CN101463470A - Method for loading TiO2 photocatalyst on ferromagnetic metal thin film - Google Patents
Method for loading TiO2 photocatalyst on ferromagnetic metal thin film Download PDFInfo
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- CN101463470A CN101463470A CNA2007101511593A CN200710151159A CN101463470A CN 101463470 A CN101463470 A CN 101463470A CN A2007101511593 A CNA2007101511593 A CN A2007101511593A CN 200710151159 A CN200710151159 A CN 200710151159A CN 101463470 A CN101463470 A CN 101463470A
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- ferromagnetic metal
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Abstract
A method for loading TiO2 photocatalyst on a ferromagnetic metallic film comprises the steps: hollow microballon particle material is taken as a substrate, ferromagnetic metal Ni or Co is taken as sputtering target material, and the metal Ni or Co is evenly coated on the hollow microballon by magnetron sputtering; then, the coated hollow microballon is taken as the material of the substrate, metal Ti as the sputtering target material, and a layer of metal Ti is evenly coated on the microballon which is plated with a metallic film by sputtering; after that, a vacuum chamber is simultaneously pumped with argon and oxygen to lead the Ti to be oxidized as TiO2 at the same time of sputtering, and the TiO2 is sedimentated on the hollow microballon coated by the metal Ni or Co. The method has the advantages that as the ferromagnetic metal materials are sedimentated on the hollow microballon, the TiO2 photochemical catalyst film material prepared by taking the ferromagnetic metal materials as the substrate can be attracted by a magnetic collector, and is convenient for centralized collection when not in use, so that the metallic film can be recycled, saves resource and avoids the secondary pollution for the environment.
Description
(1) technical field
The present invention relates to a kind of technique for vacuum coating, particularly a kind of with TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film.
(2) background technology
Administer the pollution of water body in recent years, become the countries in the world questions of common interest, it should be noted that anatase octahedrite phase TiO
2The light-catalyzed reaction organic pollutant in the degradation water effectively, this technology has become a kind of sewage water treatment method that the important application prospect is arranged.The relevant TiO of utilization that is reporting
2In the research of noxious pollutant, that great majority adopt is TiO in the photocatalytic degradation water
2Microparticulate suspension system, because the petroleum-type organic pollutant is water insoluble and swim on the water surface, and water-fast TiO
2Density greater than water, therefore can be sunken to the bottom, if adopt this suspension system can not make TiO
2Give full play to the effect of photocatalyst.In order to make TiO
2Can fully contact with the pollutent on swimming in the water surface and carry out light-catalyzed reaction, it need be loaded on a kind of density less than water, can make TiO
2Well attached and not by TiO
2On the carrier of photochemical catalytic oxidation.This seminar is at the patent of invention of first to file " a kind of method at cenosphere surface vacuum plating titanium deoxid film " (application number: 200610015533.2) then be invention at this problem.Because the pollution of water body often is in very open waters, after the input photocatalyst is finished the organism decomposition, be very big problem to its recovery, and nano-TiO
2Reside in the water and also can cause secondary pollution, so nano-TiO
2If can not resolve with separating of water body, greatly restricted T iO with the recovery problem
2Being extensive use of of photocatalyst.
(3) summary of the invention
The objective of the invention is the problem that exists in the above-mentioned technology, provide a kind of TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film, thereby makes a kind of new floating supported titanium
2Photocatalyst, it is as TiO
2Photocatalyst can efficient degradation water surface organic pollutant, can utilize magnetic collector very easily with its recovery again simultaneously, has avoided powder TiO
2Photocatalyst waste and to the secondary pollution of water body.
