CN1491753A - Method for forming nano TiO2 light catalystic active agenbt coating on substrate - Google Patents
Method for forming nano TiO2 light catalystic active agenbt coating on substrate Download PDFInfo
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- CN1491753A CN1491753A CNA021459258A CN02145925A CN1491753A CN 1491753 A CN1491753 A CN 1491753A CN A021459258 A CNA021459258 A CN A021459258A CN 02145925 A CN02145925 A CN 02145925A CN 1491753 A CN1491753 A CN 1491753A
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Abstract
The present invention belongs to the field of coating technology, and is especially plasma spray process of forming nano TiO2 photocatalytic activator coating on substrate. The process includes utilizing the mixed gas of nitrogen or argon and hydrogen as work gas and nitrogen as powder feeding gas; cleaning the substrate, preheating at 200-600 deg.c, spraying nano TiO2 powder onto the surface of the substrate in a plasma spraying equipment to form nano TiO2 film; and sintering at 500-600 deg.c to cure the nano TiO2 film completely and obtain the nano TiO2 photocatalytic activator coating. The coating is firm, stable and high in photocatalytic activity. The present invention may be used widely in the carrying of photocatalyst and heat spraying of nano powder.
Description
Technical field
The invention belongs to field of coating, particularly a kind of plasma spraying technology that utilizes, the method for formation nano titanium dioxide photocatalysis active agent coating on base material.
Background technology
Because advancing by leaps and bounds of science and technology, the Human's production practical activity constantly enlarges, and the pollution of thing followed environment and destruction have also been developed into the degree that is enough to threaten human survival.Development in recent years get up with semiconductor as multiphase photocatalysis at environmental area, especially aspect the organic pollution in handling gas phase and water, obtained certain application.In can be used for light-catalysed semi-conducting material, titanium dioxide crystal has higher photocatalytic activity, and it also is to study extensive, the most deep a kind of metal oxide semiconductor at present aspect photocatalytic applications.It is under the irradiation of light, and energy most organic pollution of oxidation and part inorganic pollution finally are degraded to CO
2, H
2Innocuous substances such as O are called environmentally friendly material.It can be widely used in water treatment and cleaning harmful gas, the automatically cleaning technology, and anti-biotic material, antifouling, antifogging coating is killed aspects such as cancer cell and conversion of solar energy.
In the past twenty years, people extensively and have in depth studied semi-conductive modification technology improving the activity and the catalytic efficiency of photochemical catalyst, with and to the photocatalytic degradation of various harmful substances in the water and air.The photocatalytic product that existing photocatalysis efficiency has reached practical level mostly is powder, and most studies is carried out in suspension system, and in use there is the problem of separating with the recovery difficulty in photochemical catalyst like this, is difficult for utilizing again.Many in recent years people are at the immobilization technology of research photochemical catalyst, preparation block of photochemical catalyst or coating etc., be used for producing need not to do recycling just can nonexpondable photocatalytic product.Thermal spraying has great potential as a kind of face coat technology towards 21st century aspect the exploitation photocatalytic environmental-protection coating.Therefore, technological development and the application with thermal spraying optically catalytic TiO 2 coating is significant and wide application prospect.
Plasma spray technology is used for preparing nano coating as a kind of traditional coating preparation means and has special advantages, and is low as cost, efficient is high, be useful for characteristics such as suitability for industrialized production and coatings prepared bond strength height.Utilize nano-powder and plasma spraying technology to prepare the functional nano coating, make nano material be more convenient for using.Plasma spraying is in the spray gun of a particular design, the energy that utilizes arc discharge is working gas (argon gas, nitrogen and hydrogen etc.) ionization, produces one immediately and has high temperature (20000～30000 ℃), the plasma enthalpy stream of (speed 〉=1000 meter per seconds) at a high speed.The powder of the material that will spray is sent under the promotion of carrier gas in the plasma enthalpy stream of high temperature, high speed uniformly with special powder feeder, and powder is heated rapidly, ejects fast, strikes on the workpiece of desire spraying, forms coating.Because plasma torch has characteristics such as high temperature, high speed and atmosphere is controlled, so it almost can spray all materials.
