and enhances steel chemical process occurs on anode,
Plasma reaction is generated, the differential arc oxidation of steel is realized, expands the application range of traditional differential arc oxidation；Realize steel table
Face aoxidizes the preparation of Fe2O3 doping and the film containing brilliant red stone and anatase two-phase titanium dioxide, in differential arc oxidation field and its compound
It is had not been reported in processing method.
(2) present invention is suitable for various carbon steels, cast iron, steel alloy etc., and Body regions are extensive.
(3) film for being attached to steel surface has preferable visible light catalysis activity, by prepared oxidation Fe2O3 doping
Two-phase titanium deoxid film is used for visible light photocatalytic degradation methylene blue, has good degradation effect, can reach 89% drop
Solution rate.
(4) process stabilizing of the invention is reliable, and the equipment of use is simple, and reaction carries out at normal temperatures, easy to operate, is easy to
It grasps, electrolyte solution is environment-friendly type solution, meets environment protection emission requirement.
Description of the drawings
Fig. 1 is the SEM figures of the sample prepared by embodiment 1；
Fig. 2 is the XRD diagram of the sample prepared by embodiment 1；
Fig. 3 is the EDS figures of the sample prepared by embodiment 1；
Fig. 4 is design sketch of the sample prepared by embodiment 1 for visible light photocatalytic degradation methylene blue.
Specific implementation mode
The present invention is described further With reference to embodiment：
Embodiment 1：
1. pair Q235 carbon steels surface carries out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.1~0.4mol/L sodium metasilicate and 0.01~0.05mol/L biphosphates
Sodium, 0.01~0.05mol/L sodium sulphate, 5~30g/L titania powders.
3. carrying out differential arc oxidation processing, 400~600V of voltage, 5~20A/ of current density using Q235 carbon steels as anode
dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test.
Film surface appearance such as Fig. 1, surface are in porous structure, the volcanic crater pattern with typical differential arc oxidation.It is porous
Structure to increase catalyst surface area play an important role, be conducive to catalyst with by the contact of catalysis reactant.XRD diagram is shown in figure
2, which shows that film has brilliant red stone and two kinds of structure titanium dioxides of anatase.Its surface energy-spectrum scanning is shown in Fig. 3, and the figure is aobvious
Show, film is mainly made of elements such as iron, oxygen, silicon, titaniums, and the elements such as iron, silicon, sulphur, which all adulterate, enters film.Fig. 4 is will be made
Standby sample is used for visible light photocatalytic degradation methylene blue, has good degradation effect, can reach 83% degradation rate.
Embodiment 2：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.1~0.4mol/L sodium metasilicate and 0.01~0.05mol/L biphosphates
Sodium, 0.01~0.05mol/L sodium sulphate, 5~30g/L titania powders, 0~0.05mol/L sodium phosphates.
3. using 30CrMnSi steel alloys as anode carry out differential arc oxidation processing, 400~600V of voltage, current density 5~
20A/dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 85% degradation rate.
Embodiment 3：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.4~0.6mol/L sodium metasilicate and 0.05~0.08mol/L biphosphates
Potassium, 0.05~0.08mol/L sodium sulphate, 2~5g/L titania powders, 0.05~0.1mol/L sodium phosphates, 0.03~
0.07mol/L sodium pyrophosphates.
3. using 30CrMnSi steel alloys as anode carry out differential arc oxidation processing, 400~600V of voltage, current density 5~
20A/dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 83% degradation rate.
Embodiment 4：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.6~0.8mol/L sodium metasilicate and 0.08~0.1mol/L potassium dihydrogen phosphates,
0.08~0.1mol/L sodium sulphate, 30~60g/L titania powders, 0.1~0.2mol/L sodium phosphates, 0.07~0.1mol/L
Sodium pyrophosphate, 0.1~0.2mol/L ammonium dihydrogen phosphates.
3. using 30CrMnSi steel alloys as anode carry out differential arc oxidation processing, 400~600V of voltage, current density 5~
20A/dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 88% degradation rate.
Embodiment 5：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.4~0.6mol/L sodium metasilicate and 0.05~0.08mol/L biphosphates
Potassium, 0.05~0.08mol/L sodium sulphate, 2~5g/L titania powders, 0.05~0.1mol/L sodium phosphates, 0~0.03mol/
L sodium pyrophosphates.