Technical scheme of the present invention:
A kind of with TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film, adopt the preparation of microparticle magnetron sputtering film device, it is characterized in that: at first do substrate with the cenosphere particulate material, with ferromagnetic metal Ni or Co is sputtering target material, by in vacuum chamber, charging into argon gas and adopting direct current, radio frequency or pulse sputter, metal Ni or Co evenly are coated on the cenosphere surface; The cenosphere that coated with metal Ni or Co is a base material again, as sputtering target material, feeds argon gas with metal Ti in vacuum chamber, adopts d.c. sputtering to make and evenly coats layer of metal Ti on the bead surface that is coated with metallic film; Open oxygen control valve then, aerating oxygen in vacuum chamber makes oxygen in Ti and the vacuum chamber react in splash-proofing sputtering metal Ti and generates TiO
2, and be deposited on by the cenosphere surface of ferromagnetic metal Ni or Co coating.
In aforesaid method, the concrete processing condition of deposited iron magnetic metallic film are: the vacuum tightness in vacuum chamber reaches 1.0 * 10
-3～4.0 * 10
-3During Pa, charge into the argon gas that purity is 4N in vacuum chamber, the operating pressure of setting in the vacuum chamber is 0.3～5Pa, and the electric current of direct supply is 0.2～1.5A, and sputtering power is 50～600W, and base reservoir temperature is a room temperature, and sputtering time is 20～60 minutes; Depositing Ti O
2The concrete processing condition of film are: the vacuum tightness in vacuum chamber reaches 1.0 * 10
-3～4.0 * 10
-3During Pa, at first charge into high-purity argon gas in vacuum chamber, the operating pressure of setting in the vacuum chamber is 0.3～5Pa, and the electric current of direct supply is 0.2～1.5A, sputtering power is 50～1000W, base reservoir temperature is 150～400 ℃, and sputtering time is 10-30 minute, after bead particles is coated by metal titanium membrane fully, aerating oxygen in vacuum chamber, and the flow proportional of adjusting argon gas and oxygen is between 3～5:1, and other condition remains unchanged, sputtering time 2～16 hours.
In aforesaid method, ferromagnetic metal Ni, Co target are that diameter 100mm, thickness are no more than 3mm, purity 99.9%; The Ti sputtering target material is diameter 100mm, thickness 5mm, purity 99.9%; Target requires bright and clean, the inner even compact of surfacing and nothing is mingled with and the space.
Advantage of the present invention is: 1) by at cenosphere surface deposition ferromagnetic metal thin film, make the cenosphere can be by attraction, and cenosphere density is littler than water, and floatability is preferably arranged on the water surface, the recovery after easy to use; 2) at reactive sputter-deposition TiO
2On cenosphere, deposit layer of metal Ti film before earlier, prevent that ferromagnetic metal thin film is oxidized to sull in the subsequent reaction sputter procedure; 3) processing condition such as flow by changing operating air pressure in the vacuum chamber, sputtering power, temperature, argon gas and sputtering time, can be on the cenosphere surface deposition of different-grain diameter the ferromagnetic metal thin film of different thickness.
(4) embodiment
Embodiment 1:
A kind of with TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film, adopts the preparation of microparticle magnetron sputtering film device, is that 1～100 μ m, median size are that 80 μ m, density of material are about 0.3g/cm with the 1g particle size range
3The cenosphere particulate material do substrate, this cenosphere is taken from the pearl that floats in thermal power plant's flyash.Before implementing plated film, preliminary cleaning is carried out on the cenosphere surface handled, treatment step is 1) at first cenosphere is cleaned with scavenging solution, stir and left standstill 3 minutes after 10 minutes, remove down clear liquid afterwards, use washed with de-ionized water then three times; 2) under 50-70 ℃, soak and abundant the stirring 15 minutes, use washed with de-ionized water then three times with weakly alkaline solution; 3) at room temperature soak also fully stirring 15 minutes, then with washed with de-ionized water three times and filtration with weakly acid soln; 4) cenosphere after will handling is put into 105 ℃ baking oven baking and is taken out standby after 4 hours.