Summary of the invention
The purpose of this invention is to provide a kind of method that on base material, forms the nano titanium dioxide photocatalysis active agent coating, the technology of using thermal spraying will have the nano-powder spraying of photocatalytic activity and be solidificated on the surface of acceptable substrate, and the coating surface of gained has close with nano-powder or be better than weather resisteant energy, physical property and the serviceability of nano-powder.The surface that makes nano-functional material can be convenient, cheap, be effectively applied to acceptable substrate.
Using plasma technology spraying nano-powder is a new field.The inventor is when using the plasma spraying nano-titanium dioxide powder, by adjusting and control the running parameter of plasma spraying equipment, can directly nano-powder be sprayed on the base material through cleaning and The pre-heat treatment, again with this base material again in 500～600 ℃ of following sintering of temperature 2～4 hours, the result obtains in conjunction with firm, stable, and has the coating of high light catalytic activity.
The method that on base material, forms the nano titanium dioxide photocatalysis active agent coating of the present invention, described method step comprises:
(1). with ordinary nitrogen (N
2) and common hydrogen (H
2) mist or argon gas (Ar) and hydrogen (H
2) mist as working gas; Wherein, hydrogen accounts for 10～30% of mist volume; With ordinary nitrogen (N
2) be powder feeding gas, the purity of gas 〉=99.9%.
(2). substrate surface is cleaned and/or polishing, after temperature is 200～600 ℃ of preheatings, behind the constant temperature 1～3 hour, use plasma spraying equipment, powder feeding gas and working gas with step (1) are sprayed on substrate surface with nano-titanium dioxide powder, just form nano titanium dioxide film at substrate surface;
(3). the base material that step (2) is coated with nano titanium dioxide film is sintering 2～4 hours at high temperature, described high temperature is 500～600 ℃, after nano titanium dioxide film thoroughly solidifies, can obtain in conjunction with firm, stabilized nano optically catalytic TiO 2 active agent coating.
Described titanium dioxide is Detitanium-ore-type, rutile ore type or the mixing ore deposit type of the two, and the particle size distribution range of its aggregate is greatly about 10～80nm.
Employed plasma spraying equipment adopts the diatomic gas of internal powder conveying formula spray gun and ordinary purity as working gas.Can (10～80nm) direct powder feedings, if be 200～350 orders (Mesh) with the granulation of nanoclusters aggressiveness, it be easier to spray with the nanoclusters aggressiveness.
When spraying, step (1) further comprises the step of striking argon gas; At first open the argon gas valve during operation, other gas valve wouldn't be opened, the striking argon gas, treat the spray gun starting the arc after, and then carry out gas and switch to hydrogen or nitrogen and hydrogen by argon gas.Switching as the mist to nitrogen and hydrogen is to open the nitrogen valve gradually, and close simultaneously the argon gas valve gradually, working gas is switched to nitrogen by argon gas, and opens the hydrogen valve gradually, adjust to hydrogen account for nitrogen and hydrogen the mist volume 10～30%.The general gas flow of working gas is about 30～50m
3/ h, pressure are 0.5～0.7MPa.With ordinary nitrogen (N
2) be powder feeding gas.Open the powder feeding gas valve, adjust to suitable flow, start powder feeder and begin spraying.
Described plasma is a gas discharge, comprises types such as direct-current discharge, low frequency discharge, high-frequency discharge or microwave discharge.The plasma spraying nano-titanium dioxide powder is under the power of 20～50kW nano-powder to be sprayed on the base material, can adopt continuously or the discontinuous spraying coating layer thickness scope 0.5～1.2 μ m.The spray distance is 60～300mm.The powder feeding flow is 35～100g/min.
The base material that described coating is adhered to comprises various forms of metallic plates, ceramic wafer, glass plate or is the various types of base material of main component with three that as wire netting, porous ceramics or bead, metallic plate wherein comprises: steel plate, aluminium sheet, titanium plate and zine plate.