3. using 30CrMnSi steel alloys as anode carry out differential arc oxidation processing, 400~600V of voltage, current density 5~
20A/dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 83% degradation rate.
Embodiment 6：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.6~0.8mol/L sodium metasilicate and 0.08~0.1mol/L potassium dihydrogen phosphates,
0.08~0.1mol/L sodium sulphate, 30~60g/L titania powders, 0.1~0.2mol/L sodium phosphates, 0.07~0.1mol/L
Sodium pyrophosphate, 0.05~0.1mol/L ammonium dihydrogen phosphates.
3. using 30CrMnSi steel alloys as anode carry out differential arc oxidation processing, 400~600V of voltage, current density 5~
20A/dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 85% degradation rate.
Embodiment 7：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.6~0.8mol/L sodium metasilicate and 0.08~0.1mol/L potassium dihydrogen phosphates,
0.08~0.1mol/L sodium sulphate, 30~60g/L titania powders, 0.1~0.2mol/L sodium phosphates, 0.07~0.1mol/L
Sodium pyrophosphate, 0~0.05mol/L ammonium dihydrogen phosphates.
3. using 30CrMnSi steel alloys as anode carry out differential arc oxidation processing, 400~600V of voltage, current density 5~
20A/dm2, handle 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 87% degradation rate.
Embodiment 8：
1. pair Q235 carbon steels surface carries out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.1mol/L sodium metasilicate and 0.01mol/L sodium dihydrogen phosphates, 0.01mol/L
Sodium sulphate, 5g/L titania powders.
3. carrying out differential arc oxidation processing, voltage 400V, current density 5A/dm using Q235 carbon steels as anode2, handle 15 points
Clock.
4. pair film obtained carries out structural characterization and performance test product phenogram is similar with Fig. 1~Fig. 3, show product
Successful preparation, which is equally applicable to visible light photocatalytic degradation methylene blue, can reach 86% degradation rate.
Embodiment 9：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.4mol/L sodium metasilicate and 0.05mol/L sodium dihydrogen phosphates, 0.05mol/L
Sodium sulphate, 30g/L titania powders, 0.05mol/L sodium phosphates.
3. carrying out differential arc oxidation processing, voltage 500V, current density 10A/dm using 30CrMnSi steel alloys as anode2,
Processing 30 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 80% degradation rate.
Embodiment 10：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.6mol/L sodium metasilicate and 0.08mol/L potassium dihydrogen phosphates, 0.08mol/L
Sodium sulphate, 2g/L titania powders, 0.1mol/L sodium phosphates, 0.03mol/L sodium pyrophosphates.
3. carrying out differential arc oxidation processing, voltage 600V, current density 20A/dm using 30CrMnSi steel alloys as anode2,
Processing 15~50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 85% degradation rate.
Embodiment 11：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.8mol/L sodium metasilicate and 0.1mol/L potassium dihydrogen phosphates, 0.1mol/L sulphur
Sour sodium, 60g/L titania powders, 0.2mol/L sodium phosphates, 0.07mol/L sodium pyrophosphates, 0.1mol/L ammonium dihydrogen phosphates.
3. carrying out differential arc oxidation processing, voltage 600V, current density 15A/dm using 30CrMnSi steel alloys as anode2,
Processing 50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 88% degradation rate.
Embodiment 12：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.8mol/L sodium metasilicate and 0.1mol/L potassium dihydrogen phosphates, 0.1mol/L sulphur
Sour sodium, 60g/L titania powders, 0.2mol/L sodium phosphates, 0.1mol/L sodium pyrophosphates, 0.2mol/L ammonium dihydrogen phosphates.
3. carrying out differential arc oxidation processing, voltage 600V, current density 15A/dm using 30CrMnSi steel alloys as anode2,
Processing 50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 89% degradation rate.
Embodiment 13：
1. pair 30CrMnSi alloy steel surfaces carry out deoiling cleaning.
2. being formulated as follows the electrolyte of concentration：0.8mol/L sodium metasilicate and 0.1mol/L potassium dihydrogen phosphates, 0.1mol/L sulphur
Sour sodium, 60g/L titania powders, 0.2mol/L sodium phosphates, 0.1mol/L sodium pyrophosphates, 0.05mol/L ammonium dihydrogen phosphates.
