CN104480509A - Titanium oxide film manufactured through plasma electrolysis deposition of organic aqueous solution system - Google Patents
Titanium oxide film manufactured through plasma electrolysis deposition of organic aqueous solution system Download PDFInfo
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- CN104480509A CN104480509A CN201510010573.7A CN201510010573A CN104480509A CN 104480509 A CN104480509 A CN 104480509A CN 201510010573 A CN201510010573 A CN 201510010573A CN 104480509 A CN104480509 A CN 104480509A
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Abstract
The invention relates to a technological method for preparing a titanium oxide film through plasma electrolysis deposition of an organic aqueous solution system. The method is characterized in that the organic aqueous solution electrolyte system is composed of, by percentage, 15%-40% of organic titanium, 50%-65% of organic solvents, 1%-5% of conducting media and 10%-15% of water. Preferentially, deposition parameters are as follows: the temperature of electrolyte is 30 DEG C to 100 DEG C, the electric current density is 500 mA / mm<2>-1500 mA/ mm<2>, the voltage is 1000 V-3000V, the cathode/anode area ratio is 1:1-2, and the space between the electrodes is 10 mm-20 mm. The method is mild in production condition, simple in equipment, easy to operate and low in cost, and industrial production can be achieved easily.
Description
Technical field
The present invention relates to the preparing technical field of thin film of titanium oxide material, specifically refer to that the processing method of thin film of titanium oxide material is prepared in the galvanic deposit of a kind of aqueous organopolysiloxane plasma body.
Background technology
TiO
2have and have unique optics, electricity and chemical property, being widely used in the fields such as electronics, optics and biomedicine, as can be used as optical coating or photocatalyst material, organic photocatalytic degradation can having been realized; Wet sensitive, pressure-active element and automobile exhaust sensor is used for as oxygen sensor; Utilize TiO
2the strong oxidizing property of film carries out the process of organic decomposition, sewage agricultural chemicals and promoting agent; Utilize its biocompatibility, as Artificial heart valve mould material, etc.
At present, TiO is prepared
2the technology of film mainly comprises physical method and the large class of chemical process two.Chemical process mainly contains sol-gel method, and chemical liquid phase sedimentation, spraying plating pyrolysis method etc., physical method mainly contains electron-beam vapor deposition method, magnetron sputtering method, powder charcoal etc.There are some defects in these, the titanium deoxid film prepared as sol-gel method is shaping owing to tying titanium dioxide crystal in sintering process, and the crystallization of titanium dioxide is by the impact of a lot of condition, so be difficult to the content of different crystal forms titanium dioxide film in controlling diaphragm.And processing condition are difficult to control, and are difficult to obtain thicker film.Although titanium deoxid film prepared by powder charcoal has higher photoelectric transformation efficiency, and processing condition are relatively easy to control, cost is also lower, but the top layer of titanium deoxid film of preparation and the inconsistent titanium deoxid film that result in of the moisture evaporation speed of bottom produce strong contraction, thus produce cracking phenomena.The cracking of film can make the transmission of electronics be hindered, and has a strong impact on electricity conversion.So by the preparation method that technique is simple and with low cost, the titanium deoxid film of synthesis performance excellence just seems particularly important.
Summary of the invention
The object of the invention is invention in a kind of processing method utilizing liquid phase plasma electro-deposition techniques to prepare thin film of titanium oxide in the electrolyte system of organic water solvent.
Not enough for prior art, the present invention, in organic electrolyte water solution system, prepares thin film of titanium oxide by liquid phase plasma electro-deposition techniques
The technological process that thin film of titanium oxide is prepared in liquid phase plasma galvanic deposit of the present invention is:
Plasma electrically is deposited on low-temperature atmosphere-pressure operation, and with high-purity carbon-point or platinized platinum etc. for anode, with the metal sheet such as stainless steel plate or copper for negative electrode, ratio of cathodic to anodic area is 1:1 ~ 2, and interpole gap is 10mm ~ 20 mm.Constant voltage mode or constant current mode is adopted to carry out plasma electrically electroless copper deposition operation.Before operation, pre-treatment need be carried out in workpiece (negative electrode) surface, and comprise purification and etching, polishing etc., can with reference to conventional electrodeposition job specification, comprises alkali cleaning oil removing and pickling is derusted, and electrolytic etching etc.During plasma body galvanic deposit, the electrolytic solution of anode and cathode near zone is under action of high voltage, and electrolysis forms group of bubble race.When voltage reaches a certain particular value, make bubble area produce glow discharge, in bubble, the elemental precursors to be plated of gasification is subject to electron puncture, forms the plasma body of ionization form.Plasma body obtains high-energy in argon-arc plasma field, crosses interface energy barrier under the effect of extra electric field power, is deposited on electrode (matrix) surface.After operation terminates, take out negative plate and rinse well, dry, obtain thin film of titanium oxide material.
The outer configurable heating installation of electrolyzer, keeps the temperature needed for experiment in operating process heating.Above electrolyzer, condenser is housed, for the steam of condensing reflux solvent.In addition, liquid phase plasma electric deposition device is furnished with fluid infusion system, according to circumstances supplements electrolytic solution to electrolyzer.
The composition of aqueous organopolysiloxane electrolytic solution comprises organic titanium, organic solvent, water and conducting medium, it consists of: organic titanium 15 ~ 40%, organic solvent 50 ~ 65%, conducting medium 1 ~ 5%, water 10 ~ 15%, the one in the optional mineral acid of conducting material, organic acid, inorganic salt.