The inventor uses ultrasonic wave under operating frequency 20Hz the substrate of spraying to be carried out ultrasonic processing 120min, detects adhering in conjunction with situation of spraying sample.When expulsion rate (being sprayed onto the percentage of the powder weight on the substrate on the weight ratio of the powder that comes off)≤5.0%, the inventor thinks and can accept.
Under so high temperature (about 7000～8000 ℃ of the temperature of powder feeding mouth), can nano material change another kind of phase into mutually by a kind of? answer is yes, as the anatase phase titanium dioxide of sending into, after spray gun comes out, produce brookite type titanium dioxide sometimes, if but we want to suppress the crystal transfer of the titanium dioxide powder material that sprayed, also can accomplish.Because in the running time of Spray gun nozzle between the contact nanometer powder, the limited hot transfer time of the 1ms that only has an appointment.Perpendicular to injection direction, can be blown into cold wind at nozzle exit,, also can try every possible means to make the enthalpy stream of nozzle ejection to be the shape that gradually looses, control the crystal transfer of titanium dioxide to reduce in the time that the high-temperature region was stopped.Yet this sometimes crystal transfer also is that we are needed.As when using the anatase titanium dioxide spraying, the result has the crystal structure transition of part titanium dioxide in the gained coating be rutile-type, this nanometer titanium dioxide coating that contains the mixing crystal formation of anatase and rutile has higher photocatalytic activity sometimes, and does not influence for the physical property of coating.
Method of the present invention can be widely used in the thermal spraying of the appendix and the nano-powder of photochemical catalyst; method of the present invention is simple and convenient; the prepared material coating that goes out firmly, stable; this visible light that utilizes that can be mass-produced brings out light-catalyzed reaction; and the material with high light catalytic activity, this material has broad application prospects in photocatalysis field such as environmental protection, water treatment, air cleanings.
Description of drawings
Fig. 1. method operation chart of the present invention.
Fig. 2. method operating process schematic diagram of the present invention.
Fig. 3. the scanning electron microscope image of the coating sample of the embodiment of the invention 3.
Fig. 4. the coating sample of the embodiment of the invention 3, the powder titanium dioxide that uses and commodity P-25 photocatalytic activity relatively;
Reference numeral
1. commodity P-25
2. titanium dioxide powder
3. the plasma spraying gained coating used of the present invention
The specific embodiment
Below in conjunction with embodiment and accompanying drawing technical scheme of the present invention is further described, but cited embodiment is not to be limited embodiment.
Earlier metal aluminum sheet is carried out polishing, then be heated to 500 ℃, behind the constant temperature 3h, use plasma spraying equipment that the side of its polishing is sprayed anatase-phase nano titanium dioxide powder.Use nitrogen (N during spraying
2) and common hydrogen (H
2) mist, the volume ratio that hydrogen accounts for mist is 10%.The general gas flow of working gas is about 40m
3/ h, pressure are 0.5MPa, with ordinary nitrogen (N
2) be powder feeding gas.Its parameter is: spray is apart from 200mm, and the powder feeding flow is 60g/min, and power is 27.5kW, and the control coating layer thickness is about 1.0 μ m.After having sprayed, this aluminium sheet in 300 ℃ of following constant temperature 2h of temperature, is naturally cooled to room temperature.Substrate to spraying under operating frequency 20Hz carries out ultrasonic processing 120min, powder expulsion rate≤5wt%.
Earlier sheet glass is carried out cleaning, then be heated to 200 ℃, behind the constant temperature 2h, use plasma spraying equipment that its cleaning face is sprayed anatase-phase nano titanium dioxide powder.Use nitrogen (N during spraying
2) and common hydrogen (H
2) mist, the ratio that hydrogen accounts for the mist volume is 15%.The general gas flow of working gas is about 40m
3/ h, pressure are 0.7MPa, with ordinary nitrogen (N
2) be powder feeding gas.Its parameter is: spray is apart from 150mm, and the powder feeding flow is 50g/min, and power is 25.0kW, and the control coating layer thickness is about 0.8 μ m.After having sprayed, this sheet glass in 300 ℃ of following constant temperature 3h of temperature, is naturally cooled to room temperature.Substrate to spraying under operating frequency 20Hz carries out ultrasonic processing 120min, powder expulsion rate≤5wt%.
