CN103924280A - Molybdenum and carbon-codoped titanium oxide nanotube array thin film material and preparation method thereof - Google Patents
Molybdenum and carbon-codoped titanium oxide nanotube array thin film material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of an environmental material, and particularly relates to a molybdenum and carbon-codoped titanium oxide nanotube array thin film material and a preparation method thereof. The molybdenum and carbon codoping of a titanium oxide nanotube can be realized by introducing molybdenum element into the titanium oxide nanotube formed on a titanium sheet and the surface thereof through alloying, and then introducing carbon element through carbon monoxide atmospheric thermal treatment; in the obtained molybdenum and carbon-codoped titanium oxide nanotube array thin film material, a part of titanium atoms in the titanium oxide nanotube are replaced by molybdenum, a part of oxygen atoms are replaced by carbon, the ratio of the molybdenum atoms to carbon atoms ranges from 0.03 to 0.15, and the ratio of the doped carbon atoms to titanium atoms ranges from 0.01 to 0.09. The thin film material is attached to a titanium alloy substrate, and comprises orderly titanium oxide nanotubes perpendicular to the substrate. The photocatalysis and photo-electrochemical properties of the thin film material in visible light are far higher than those of the traditional titanium oxide thin film material, and the thin film material has excellent application prospects on the aspects of photocatalytically degrading organic matters in water and reducing heavy metal ions.
Description
Technical field
The invention belongs to environmentally conscious materials technical field, carbon co-doped titania nanotube array film material of concrete a kind of molybdenum and preparation method thereof.
Background technology
Photocatalysis technology is having huge using value aspect environmental pollution improvement and clear energy sources production, and its Research Emphasis is to design and synthesize efficient photocatalyst material.As a kind of good photocatalyst, TiO
2practical application still face two key issues, without visible light-responded and lower photocatalysis efficiency.Large quantity research shows, by TiO
2carry out suitable doping and appearance structure control, can improve its visible absorption ability and photocatalysis performance.
TiO
2the special construction of nano-tube array makes it have series of advantages, its ordered structure and thin-walled characteristic can improve the rate of migration of photo-generated carrier, shorten migration path, reduce the recombination probability in light induced electron and hole, thereby increase the touch opportunity of itself and goal response thing, improve photocatalysis efficiency.In addition TiO,
2nano-tube array also has the advantages such as high-specific surface area, high porosity, is conducive to diffusion and the absorption of reactant on its surface, and effective incident and the utilization of light.Due to above plurality of advantages, TiO
2nano-tube array has broad application prospects in photochemical catalysis and photoelectrochemistry field, in recent years about TiO
2the action oriented research of nano-tube array is also more and more.But, titanium dioxide itself without visible light-responded drawbacks limit TiO
2nano-tube array is in the application of photocatalysis field.In solar spectrum, having high-octane ultraviolet content is only 5% left and right, and the content of visible ray is up to 45%, in order to improve TiO
2the utilization ratio of nano-tube array to sunlight, must improve its visible absorption ability.
Transition metal (V, Mo, W etc.) is to improve TiO with nonmetal (N, C etc.) codoped
2the effective way of visible absorption ability and photocatalysis performance, it is at TiO
2also Worth Expecting of application on nano-tube array.But anonizing is prepared TiO
2the process characteristic of nano-tube array makes the very difficult form Uniform Doped with metal ion of transition metal to TiO
2in lattice, transition metal/nonmetal codoped also just cannot be realized.Up to the present, do not see the report about transition metal/non-metallic element codoping titanium oxide nano-tube array.
Summary of the invention
The object of the present invention is to provide carbon co-doped titania nanotube array film material of a kind of molybdenum and preparation method thereof, the photochemical catalysis of this thin-film material under visible ray and photoelectrochemical behaviour are far above conventional oxidation titanium thin-film material, and in photocatalytic degradation water, organism and reducing heavy metal ions have a good application prospect.
Technical scheme of the present invention is:
The carbon co-doped titania nanotube array film material of a kind of molybdenum, this thin-film material is attached to titanium maxter alloy substrate, is made up of the orderly titanium oxide nanotubes perpendicular to substrate.
