CN106148902A - A kind of femtosecond laser preparation method of uniformly thicker meso-porous titanium oxide nanometer particle film - Google Patents
A kind of femtosecond laser preparation method of uniformly thicker meso-porous titanium oxide nanometer particle film Download PDFInfo
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Abstract
The invention discloses a kind of mesoporous nano-grain method for manufacturing thin film, belong to femtosecond laser deposition and prepare the technology of specific properties thin film.The method, with high-purity mangesium oxide titanium as target, uses pulsewidth 300 femtosecond, centre wavelength 537 nanometer, frequency 33 hertz, and maximum single pulse energy is the vacuum laser precipitation equipment of 0.9 MJ, it is achieved uniformly prepared by thicker meso-porous titanium oxide nanometer particle film.It is characterized in that: when sedimentation time is shorter, nano-particle yardstick is averagely at 20 ran.After long period deposition, there is Cluster Phenomenon in granule, and thin film is thicker and mesoporous gap is obvious.Advantages of the present invention: control pulse energy, sedimentation time can change thin film parameter；Control target chamber air pressure and inflation type can realize the difference of thin film crystallization form and change；Doping or compound other materials are convenient；There is higher solar conversion efficiency in unit thickness；It is easy to study different types of femtosecond laser deposition and prepares the application in terms of hydrogen manufacturing of the thin film of specific properties.
Description
Technical field
The present invention relates to a kind of semiconductor film membrane preparation method, a kind of femtosecond laser deposition prepares the method for mesoporous nano-grain thin film.
Background technology
Titanium oxide (TiO2) nano material shows the highest catalytic reaction ability and chemical stability at hydrogen production by water decomposition (Water Splitting) aspect.Use TiO2Nano-particular film, can realize photochemical breakdown water hydrogen under solar irradiation.At TiO2In nanometer particle film, gold doping (Au), cadmium sulfide (CdS), nitrogen (N) and rubidium (Nd) are co-doped with, and cadmium sulfide (CdS) base mixes platinum (Pt) and tungsten carbide (WC) etc. and can fully absorb solar irradiation energy further, it is achieved illumination utilization rate and the raising of hydrogen production efficiency.The TiO of tradition application photochemical breakdown water hydrogen manufacturing2Nano-particular film generally uses the chemical methodes such as collosol and gel to prepare, and nano particle diameter size, granule interval and composite type are relatively big on experimental result impact, there is adhesive force the highest, the deficiency that operation is complicated.
TiO2Nanometer particle film application prospect in terms of the preparation research of clean energy resource hydrogen is extensive.Document and report about relating to the technology of the present invention are as follows:
[1]、Huihu Wang, Joaquim Luís Faria, Shijie Dong, Ying
Chang, Mesoporous Au/TiO2 composites preparation, characterization, and
Photocatalytic properties, Materials Science and Engineering B, 2012,177:913～919
[2]、W. H. Leng, Piers R. F. Barnes,
Mindaugas Juozapavicius, Brian C. O'Regan, and James R. Durrant, Electron
Diffusion Length in Mesoporous Nanocrystalline TiO2 Photoelectrodes during
Water Oxidation, J. Phys. Chem. Lett. 2010,1,967～972
[3]、Rony S. Khnayzer, Lucas B. Thompson,
Mikhail Zamkov, Shane Ardo, Gerald J. Meyer, Catherine J. Murphy, and
Felix N. Castellano, Photocatalytic Hydrogen Production at Titania-Supported Pt
Nanoclusters That Are Derived from Surface-Anchored Molecular Precursors, J.
Phys. Chem. C 2012,116,1429～1438
[4]、Jonghun Lim, Palanichamy Murugan,
Narayanan Lakshminarasimhan, Jae Young Kim, Jae Sung Lee, Sang-Hyup Lee,
Wonyong Choi, Synergic photocatalytic effects of nitrogen and niobium co-doping
in TiO2 for the redox conversion of aquatic pollutants under visible light,
Journal of Catalysis, 2014,310:91～99
[5]、Narayanan Lakshminarasimhan, Eunyoung
Bae, and Wonyong Choi, Enhanced Photocatalytic Production of H2 on Mesoporous
TiO2 Prepared by Template-Free Method: Role of Interparticle Charge Transfer,
J. Phys. Chem. C 2007,111,15244～15250
[6]、N. Lakshminarasimhan, AD Bokare and
W. Choi, Effect of agglomerated state in mesoporous TiO2 on the morphology of
photodeposited Pt and photocatalytic activity, J. Phys. Chem. C, 2012, 116,
17531～17539
[7]、Mohammad Mansoob Khan, Sajid A.