3. carrying out differential arc oxidation processing, voltage 600V, current density 15A/dm using 30CrMnSi steel alloys as anode2,
Processing 50 minutes.
4. pair film obtained carries out structural characterization and performance test, product phenogram is similar with Fig. 1~Fig. 3, shows to produce
The successful preparation of product, the product are equally applicable to visible light photocatalytic degradation methylene blue, can reach 87% degradation rate.
Claims (7)
1. a kind of method that differential arc oxidation directly prepares iron-silicon-sulphur codope titanium dioxide thin film, includes the following steps：
Step 1 carries out deoiling cleaning conventional surface cleaning to steel material surface first；
Step 2, using steel material as anode, be placed in electrolyte solution, carry out differential arc oxidation processing；
Surface there is the steel sample of micro-arc oxidation films to be cleaned and be dried by step 3, obtained steel sample, as mesh
Mark sample；
It is characterized in that, for the purpose of realization steel surface differential arc oxidation film layer, in step 2, the electrolyte solution is at least answered
This includes each component of following concentration：0.1 ~ 0.8mol/L silicates, 0.01 ~ 0.1mol/L dihydric phosphates, 0.01 ~
0.1mol/L sulfate, 30 ~ 60g/L titania powders；The differential arc oxidation is using bi-directionally or uni-directionally the pulse power, voltage are
400 ~ 600V, current density is in 10 ~ 15A/dm2Between, processing time is 15 ~ 50min.
2. a kind of differential arc oxidation according to claim 1 directly prepares the side of iron-silicon-sulphur codope titanium dioxide thin film
Method, which is characterized in that in order to improve the quality of the stability and film layer that adjust micro-arc oxidation process, electrolyte solution also contains phosphorus
At least one of hydrochlorate, pyrophosphate, ammonium dihydrogen phosphate；The phosphate concn is 0 ~ 0.2mol/L, the pyrophosphate
A concentration of 0 ~ 0.1mol/L, a concentration of 0 ~ 0.2mol/L of ammonium dihydrogen phosphate.
3. a kind of differential arc oxidation according to claim 1 or 2 directly prepares iron-silicon-sulphur codope titanium dioxide thin film
Method, which is characterized in that the silicate, dihydric phosphate, sulfate, phosphate, pyrophosphate are sodium salt or sylvite.
4. a kind of differential arc oxidation according to claim 3 directly prepares the side of iron-silicon-sulphur codope titanium dioxide thin film
Method, which is characterized in that electrolyte solution contains each component of following concentration：0.1 ~ 0.4mol/L sodium metasilicate and 0.01 ~
0.05mol/L sodium dihydrogen phosphates, 0.01 ~ 0.05mol/L sodium sulphate, 30 ~ 60g/L titania powders, 0 ~ 0.05mol/L phosphoric acid
Sodium.
5. a kind of differential arc oxidation according to claim 3 directly prepares the side of iron-silicon-sulphur codope titanium dioxide thin film
Method, which is characterized in that electrolyte solution contains each component of following concentration：0.4 ~ 0.6mol/L sodium metasilicate and 0.05 ~
0.08mol/L potassium dihydrogen phosphates, 0.05 ~ 0.08mol/L sodium sulphate, 30 ~ 60g/L titania powders, 0.05 ~ 0.1mol/L phosphorus
Sour sodium, 0.03 ~ 0.07mol/L sodium pyrophosphates.
6. a kind of differential arc oxidation according to claim 3 directly prepares the side of iron-silicon-sulphur codope titanium dioxide thin film
Method, which is characterized in that electrolyte solution contains each component of following concentration：0.6 ~ 0.8mol/L sodium metasilicate and 0.08 ~ 0.1mol/
L potassium dihydrogen phosphates, 0.08 ~ 0.1mol/L sodium sulphate, 30 ~ 60g/L titania powders, 0.1 ~ 0.2mol/L sodium phosphates, 0.07 ~
0.1mol/L sodium pyrophosphates, 0.1 ~ 0.2mol/L ammonium dihydrogen phosphates.
7. iron-silicon-sulphur the codope titanium dioxide thin film prepared by method as claimed in claim 1 or 2, which is characterized in that institute
Iron-silicon-sulphur the codope titanium dioxide thin film stated is used for photocatalytic degradation methylene blue.
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