The carbon co-doped titania nanotube array film material of described molybdenum, the partial-titanium atom in titanium oxide nanotubes is substituted by molybdenum, and partial oxygen atom is substituted by carbon, and molybdenum titanium atom is than between 0.03～0.15, and the atomic ratio of doping carbon and titanium is between 0.01～0.09.
The carbon co-doped titania nanotube array film material of described molybdenum, the thickness of this thin-film material is 0.5～6 μ m, and nanotube caliber is 50～120 μ m, and the crystalline structure of titanium oxide nanotubes is anatase octahedrite.
The preparation method of the carbon co-doped titania nanotube array film material of described molybdenum, first adopt alloying to prepare titanium maxter alloy, then at fluorine-containing electrolytic solution Anodic Oxidation titanium maxter alloy sheet, finally thermal treatment in air and carbon monoxide atmosphere successively, obtains the carbon co-doped titania nanotube array film material of molybdenum.
The preparation method of the carbon co-doped titania nanotube array film material of described molybdenum, concrete steps are as follows:
(1) at 1000 DEG C ± 50 DEG C, Ti-xMo alloy is carried out to homogenizing and process 2～4 hours, 2.5≤x≤10 in Ti-xMo alloy, then quench and obtain single-phase titanium maxter alloy;
(2) by after titanium maxter alloy section polishing, moisture Neutral ammonium fluoride/ethylene glycol electrolytic solution Anodic Oxidation 0.5～4 hour, anodised operating voltage is 20～30V, and obtaining thickness on titanium maxter alloy surface is that 0.5～6 μ m, caliber are that 50～120 μ m, molybdenum titanium atom are than the amorphous titanium peroxide nano-tube array that is 0.03～0.15; In this electrolytic solution, the massfraction of Neutral ammonium fluoride is 0.2%～1%, and the volume fraction of water is 2～4%;
(3) by the amorphous titanium peroxide nano-tube array that contains molybdenum element in air in 450～500 DEG C of thermal treatments 1～3 hour, obtain the Anatase titania nanotube array of molybdenum doping, then 500 DEG C～600 DEG C thermal treatment 2～4 hours in carbon monoxide atmosphere, obtains the carbon co-doped Anatase titania nanotube array film of molybdenum.
Advantage of the present invention and beneficial effect are as follows:
1, the material that prepared by the present invention and traditional TiO
2the difference of nano-tube array is, the molybdenum of successfully having realized Nano tube array of titanium dioxide is carbon co-doped, and the carbon co-doped titania nanotube array of molybdenum shows following advantage:
1. the synergistic effect of the carbon co-doped generation of molybdenum makes bill of material reveal good visible absorption ability, thereby makes it produce the prerequisite that possesses visible light catalytic ability;
2. the photoelectrochemical behaviour that the carbon co-doped titania nanotube array film of molybdenum shows under visible ray and simulated solar irradiation is obviously better than unadulterated TiO
2film of Nano tube array;
3. the carbon co-doped titania nanotube array film of molybdenum under visible ray to the degradation efficiency of methylene blue far above unadulterated TiO
2film of Nano tube array;
4. the efficiency of the carbon co-doped titania nanotube array film of molybdenum reduction of hexavalent chromium under visible ray is apparently higher than unadulterated TiO
2film of Nano tube array.
2, the present invention is heat-treated to merit by alloying and atmosphere and has prepared the carbon co-doped titania nanotube array film of molybdenum with good visible light catalytic performance, not only for Degradation of Organo-pollutants in Water with Photo-catalysis and reducing heavy metal ion provide a kind of selection, and provide a kind of TiO
2the method of nano-tube array doping vario-property.
3, the present invention has prepared the titania nanotube array film containing molybdenum by anodic oxidation titanium maxter alloy, and has successfully prepared a kind of carbon co-doped titania nanotube array film of molybdenum with visible absorption ability and visible light catalytic performance by atmosphere heat treatment.
Brief description of the drawings
Fig. 1 is the FESEM photo (a: top view, b: side-view) of the carbon co-doped titania nanotube array film of molybdenum.
Fig. 2 is XPS High Resolution Spectrum and the fitting data (a:Ti2p, b:Mo3d) thereof of the carbon co-doped titania nanotube array film of molybdenum.Wherein, X-coordinate Binding Energy is that ordinate zou N is photoelectron intensity in conjunction with energy.