Ansari, D. Pradhan, M. Omaish Ansari, Do Hung Han, Jintae Lee and Moo Hwan Cho,
Band gap engineered TiO2 nanoparticles for visible light induced
photoelectrochemical and photocatalytic studies, J. Mater. Chem. A, 2014, 2,
637～644
Summary of the invention
It is an object of the invention to provide the femtosecond laser preparation method of a kind of uniformly thicker meso-porous titanium oxide nanometer particle film.The method is applicable to different base, prepare mesoporous substantially, uniformly and thicker, degree of crystallinity preferably, adhesive force Titanium dioxide nanoparticle thin film stronger, simple to operate.
For achieving the above object, the present invention is realized by the following technical scheme: use femtosecond pulse technology sputtering sedimentation preparation uniformly thicker meso-porous titanium oxide nanometer particle film in vacuum target chamber.Using pulsewidth is 300 femtoseconds (fs), centre wavelength 537 nanometer (nm), repetition rate is 33 hertz (Hz), maximum single pulse energy is the femtosecond pulse precipitation equipment of 0.9 MJ (mJ), from laser instrument laser out by electric-controlled switch (shutter), energy attenuator, metal mirrors, long focusing planoconvex lens and vacuum target chamber window, final with 45 degree of target material surfaces being introduced in vacuum target chamber of vertical target surface, air pressure 10-1-10- 7Millibar (mbar), laser beam can control focusing concave mirror by computer and sweep away in the little scope of target material surface, using rutile or anatase titanium oxide crystal as target, using the titanium foil after surface finish as substrate, substrate and target distance 25 to 35 centimetres (cm), with energy-flux density 0.13-1.4 joules per cm (J/cm2) laser beam irradiation target material surface be initially formed plasma, nano-particle target as sputter deposits to substrate surface and is epitaxially-formed meso-porous titanium oxide nanometer particle film afterwards.It is characterized in that: when sedimentation time is shorter, nano-particle yardstick is averagely at about 20nm.After long period deposition, there is Cluster Phenomenon in nano-particle, and thin film is thicker, and granule or the mesoporous gap of cluster are obvious.Thin film crystalline phase after annealing is obviously improved.
In technique scheme, when using other pulsewidth femtosecond laser sources, suitably fine setting target source and substrate distance, it is ensured that laser energy-flux density is higher than target ablation threshold, reduces repetition rate to 33Hz so that electric-controlled switch drives.
By preventing the fixing plasma a little brought of laser beam ablation target material surface from changing, improve target utilization, focusing concave mirror level is slightly driven to realize focal spot to adjustment frame regulation button by motor and sweeps away in the little scope in target material surface off-center region, and target does constant amplitude stepping circular motion with center for round dot simultaneously.
Described substrate is titanium (Ti) paper tinsel or other hydrogen manufacturing backing materials.
Described fine setting target source and substrate distance are not affect laser splash and the higher distance range of deposition efficiency.
Described energy-flux density is the area ratio that average single-pulse laser energy and light beam focus on target material surface.
Described deposition energy-flux density is the femto-second laser used energy-flux density scope higher than target ablation threshold.
Described vacuum target chamber air pressure be fine vacuum and fill oxygen, coarse vacuum scope after nitrogen.
Described thin film is thicker refers to that film thickness is more than 100nm, reaches the electricity conversion requirement in water decomposition hydrogen manufacturing experiment.
Deposition of described long period refers to reach the sedimentation time that above-mentioned relatively thick film needs.
Described granule or the mesoporous gap of cluster substantially refer to granule or cluster is mesoporous substantially refers to that thin film is apparent and manifest with granule and cluster form, and gap dimension is the most mesoporous about granule and cluster range scale, the most photoelectric generation.