Earlier ceramic wafer is carried out cleaning, then be heated to 400 ℃, behind the constant temperature 2h, use plasma spraying equipment that its cleaning face is sprayed the rutile-phase nano-titanium dioxide powder.Use nitrogen (N during spraying
2) and common hydrogen (H
2) mist, the ratio that hydrogen accounts for the mist volume is 20%.The general gas flow of working gas is about 40m
3/ h, pressure are 0.6MPa, with ordinary nitrogen (N
2) be powder feeding gas.Its parameter is: spray is apart from 200mm, and the powder feeding flow is 30g/min, and power is 40.5kW, and the control coating layer thickness is about 1.0 μ m.After having sprayed, this ceramic wafer in 400 ℃ of following constant temperature 2h of temperature, is naturally cooled to room temperature.Substrate to spraying under operating frequency 20Hz carries out ultrasonic processing 120min, powder expulsion rate≤5wt%.Its scanning electron microscope image sees that accompanying drawing 3 and its photocatalytic activity relatively see accompanying drawing 4.
As can be seen from Figure 4, use coating of the present invention and coating curing technology, the photocatalytic activity of the coating of titanium dioxide that obtains is higher than the photocatalytic activity of corresponding powder, and the two catalytic activity of powder and coating is all apparently higher than the activity of commodity P-25.The test of photocatalytic activity is to weigh with the palliating degradation degree of the adsorbed methylene blue of coating surface, and Measuring Time is 240min.Used photocatalytic activity detector is that detector is estimated in the PCC-1 type photocatalysis of Japanese science and engineering vacuum Co., Ltd..
Embodiment 4
Earlier metal aluminum sheet is carried out polishing, then be heated to 600 ℃, behind the constant temperature 3h, use plasma spraying equipment that the side of its polishing is sprayed the rutile-phase nano-titanium dioxide powder.Institute's argon gas that uses (Ar) and common hydrogen (H during spraying
2) mist, the ratio that hydrogen accounts for the mist volume is 10%.The general gas flow of working gas is about 40m
3/ h, pressure are 0.6MPa, with ordinary nitrogen (N
2) be powder feeding gas.Its parameter is: spray is apart from 200mm, and the powder feeding flow is 60g/min, and power is 27.5kW, and the control coating layer thickness is about 1.0 μ m.After having sprayed, this aluminium sheet in 300 ℃ of following constant temperature 2h of temperature, is naturally cooled to room temperature.Substrate to spraying under operating frequency 20Hz carries out ultrasonic processing 120min, powder expulsion rate≤5wt%.
Embodiment 5
Earlier ceramic wafer is carried out cleaning, then be heated to 500 ℃, behind the constant temperature 3h, use plasma spraying equipment that the side of its polishing is sprayed the rutile-phase nano-titanium dioxide powder.Institute's argon gas that uses (Ar) and common hydrogen (H during spraying
2) mist, the ratio that hydrogen accounts for the mist volume is 20%.The general gas flow of working gas is about 40m
3/ h, pressure are 0.5MPa, with ordinary nitrogen (N
2) be powder feeding gas.Its parameter is: spray is apart from 200mm, and the powder feeding flow is 60g/min, and power is 27.5kW, and the control coating layer thickness is about 1.0 μ m.After having sprayed, this ceramic wafer in 500 ℃ of following constant temperature 2h of temperature, is naturally cooled to room temperature.Substrate to spraying under operating frequency 20Hz carries out ultrasonic processing 120min, powder expulsion rate≤5wt%.