Fig. 3 is the carbon co-doped (Mo/C-TiO of molybdenum
2) and (TiO that do not adulterate
2) the optical absorption spectra contrast of titania nanotube array film.Wherein, X-coordinate Wavelength is wavelength, and ordinate zou Absorbance is absorbancy.
Fig. 4 is molybdenum density of photocurrent contrast carbon co-doped and that nanotube array intermingling titanium oxide film does not produce as light anode (a:100mW/cm
2simulated solar irradiation, b: filter the simulated solar irradiation that wavelength is less than 400nm part).Wherein, X-coordinate Potential is bias voltage, and ordinate zou Current Density is current density.
Fig. 5 is an attenuation function matched curve of the carbon co-doped titania nanotube array film of molybdenum degradation of methylene blue under visible ray.Wherein, X-coordinate Interaction time is the reaction times, ordinate zou C/C
0for remaining rate.Three matched curves in Fig. 5 represent respectively: only have visible ray (visible light only), TiO
2visible ray (TiO
2and Mo/C-TiO light)
2visible ray (Mo/C-TiO
2light).
Fig. 6 is Cr (VI) reduction efficiency of the carbon co-doped titania nanotube array film of molybdenum under visible ray.Wherein, X-coordinate is sample number into spectrum, and ordinate zou is clearance.
Embodiment
First the present invention adopts alloying to obtain uniform titanium maxter alloy, then at fluorine-containing electrolytic solution Anodic Oxidation titanium maxter alloy sheet, form on its surface the titania nanotube array film that one deck contains molybdenum element, finally thermal treatment in air and carbon monoxide atmosphere successively, obtain the carbon co-doped Anatase titania nanotube array film of molybdenum, and its visible absorption ability and photocatalysis performance are tested.Wherein, the concrete preparation process of the carbon co-doped titania nanotube array film material of molybdenum is as follows:
(1) at 1000 DEG C ± 50 DEG C, Ti-xMo (2.5≤x≤10) alloy is carried out to homogenizing and process 2～4 hours, then quench and obtain single-phase titanium maxter alloy.By after titanium maxter alloy section polishing, at moisture Neutral ammonium fluoride/ethylene glycol electrolytic solution, (massfraction of Neutral ammonium fluoride is 0.2%～1%, the volume fraction of water is 2～4%) Anodic Oxidation 0.5～4 hour, anodised operating voltage is 20～30V, and obtaining thickness on titanium maxter alloy surface is that 0.5～6 μ m, caliber are that 50～120 μ m, molybdenum titanium atom are than the amorphous titanium peroxide nano-tube array that is 0.03～0.15.
(2) by the amorphous titanium peroxide nano-tube array that contains molybdenum element in air in 450～500 DEG C of thermal treatments 1～3 hour, obtain the Anatase titania nanotube array of molybdenum doping, then 500 DEG C～600 DEG C thermal treatment 2～4 hours in carbon monoxide atmosphere, obtains the carbon co-doped Anatase titania nanotube array film of molybdenum.
The present invention utilizes alloying to introduce molybdenum element in the titanium oxide nanotubes of titanium sheet and surface formation thereof, introduce carbon by carbon monoxide atmosphere thermal treatment again, the molybdenum of realizing titanium oxide nanotubes is carbon co-doped, in the carbon co-doped titania nanotube array film material of molybdenum obtaining, partial-titanium atom in titanium oxide nanotubes is substituted by molybdenum, partial oxygen atom is substituted by carbon, and molybdenum titanium atom is than between 0.03～0.15, and the atomic ratio of doping carbon and titanium is between 0.01～0.09.The thickness of this thin-film material is 0.5～6 μ m, and nanotube caliber is 50～120 μ m, and the crystalline structure of titanium oxide nanotubes is anatase octahedrite.The feature of this thin-film material is as follows:
1. this thin-film material have loose porous, specific surface area is large, structurally ordered, caliber and the advantage such as thickness is controlled, composition is controlled, and makes a concerted effort by force with substrate junction, is a kind of desirable photocatalyst material and photoelectric chemical electrode material.2. this thin-film material visible absorption ability obviously improves, and the photoelectrochemical behaviour under visible ray and simulated solar irradiation is obviously better than unadulterated film of Nano tube array of titanium dioxide.3. the ability of this thin-film material photocatalytic degradation methylene blue under visible ray is far above unadulterated film of Nano tube array of titanium dioxide.4. this thin-film material under visible ray the chromic ability of photo catalytic reduction higher than unadulterated film of Nano tube array of titanium dioxide.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
To after the thermal treatment of Ti-5Mo alloy, obtain single phase structure, section, polishing, then under 30V operating voltage, be 0.3% at Neutral ammonium fluoride massfraction, volume of water mark is 3% ethylene glycol solution Anodic Oxidation 2h, obtains thickness approximately 2.4 μ m, the about 80nm of caliber, molybdenum titanium atom than the titania nanotube array film that is 0.068.By containing the titania nanotube array film of molybdenum in air in 500 DEG C of thermal treatments 2 hours, obtain the titania nanotube array film of molybdenum doping.By molybdenum nanotube array intermingling titanium oxide film in carbon monoxide atmosphere in 550 DEG C of thermal treatments 3 hours, obtain carbon titanium atom than the carbon co-doped titania nanotube array of molybdenum that is 0.08 (see Fig. 1,2 and table 1).