Can be after thin film be formed, by film sample anneal (annealing) to eliminate part stress, to improve thin film crystallization state.Annealing temperature is optimum results, and temperature is heated to 500 to 700 degree, within the most every 20 minutes, moves back temperature and once realized.
It is an advantage of the current invention that:
(1) take full advantage of the high of pulsed laser deposition and protect component characteristic, utilize again femtosecond laser process technology, improve single pulse energy and pulse width easily, improve the mean power (energy-flux density is divided by pulse width) of pulse output to realize the spatter film forming of any target, regulation nanoparticle aggregate state, grows heterogeneous Titanium dioxide nanoparticle thin film on different substrates；
(2) laser energy-flux density is when target Near Threshold, Titanium dioxide nanoparticle effective average diameter yardstick about 25nm, when improving laser energy density, particle deposition efficiency improves, particle clusters building-up effect becomes apparent (nanoparticle aggregate forms larger particles together), and mesoporous effect is notable；
(3) vacuum target chamber air pressure environment is bigger on the impact of nanometer particle film sedimentation rate, during condition of high vacuum degree, the sedimentation rate of particle film strengthens, 4 square centimeters of substrates can be distributed less than 25nm and relatively decentralized nano-particle by deposit thickness upper 20 second, the thin film crystalline phase prepared during rough vacuum is preferable, vacuum environment is conveniently adjusted by target chamber valve, thin film aggregate performance is rutile and anatase mixed phase, but Rutile Type is dominant；
(4) adulterating or be combined other materials conveniently, the other materials that only need to adhere to certain area ratio on target in light beam sweep limits can realize；
(5) powder-type target is compound or during doping other materials, doping ratio the most uniformly mixing after re-compacted one-tenth target body can be conveniently determined in advance, then utilizes this method to carry out nanometer particle film and prepare；
(6) in solar energy water decomposition experiment, comparing by flat thin film thickness electricity conversion, under same illumination condition, (about 160nm, electric current density is up to 0.2 milliampere of every square centimeter of (mA/cm for medium pore of titania nanometer particle film prepared by this method2) (about 600nm, electric current density is 0.3mA/cm to photoelectric conversion effect relatively titanium oxide nanotubes thin film2) high；
(7) can be combined easily or the different materials that adulterates carries out nanometer particle film and prepares, the solar energy utilization ratio of the different nanometer particle film of research, to improve water decomposition hydrogen manufacturing effect.
Accompanying drawing explanation
Femtosecond laser sputter deposition apparatus schematic diagram in Fig. 1 present invention.
Spatter film forming schematic diagram in vacuum target chamber in Fig. 2 present invention.
Water decomposition hydrogen manufacturing experimental provision schematic diagram in Fig. 3 present invention, whereinFor electric charge, H+For hydrion, V: sense voltage table, R: resistance.
Using pulsewidth in Fig. 4 present invention is 300fs, centre wavelength 537nm, energy-flux density 0.3mJ/cm2Femtosecond laser sputtering sedimentation 20 seconds time 4 square microns in the range of Titanium dioxide nanoparticle particle diameter distribution histogram, dependency therein finds that the granule number that effective grain size is identical accounts for the percentage ratio of total particle number in referring to field range, and effective grain size refers to that granule actual measurement volume (irregularly) using granularmetric analysis software (SPIP software) to analyze atomic force microscopy (AFM) figure calculates the equivalent diameter of the spherical granules being converted to have same volume.
Using femtosecond laser pulsewidth in Fig. 5 present invention is 300fs, centre wavelength 537nm, air pressure 10- 7Mbar, energy-flux density 1.4J/cm2Time, the sputtering sedimentation sample of 1.5 hours 1 relatively thin Titanium dioxide nanoparticle particle diameter scanning electron microscope (SEM) phenogram.
Using femtosecond laser pulsewidth in Fig. 6 present invention is 300fs, centre wavelength 537nm, air pressure 10- 7Mbar, the sputtering sedimentation sample of 3 hours 2 thicker Titanium dioxide nanoparticle particle diameter scanning electron microscope (SEM) phenogram.