Claims (10)
1. method that on base material, forms the nano titanium dioxide photocatalysis active agent coating, it is characterized in that: described method step comprises:
(1). with the mist of the mist of nitrogen and hydrogen or argon gas and hydrogen as working gas; Wherein, hydrogen accounts for 10～30% of mist volume; With nitrogen is powder feeding gas;
(2). substrate surface is cleaned and/or polishing, after temperature is 200～600 ℃ of preheatings, use plasma spraying equipment, nano-titanium dioxide powder is sprayed on substrate surface, just form nano titanium dioxide film at substrate surface with the powder feeding gas and the working gas of step (1);
(3). the base material that step (2) is coated with nano titanium dioxide film at high temperature carries out sintering, and described high temperature is 500～600 ℃, after nano titanium dioxide film thoroughly solidifies, can obtain the nano titanium dioxide photocatalysis active agent coating.
2. the method for claim 1, it is characterized in that: the particle size distribution range of the aggregate of described nano-titanium dioxide powder is 10～80nm.
3. method as claimed in claim 1 or 2 is characterized in that: described titanium dioxide is Detitanium-ore-type, rutile ore type or the mixing ore deposit type of the two.
4. the method for claim 1, it is characterized in that: the thickness of described coating is 0.5～1.2 μ m.
5. the method for claim 1, it is characterized in that: described step (1) further comprises the step of striking argon gas; At first open the argon gas valve during operation, other gas valve wouldn't be opened, the striking argon gas, treat the spray gun starting the arc after, and then carry out gas and switch to hydrogen or nitrogen and hydrogen by argon gas.
6. the method for claim 1, it is characterized in that: the discharge type of described plasma spray coating equipment is direct-current discharge, low frequency discharge, high-frequency discharge or microwave discharge.
7. the method for claim 1, it is characterized in that: described base material comprises steel plate, aluminium sheet, titanium plate, zine plate, ceramic wafer, glass plate, wire netting, porous ceramics or bead.
8. the method for claim 1 is characterized in that: the spray parameters of described plasma spraying equipment: spray is apart from being 60～300mm; The powder feeding flow is 35～100g/min; Spray gun power during spraying is 20～50kW.
9. the method for claim 1, it is characterized in that: the general gas flow of working gas is 30～50m
3/ h, pressure is 0.5～0.7MPa, is powder feeding gas with the ordinary nitrogen, the purity of gas 〉=99.9%.
10. the method for claim 1, it is characterized in that: described sintering time is 2～4 hours.
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| CNB021459258A CN1206384C (en) | 2002-10-23 | 2002-10-23 | Method for forming nano TiO2 light catalystic active agenbt coating on substrate |
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|---|---|---|---|
| CNB021459258A CN1206384C (en) | 2002-10-23 | 2002-10-23 | Method for forming nano TiO2 light catalystic active agenbt coating on substrate |
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Cited By (17)
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|---|---|---|---|---|
| CN1306059C (en) * | 2004-08-20 | 2007-03-21 | 四川大学 | Process for preparing nano coating by plasma spraying |
| CN100500304C (en) * | 2004-10-22 | 2009-06-17 | 中国科学院力学研究所 | Method and apparatus for feeding nano-particle powder evenly and quantitatively |
| CN102560325A (en) * | 2012-02-23 | 2012-07-11 | 常州天合光能有限公司 | Method for preparing nanometer titanium dioxide (TiO2) self-cleaning film |
| CN103611518A (en) * | 2013-12-06 | 2014-03-05 | 黑龙江大学 | Preparation method of sequential black mesoporous titanium dioxide visible light catalyst film |
| CN103714880A (en) * | 2013-12-10 | 2014-04-09 | 西安理工大学 | Ceramic material preventing high voltage line surface corona discharge and pollution flashover and spraying method |