The composition analysis result of the carbon co-doped titania nanotube array of table 1 molybdenum
| Element or atomic ratio | Ti | O | Mo | C doped | Mo/Ti | C doped/Ti |
| Weight, % | 48.9 | 35.9 | 14.2 | 1.0 | - | - |
| Atom, % | 29.2 | 64.2 | 4.24 | 2.36 | 0.145 | 0.081 |
In table 1, C
dopedrepresentative doping state carbon atom, C
dopedthe atomic ratio of/Ti representative doping state carbon and titanium.
Can be found out by Fig. 1, Fig. 2 and table 1, after treatment, Ti-5Mo alloy slice surface forms uniform titania nanotube array film, and (b), film thickness is about 2.4 μ m for Fig. 1 a, Fig. 1, and caliber is about 80nm.XPS photoelectron spectrum shows that (b), in film, part titanium atom and carbon atom form Ti-C key for Fig. 2 a, Fig. 2, and carbon atom has successfully been doped in titanium oxide lattice with the form of replace oxygen atom; Molybdenum is realized doping with the form of instead of titanium atom.The demonstration of composition analysis result, the molybdenum titanium atom ratio in thin-film material is 0.145, the atomic ratio of doping state carbon and titanium is 0.081.
Embodiment 2
Utilize UV-vis2550 ultraviolet-visible spectrophotometer to measure the absorption spectrum of the carbon co-doped titania nanotube array film of molybdenum, and compare with the not nanotube array intermingling titanium oxide film of same thickness.Result shows, the visible absorption ability of the carbon co-doped titania nanotube array film of molybdenum is far above unadulterated titania nanotube array film (seeing Fig. 3).
Embodiment 3
Taking intensity as 100mW/cm
2simulated solar irradiation be light source, the metabisulfite solution of 0.2M is electrolytic solution, the carbon co-doped titania nanotube array film of molybdenum is light anode, investigates its photoelectrochemical behaviour under simulated solar irradiation.Result shows, the density of photocurrent of the carbon co-doped titania nanotube array film of molybdenum is 400mA/cm
2, more than high 2 doubly (see Fig. 4 a) than unadulterated sample.
Embodiment 4
Be less than the simulated solar irradiation (100mW/cm of 400nm part to filter wavelength
2) be light source, the metabisulfite solution of 0.2M is electrolytic solution, the carbon co-doped titania nanotube array film of molybdenum is light anode, investigates its visible light-responded ability.Result shows, the carbon co-doped titania nanotube array film of molybdenum shows higher visible light-responded ability than doped samples not, and its density of photocurrent is 132 μ A/cm
2, (see Fig. 4 b) than high 6 times of the latter.
Embodiment 5
Taking the carbon co-doped and unadulterated titania nanotube array film of molybdenum as photocatalyst, the methylene blue solution that concentration is 2ppm is that target contaminant is 3mW/cm in intensity
2visible ray under carry out photocatalytic degradation experiment
Result shows, the carbon co-doped titania nanotube array film of molybdenum has improved 5 times to the degradation rate of methylene blue than unadulterated titania nanotube array film, shows the visible light catalytic performance (seeing Fig. 5 and table 2) far above the latter.