Fig. 7 utilizes sample 1(Fig. 5) and sample 2(Fig. 6) the density of photocurrent result figure that obtains of the water decomposition hydrogen experiment that carries out according to Fig. 3 indication device of medium pore of titania nanometer particle film.
Detailed description of the invention
Embodiment 1:
Utilize femtosecond laser sputter deposition apparatus (Fig. 1), employing pulsewidth is 300fs, centre wavelength 537nm, repetition rate is 33Hz, single pulse energy is the Nd:Glass femtosecond double frequency pulse laser of 0.8mJ, pass sequentially through energy attenuator, gilding mirror, plano-convex focusing objective len and vacuum target chamber silicon oxide transmission window that pulse-triggered electric-controlled switch, half-wave plate and polarizing crystals are constituted, finally with the 45 degree of angular focusing of vertical target surface to target material surface, air pressure 10- 7Mbar, laser beam controls gilding by computer software and sweeps away in the outer 1cm scope of Rutile Type titanium oxide (99.99%) target material surface central point, using the marble substrate of a diameter of 1cm as substrate, substrate and target distance 35cm, with energy-flux density about 0.36J/cm2Laser beam irradiation target, sedimentation time is 10 seconds, is epitaxially-formed Titanium dioxide nanoparticle at substrate surface, grain diameter size through atomic force microscope characterize and software statistics after distribution histogram such as Fig. 4.
Embodiment 2:
Utilize femtosecond laser sputter deposition apparatus (Fig. 1), employing pulsewidth is 300fs, centre wavelength 537nm, repetition rate is 33Hz, single pulse energy is the Nd:Glass femtosecond double frequency pulse laser of 0.8mJ, pass sequentially through energy attenuator, gilding mirror, plano-convex focusing objective len and vacuum target chamber silicon oxide transmission window that pulse-triggered electric-controlled switch, half-wave plate and polarizing crystals are constituted, finally with the 45 degree of angular focusing of vertical target surface to target material surface, air pressure 10- 7Mbar, laser beam controls gilding by computer software and sweeps away in the outer 1cm scope of Rutile Type titanium oxide (99.99%) target material surface central point, using the 0.5 × 1cm titanium foil after surface physics grinding and polishing as substrate, substrate and target distance 35cm, with energy-flux density 1.4J/cm2Laser beam irradiation target, nano-particle sputtering sedimentation 1.5 hours, be epitaxially-formed meso-porous titanium oxide nanometer particle film Fig. 5 at substrate surface.
Embodiment 3:
Utilize femtosecond laser sputter deposition apparatus (Fig. 1), employing pulsewidth is 300fs, centre wavelength 537nm, repetition rate is 33Hz, single pulse energy is the Nd:Glass femtosecond double frequency pulse laser of 0.8mJ, pass sequentially through energy attenuator, gilding mirror, plano-convex focusing objective len and vacuum target chamber silicon oxide transmission window that pulse-triggered electric-controlled switch, half-wave plate and polarizing crystals are constituted, finally with the 45 degree of angular focusing of vertical target surface to target material surface, air pressure 10- 7Mbar, laser beam controls gilding by computer software and sweeps away in the outer 1cm scope of Rutile Type titanium oxide (99.99%) target material surface central point, using the 0.5 × 1cm titanium foil after surface physics grinding and polishing as substrate, substrate and target distance 35cm, with energy-flux density 1.4J/cm2Laser beam irradiation target, nano-particle sputtering sedimentation 3 hours, be epitaxially-formed meso-porous titanium oxide nanometer particle film Fig. 6 at substrate surface.
Claims (6)
1. a mesoporous nano-grain semiconductor film membrane preparation method: the method is using the titanium oxide of high-purity (99.99%) Rutile Type as target, using pulsewidth is 300 femtoseconds, centre wavelength 537 nanometer, repetition rate is 33 hertz, maximum single pulse energy is the femtosecond pulse vacuum deposition apparatus of 0.9 MJ, realize uniformly thicker meso-porous titanium oxide nanometer particle film to prepare, it is characterized in that: when sedimentation time is shorter, nano-particle yardstick is averagely at about 20nm, after long period deposition, there is Cluster Phenomenon in nano-particle, thin film is thicker, granule or the mesoporous gap of cluster are obvious, thin film crystalline phase after annealing is obviously improved.