Plasma electrically deposition parameter is: the temperature of electrolytic solution is 30 DEG C ~ 100 DEG C, and current density is 500mA/mm
2~ 1500mA/mm
2, voltage is 1000V ~ 3000V.
This law equipment is simple, and low-temperature atmosphere-pressure operates, and working condition is gentle, and technical process is simple, and processing ease, cost is low.The impact of hot conditions on body material of CVD (Chemical Vapor Deposition) method can be avoided, reduce internal stress, increase the bonding strength of film/base, widen the selection range of matrix.
Specific embodiments
Embodiment 1
1. the volume ratio of each component of electrolytic solution is butyl (tetra) titanate: ethanol: HCl:H
2o=25:55:5:15.
2. the processing parameter of galvanic deposit is: voltage across poles 2000 V, and current density is 900mA/mm
2, system is atmospheric operation, pH neutral range, temperature 60 DEG C, depositing time 180 min.
3. negative electrode adopts copper sheet, and anode is high-purity carbon-point, ratio of cathodic to anodic area 1:1, cathode and anode spacing 10 mm.
Embodiment 2
1. the volume ratio of each component of electrolytic solution is butyl (tetra) titanate: ethanol: HCl:H
2o=27:60:3:10.
2. the processing parameter of galvanic deposit is: voltage across poles 2200 V, and current density is 900mA/mm
2, system is atmospheric operation, pH neutral range, temperature 70 DEG C, depositing time 180 min.
3. negative electrode adopts copper sheet, and anode is high-purity carbon-point, ratio of cathodic to anodic area 1:1, cathode and anode spacing 10 mm.
Adopt energy spectrometer (EDS), X X-ray photoelectron spectroscopy X (XPS), x-ray diffractometer (XRD), Raman spectrometer to carry out analysis and characterization to thin film of titanium oxide prepared by embodiment, result shows TiO
2the Ti of film
2p1/2and Ti
2p3/2peak position at 464.5eV and 458.8eV, two peak separations are approximately 5.7eV, corresponding to Ti in titanium dioxide
4+in conjunction with energy, the price of having demarcated Ti is Ti
4+; On XRD collection of illustrative plates, there are three diffraction peaks at 25.6 °, 37.8 ° and 48.1 ° of places, correspond respectively to TiO
2standard peak position, the main component of the known film crystal grain in reference standard peak is TiO
2; Raman spectrogram can see that its characteristic peak lays respectively at 150cm
-1strong peak and be positioned at 403cm
-1, 516cm
-1, and 641cm
-1weak peak, the characteristic peak (144cm of measured peak position and Anatase
-1, 196cm
-1, 396cm
-1, 515cm
-1, and 640cm
-1) basically identical.
Claims (9)
1. organic water-soluble liquid system plasma electrically deposition prepares a processing method for thin film of titanium oxide material, it is characterized in that, in the water solution system of organic electrolyte, preparing thin film of titanium oxide by plasma body electro-deposition techniques.
2., according to claim 1, it is characterized in that liquid phase electrolyte solution is for adopting organic water-soluble liquid system, the composition of aqueous organopolysiloxane electrolytic solution comprises organic titanium, organic solvent, water and conducting medium.
3. according to claim 1, consisting of of the water solution system of organic electrolyte: organic titanium 15 ~ 40%, organic solvent 50 ~ 65%, conducting medium 1 ~ 5%, water 10 ~ 15%.
4. according to claim 1, it is characterized in that plasma body electro-deposition techniques, can constant voltage mode be adopted, also can adopt constant current mode.
5., according to claim 1, it is characterized in that the temperature of electrolytic solution in liquid phase plasma electrodeposition process remains on 30 DEG C ~ 100 DEG C.
6., according to claim 1, it is characterized in that current density is 500mA/mm in liquid phase plasma electrodeposition process
2~ 1500mA/mm
2.
7., according to claim 1, it is characterized in that voltage change region is 1000V ~ 3000V in liquid phase plasma electrodeposition process.
8. want 1 according to right, it is characterized in that working pressure remains normal pressure in liquid phase plasma electrodeposition process.
9., according to claim 1, it is characterized in that ratio of cathodic to anodic area is 1:1 ~ 2, interpole gap is 10mm ~ 20 mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568341A (en) * | 2016-02-22 | 2016-05-11 | 深圳市威勒科技股份限公司 | Tungsten oxide thin film and preparation method thereof |
| CN107385485A (en) * | 2017-07-11 | 2017-11-24 | 北京科技大学 | Large area successive sedimentation coating and surface modifying method |
-
2015
- 2015-01-09 CN CN201510010573.7A patent/CN104480509A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568341A (en) * | 2016-02-22 | 2016-05-11 | 深圳市威勒科技股份限公司 | Tungsten oxide thin film and preparation method thereof |
| CN105568341B (en) * | 2016-02-22 | 2018-08-03 | 深圳市威勒科技股份限公司 | A kind of tungsten oxide film and preparation method thereof |
| CN107385485A (en) * | 2017-07-11 | 2017-11-24 | 北京科技大学 | Large area successive sedimentation coating and surface modifying method |
| CN107385485B (en) * | 2017-07-11 | 2019-03-15 | 北京科技大学 | Large area successive sedimentation coating and surface modifying method |
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Application publication date: 20150401 |
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