Make sputtering target material with diameter 100mm, thickness 3mm, purity 99.9%, surfacing is bright and clean and inner nothing is mingled with pore metal Ni; Concrete processing condition are: at first with metal Ni as target, the vacuum tightness in vacuum chamber reaches 1.0 * 10
-3During Pa, charge into high-purity argon gas in vacuum chamber, the setting operating pressure is 1.2Pa, and base reservoir temperature is a room temperature, sputtering target electric current 0.5A, and target voltage 320V, sputtering power are 160W, sputtering time 30 minutes; The metal Ti target shut down to be changed as sputtering target and vacuumize in the deposition back that finishes, and the vacuum tightness in vacuum chamber reaches 1.0 * 10
-3During Pa, charge into high-purity argon gas in vacuum chamber, the setting operating pressure is 1.2Pa, and base reservoir temperature is 300 ℃, sputtering target electric current 1.2A, and target voltage 400V, sputtering power are 480W, sputtering time 10 minutes; Open oxygen control valve then, regulate argon flow amount when vacuum chamber feeds high purity oxygen gas, the air pressure in the vacuum chamber is remained unchanged, and make the throughput ratio of argon gas oxygen maintain 4:1, sputtering time is 480 minutes.
By scanning electronic microscope (Germany Leo 1530VP) cenosphere before and after the plated film is compared observation, find that bead surface has coated the film of one deck even compact, high power is amplified observation and is found that film presents obvious island growth, and the increase of sample specific surface area is nearly one times behind the specific surface test shows plated film.The sample that is obtained is carried out X-ray diffraction (GermanyBruker D8Advance, Cu target, K α, λ=1.54056
) analyze, find to occur altogether eight main diffraction peaks, cenosphere body (Mullite) diffraction peak does not occur, wherein three 2 θ angles equal 44.38,51.68 and 76.29 diffraction peak respectively, correspond respectively to (111) of the metal Ni (PDF card:040850) of FCC structure, the diffraction of (200) and (220) crystal face, the sedimentary metal Ni of the first step that hence one can see that exists with metallic state, oxidation does not take place, show the cenosphere surface on the plating evenly continuously, the metal Ni film of strong adhesion.In diffracting spectrum, do not find the diffraction peak of pure metal Ti in addition, the very thin also complete crystallization not of metal Ti film is described, perhaps in process subsequently, be oxidized into TiO
2And 2 θ angles equal five diffraction peaks of 25.25,37.61,47.91,53.96,62.67 corresponding to anatase octahedrite phase TiO
2The diffraction of (101) of (PDF card:894921), (004), (200), (105) and (204) crystal face can the sedimentary film of proved response sputter be anatase octahedrite phase TiO thus
2We carry out Raman spectrum (BritishRenishaw RM2000 with sample in addition, λ=514.5nm) analyze, choose in the sample any single cenosphere and carry out the test of microcell Raman spectrum, four raman signatures frequency displacements that obtained are respectively 141.2,393.4,518.8 and 636.3cm
-1, itself and anatase octahedrite TiO mutually
2The feature Raman frequency shift identical, with this also provable glass microsphere surface fully by anatase octahedrite phase TiO
2Coat.
Embodiment 2:
A kind of method that the TiO2 photocatalyst is carried on ferromagnetic metal thin film, adopt the preparation of microparticle magnetron sputtering film device, the concrete steps of plated film are identical with embodiment 1, but metal refining Co on cenosphere at first, pulse power frequency is 30KHz, power 400W, other condition is with metal refining Ni in the example 1.The second step metal refining Ti is with example 1, and only power supply is the pulse power, and power is 400W.The 3rd step deposition thin film of titanium oxide condition is: charge into argon gas and oxygen in vacuum chamber simultaneously, the flow proportional of adjusting argon gas and oxygen is 4:1, and the operating pressure in the vacuum chamber is 1.2Pa, and pulse power frequency is 30KHz; Sputtering power is 600W; Base reservoir temperature is 150 ℃; Sputtering time is 600 minutes.Other condition is with example 1.This sample is by SEM, and XRD and Raman detect, and the result shows, on the same plating in cenosphere surface evenly continuously, the metal Co film of strong adhesion and anatase octahedrite TiO mutually
2Film.