| CN104941833A (en) * | 2015-06-16 | 2015-09-30 | 浙江大学 | Plasma nozzle, spray gun and spray method |
| CN105478267A (en) * | 2015-12-24 | 2016-04-13 | 浙江海洋学院 | Spraying system and method for spraying titanium dioxide film to surface of steel body in large area |
| CN105671472A (en) * | 2016-01-23 | 2016-06-15 | 苏州月辉环保科技有限公司 | Manufacturing method of novel photocatalytic plate |
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| CN107497413A (en) * | 2017-07-27 | 2017-12-22 | 东华大学 | A kind of preparation method of black titanium dioxide coating |
| CN108559939A (en) * | 2018-04-18 | 2018-09-21 | 广东省新材料研究所 | A kind of nano-titanium dioxide catalyst coatings and the preparation method and application thereof |
| CN108636394A (en) * | 2018-05-22 | 2018-10-12 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of nano titanium dioxide photocatalysis coating |
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- 2002-10-23 CN CNB021459258A patent/CN1206384C/en not_active Expired - Fee Related
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| CN1306059C (en) * | 2004-08-20 | 2007-03-21 | 四川大学 | Process for preparing nano coating by plasma spraying |
| CN100500304C (en) * | 2004-10-22 | 2009-06-17 | 中国科学院力学研究所 | Method and apparatus for feeding nano-particle powder evenly and quantitatively |
| CN102560325A (en) * | 2012-02-23 | 2012-07-11 | 常州天合光能有限公司 | Method for preparing nanometer titanium dioxide (TiO2) self-cleaning film |
| CN103611518A (en) * | 2013-12-06 | 2014-03-05 | 黑龙江大学 | Preparation method of sequential black mesoporous titanium dioxide visible light catalyst film |
| CN103714880A (en) * | 2013-12-10 | 2014-04-09 | 西安理工大学 | Ceramic material preventing high voltage line surface corona discharge and pollution flashover and spraying method |
| CN103714880B (en) * | 2013-12-10 | 2016-04-06 | 西安理工大学 | Prevent ceramic material and the spraying method of high-voltage line surface corona and pollution flashover |
| CN104941833A (en) * | 2015-06-16 | 2015-09-30 | 浙江大学 | Plasma nozzle, spray gun and spray method |
| CN105478267A (en) * | 2015-12-24 | 2016-04-13 | 浙江海洋学院 | Spraying system and method for spraying titanium dioxide film to surface of steel body in large area |
| CN105671472A (en) * | 2016-01-23 | 2016-06-15 | 苏州月辉环保科技有限公司 | Manufacturing method of novel photocatalytic plate |
| CN105728063B (en) * | 2016-03-23 | 2018-06-12 | 新奥科技发展有限公司 | A kind of preparation method of metal substrate catalyst |
| CN105728063A (en) * | 2016-03-23 | 2016-07-06 | 新奥科技发展有限公司 | Preparation method of metal substrate catalyst |
| CN107163806A (en) * | 2017-04-04 | 2017-09-15 | 郴州市泰益表面涂层技术有限公司 | It is a kind of for nano-structured coating of air purifier and preparation method thereof |
| CN107497413A (en) * | 2017-07-27 | 2017-12-22 | 东华大学 | A kind of preparation method of black titanium dioxide coating |
| CN108559939A (en) * | 2018-04-18 | 2018-09-21 | 广东省新材料研究所 | A kind of nano-titanium dioxide catalyst coatings and the preparation method and application thereof |
| CN108559939B (en) * | 2018-04-18 | 2020-08-04 | 广东省新材料研究所 | Nano titanium dioxide catalytic coating and preparation method and application thereof |
| CN108636394A (en) * | 2018-05-22 | 2018-10-12 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of nano titanium dioxide photocatalysis coating |
| CN108636394B (en) * | 2018-05-22 | 2021-01-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nano titanium dioxide photocatalytic coating |
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| CN109023366A (en) * | 2018-09-02 | 2018-12-18 | 张家港市六福新材料科技有限公司 | A kind of preparation method of hydroxyapatite-composite titania material |
| CN110170413A (en) * | 2019-05-31 | 2019-08-27 | 唐山佐仑环保科技有限公司 | A kind of spraying film-forming system of photo-catalytic sterilization glass |
| CN110170413B (en) * | 2019-05-31 | 2020-11-24 | 唐山佐仑环保科技有限公司 | Spraying film forming system of photocatalyst sterilizing glass |
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