An attenuation function fitting data of table 2 methylene blue degradation curve
| Sample | Coefficient | Diminution factor | R 2 |
| Nothing | 1 | 1.413×10 -3min -1 | 0.9968 |
| TiO 2 | 1 | 2.100×10 -3min -1 | 0.9850 |
| Mo/C-TiO 2 | 1 | 1.272×10 -2min -1 | 0.9979 |
In table 2, R
2represent significance coefficient of determination, its value more approaches 1, represents that methylene blue degradation rule meets attenuation function (C/C one time
0=ae
-bt) degree higher.
Can be found out by Fig. 5 and table 2, the photocatalysis performance of the carbon co-doped titania nanotube array film of molybdenum under visible ray is far above unadulterated titania nanotube array film, and its degradation rate to methylene blue is about 6 times of the latter.
Embodiment 6
Taking the carbon co-doped and unadulterated titania nanotube array film of molybdenum as photocatalyst, the sexavalent chrome solution (potassium bichromate) that concentration is 5ppm is target contaminant, is 10mW/cm in intensity
2visible ray under carry out photo catalytic reduction Cr (VI) experiment.Result shows, the carbon co-doped titania nanotube array film of molybdenum has improved nearly 6 times (seeing Fig. 6) to the reduction efficiency of Cr (VI) than unadulterated titania nanotube array film.
Embodiment result shows, the present invention adopts specific method to prepare to have the carbon co-doped titanium oxide porous film material of visible light-responded novel Mo, and this thin-film material is attached to titanium alloy substrate, is made up of the orderly titanium oxide nanotubes perpendicular to substrate.Compared with existing film of Nano tube array of titanium dioxide, partial-titanium atom in the carbon co-doped titanium oxide nanotubes of molybdenum is substituted by molybdenum atom, partial oxygen ion is substituted by carbon atom, consisting of the visible absorption ability of thin-film material obviously strengthen, the photocatalysis performance under visible ray condition significantly promotes.
Claims (5)
1. the carbon co-doped titania nanotube array film material of molybdenum, is characterized in that, this thin-film material is attached to titanium maxter alloy substrate, is made up of the orderly titanium oxide nanotubes perpendicular to substrate.
2. according to the carbon co-doped titania nanotube array film material of molybdenum claimed in claim 1, it is characterized in that, partial-titanium atom in titanium oxide nanotubes is substituted by molybdenum, partial oxygen atom is substituted by carbon, molybdenum titanium atom is than between 0.03～0.15, and the atomic ratio of doping carbon and titanium is between 0.01～0.09.
3. according to the carbon co-doped titania nanotube array film material of molybdenum claimed in claim 1, it is characterized in that, the thickness of this thin-film material is 0.5～6 μ m, and nanotube caliber is 50～120 μ m, and the crystalline structure of titanium oxide nanotubes is anatase octahedrite.
4. the preparation method of the carbon co-doped titania nanotube array film material of molybdenum claimed in claim 1, it is characterized in that, first adopt alloying to prepare titanium maxter alloy, then at fluorine-containing electrolytic solution Anodic Oxidation titanium maxter alloy sheet, finally thermal treatment in air and carbon monoxide atmosphere successively, obtains the carbon co-doped titania nanotube array film material of molybdenum.