Claims (3)
1. one kind with TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film, adopt the preparation of microparticle magnetron sputtering film device, it is characterized in that: at first do substrate with the cenosphere particulate material, with ferromagnetic metal Ni or Co is sputtering target material, by in vacuum chamber, charging into argon gas and adopting direct current, radio frequency or pulse sputter, metal Ni or Co evenly are coated on the cenosphere surface; The cenosphere that coated with metal Ni or Co is a base material again, as sputtering target material, feeds argon gas with metal Ti in vacuum chamber, adopts d.c. sputtering to make and evenly coats layer of metal Ti on the bead surface that is coated with metallic film; Open oxygen control valve then, aerating oxygen in vacuum chamber makes oxygen in Ti and the vacuum chamber react in splash-proofing sputtering metal Ti and generates TiO
2, and be deposited on by the cenosphere surface of ferromagnetic metal Ni or Co coating.
2. according to claim 1 with TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film, and it is characterized in that the concrete processing condition of deposited iron magnetic metallic film are: the vacuum tightness in vacuum chamber reaches 1.0 * 10
-3～4.0 * 10
-3During Pa, charge into the argon gas that purity is 4N in vacuum chamber, the operating pressure of setting in the vacuum chamber is 0.3～5Pa, and the electric current of direct supply is 0.2～1.5A, and sputtering power is 50～600W, and base reservoir temperature is a room temperature, and sputtering time is 20～60 minutes; Depositing Ti O
2The concrete processing condition of film are: the vacuum tightness in vacuum chamber reaches 1.0 * 10
-3～4.0 * 10
-3During Pa, at first charge into high-purity argon gas in vacuum chamber, the operating pressure of setting in the vacuum chamber is 0.3～5Pa, and the electric current of direct supply is 0.2～1.5A, sputtering power is 50～1000W, base reservoir temperature is 150～400 ℃, and sputtering time is 10-30 minute, after bead particles is coated by metal titanium membrane fully, aerating oxygen in vacuum chamber, and the flow proportional of adjustment argon gas and oxygen is 3～5: between 1, other condition remains unchanged, sputtering time 2～16 hours.
3. according to claim 1 with TiO
2Photocatalyst is carried on the method for ferromagnetic metal thin film, it is characterized in that: ferromagnetic metal Ni, Co target are that diameter 100mm, thickness are no more than 3mm, purity 99.9%; The Ti sputtering target material is diameter 100mm, thickness 5mm, purity 99.9%; Target requires bright and clean, the inner even compact of surfacing and nothing is mingled with and the space.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101511593A CN101463470A (en) | 2007-12-21 | 2007-12-21 | Method for loading TiO2 photocatalyst on ferromagnetic metal thin film |
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|---|---|---|---|
| CNA2007101511593A CN101463470A (en) | 2007-12-21 | 2007-12-21 | Method for loading TiO2 photocatalyst on ferromagnetic metal thin film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104772166A (en) * | 2015-03-31 | 2015-07-15 | 嘉兴学院 | Composite floating bead photocatalyst as well as preparation method and application thereof |
| CN108659536A (en) * | 2018-03-23 | 2018-10-16 | 昆山德睿懿嘉电子材料科技有限公司 | Heat Conduction Material and preparation method thereof |
-
2007
- 2007-12-21 CN CNA2007101511593A patent/CN101463470A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104772166A (en) * | 2015-03-31 | 2015-07-15 | 嘉兴学院 | Composite floating bead photocatalyst as well as preparation method and application thereof |
| CN108659536A (en) * | 2018-03-23 | 2018-10-16 | 昆山德睿懿嘉电子材料科技有限公司 | Heat Conduction Material and preparation method thereof |
| CN108659536B (en) * | 2018-03-23 | 2020-11-06 | 昆山德睿懿嘉电子材料科技有限公司 | Heat conducting material and preparation method thereof |
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Open date: 20090624 |