5. according to the preparation method of the carbon co-doped titania nanotube array film material of molybdenum claimed in claim 4, it is characterized in that, concrete steps are as follows:
(1) at 1000 DEG C ± 50 DEG C, Ti-xMo alloy is carried out to homogenizing and process 2～4 hours, 2.5≤x≤10 in Ti-xMo alloy, then quench and obtain single-phase titanium maxter alloy;
(2) by after titanium maxter alloy section polishing, moisture Neutral ammonium fluoride/ethylene glycol electrolytic solution Anodic Oxidation 0.5～4 hour, anodised operating voltage is 20～30V, and obtaining thickness on titanium maxter alloy surface is that 0.5～6 μ m, caliber are that 50～120 μ m, molybdenum titanium atom are than the amorphous titanium peroxide nano-tube array that is 0.03～0.15; In this electrolytic solution, the massfraction of Neutral ammonium fluoride is 0.2%～1%, and the volume fraction of water is 2～4%;
(3) by the amorphous titanium peroxide nano-tube array that contains molybdenum element in air in 450～500 DEG C of thermal treatments 1～3 hour, obtain the Anatase titania nanotube array of molybdenum doping, then 500 DEG C～600 DEG C thermal treatment 2～4 hours in carbon monoxide atmosphere, obtains the carbon co-doped Anatase titania nanotube array film of molybdenum.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637350A (en) * | 2016-12-08 | 2017-05-10 | 西南交通大学 | Preparation method of molybdenum-doped titanium dioxide nano-tube array thin film |
| CN106731881A (en) * | 2016-12-20 | 2017-05-31 | 济南大学 | Based on metal, nonmetallic codope nTiO2Visible light catalytic hollow fiber ultrafiltration membrane and preparation method |
| CN108396381A (en) * | 2017-02-04 | 2018-08-14 | 中国科学院金属研究所 | A kind of optical drive shape-changing material and its preparation method and application |
| CN109482173A (en) * | 2017-09-11 | 2019-03-19 | 中国科学院金属研究所 | A kind of bulk phase-doped nano-photocatalyst material and its preparation method and application |
| CN109569574A (en) * | 2017-09-28 | 2019-04-05 | 中国科学院金属研究所 | A kind of body phase codope visible-light photocatalysis material and its preparation method and application |
| CN110129730A (en) * | 2019-06-03 | 2019-08-16 | 复旦大学 | A kind of preparation method of molybdenum doping titanium dioxide nano-pipe array thin film |
| CN110653348A (en) * | 2018-06-29 | 2020-01-07 | 南京理工大学 | Titanium-based amorphous nanotube and preparation method thereof |
| CN110656257A (en) * | 2018-06-29 | 2020-01-07 | 南京理工大学 | Method for preparing nano porous gold based on titanium-based amorphous alloy |
| CN114197014A (en) * | 2021-12-14 | 2022-03-18 | 合肥工业大学 | Method for realizing surface nanocrystallization of pure titanium part with complex shape |
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2014
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| CN106637350A (en) * | 2016-12-08 | 2017-05-10 | 西南交通大学 | Preparation method of molybdenum-doped titanium dioxide nano-tube array thin film |
| CN106731881A (en) * | 2016-12-20 | 2017-05-31 | 济南大学 | Based on metal, nonmetallic codope nTiO2Visible light catalytic hollow fiber ultrafiltration membrane and preparation method |
| CN108396381A (en) * | 2017-02-04 | 2018-08-14 | 中国科学院金属研究所 | A kind of optical drive shape-changing material and its preparation method and application |
| CN108396381B (en) * | 2017-02-04 | 2020-10-30 | 中国科学院金属研究所 | Light-driven deformation material and preparation method and application thereof |
| CN109482173A (en) * | 2017-09-11 | 2019-03-19 | 中国科学院金属研究所 | A kind of bulk phase-doped nano-photocatalyst material and its preparation method and application |
| CN109569574A (en) * | 2017-09-28 | 2019-04-05 | 中国科学院金属研究所 | A kind of body phase codope visible-light photocatalysis material and its preparation method and application |
| CN110653348A (en) * | 2018-06-29 | 2020-01-07 | 南京理工大学 | Titanium-based amorphous nanotube and preparation method thereof |
| CN110656257A (en) * | 2018-06-29 | 2020-01-07 | 南京理工大学 | Method for preparing nano porous gold based on titanium-based amorphous alloy |
| CN110653348B (en) * | 2018-06-29 | 2021-12-31 | 南京理工大学 | Titanium-based amorphous nanotube and preparation method thereof |
| CN110656257B (en) * | 2018-06-29 | 2022-04-08 | 南京理工大学 | Method for preparing nano porous gold based on titanium-based amorphous alloy |
| CN110129730A (en) * | 2019-06-03 | 2019-08-16 | 复旦大学 | A kind of preparation method of molybdenum doping titanium dioxide nano-pipe array thin film |
| CN114197014A (en) * | 2021-12-14 | 2022-03-18 | 合肥工业大学 | Method for realizing surface nanocrystallization of pure titanium part with complex shape |
| CN114197014B (en) * | 2021-12-14 | 2023-04-07 | 合肥工业大学 | Method for realizing surface nanocrystallization of pure titanium part with complex shape |
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