2. the mesoporous nano-grain semiconductor film membrane preparation method as described in claim 1, it is characterised in that: when using other pulsewidth femtosecond laser sources, suitable vacuum target chamber is finely tuned target source and substrate distance, it is ensured that laser energy-flux density is higher than target ablation threshold.
3. the mesoporous nano-grain semiconductor film membrane preparation method as described in claim 1, it is characterised in that: vacuum target chamber air pressure can be fine vacuum and fill oxygen, rough vacuum after nitrogen.
4. the mesoporous nano-grain semiconductor film membrane preparation method as described in claim 1, it is characterized in that: by preventing the fixing plasma a little brought of laser beam ablation target material surface from changing, improve target utilization, focusing concave mirror level is slightly driven to realize focal spot to adjustment frame regulation button by motor and sweeps away in the little scope in target material surface off-center region, and target does constant amplitude stepping circular motion with center for round dot simultaneously.
5. the mesoporous nano-grain semiconductor film membrane preparation method as described in claim 1; it is characterized in that: thin film is thicker; granule or the mesoporous gap of cluster substantially refer to that film thickness is more than 100nm; reach the electricity conversion requirement in water decomposition hydrogen manufacturing experiment; long period deposition refers to reach the sedimentation time that above-mentioned relatively thick film needs; granule or cluster is mesoporous substantially refers to that thin film is apparent and manifest with granule and cluster form, gap dimension is referred to as mesoporous about granule and cluster range scale.
6. the mesoporous nano-grain semiconductor film membrane preparation method as described in claim 1, it is characterized in that: the thin film crystalline phase after annealing is obviously improved and refers to after thin film is formed, by film sample anneal to eliminate part stress, to improve thin film crystallization state, annealing temperature be optimum results be film temperature be heated to 500 to 700 degree, within the most every 20 minutes, move back temperature and once realized.
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Cited By (8)
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|---|---|---|---|---|
| CN108091765A (en) * | 2017-12-26 | 2018-05-29 | 福建江夏学院 | A kind of method that perovskite solar cell electron transfer layer is prepared using laser irradiation |
| CN109609915A (en) * | 2019-01-09 | 2019-04-12 | 张晓军 | Without process engineering semiconductor nano material preparation system |
| CN111057999A (en) * | 2019-12-18 | 2020-04-24 | 上海米蜂激光科技有限公司 | Method and equipment for preparing nano porous silicon dioxide film by continuous wave laser irradiation |
| CN111360146A (en) * | 2020-03-23 | 2020-07-03 | 沈阳航空航天大学 | Device and method for preparing metal film by area expansion under vacuum environment |
| CN112663333A (en) * | 2020-11-22 | 2021-04-16 | 南京理工大学 | Method for depositing superfine nano metal powder on surface of fabric |
| CN112853278A (en) * | 2019-11-12 | 2021-05-28 | 中国科学院微电子研究所 | Preparation method of short-pulse laser deposition film |
| CN113922193A (en) * | 2021-10-08 | 2022-01-11 | 山西大学 | Device and method for improving vacuum degree of vacuum system through laser local heating |
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| CN109609915A (en) * | 2019-01-09 | 2019-04-12 | 张晓军 | Without process engineering semiconductor nano material preparation system |
| CN109609915B (en) * | 2019-01-09 | 2020-12-01 | 张晓军 | Disordered engineering semiconductor nano material preparation system |
| CN112853278B (en) * | 2019-11-12 | 2023-01-17 | 中国科学院微电子研究所 | Preparation method of short-pulse laser deposition film |
| CN112853278A (en) * | 2019-11-12 | 2021-05-28 | 中国科学院微电子研究所 | Preparation method of short-pulse laser deposition film |
| CN111057999B (en) * | 2019-12-18 | 2021-12-10 | 上海米蜂激光科技有限公司 | Method and equipment for preparing nano porous silicon dioxide film by continuous wave laser irradiation |
| CN111057999A (en) * | 2019-12-18 | 2020-04-24 | 上海米蜂激光科技有限公司 | Method and equipment for preparing nano porous silicon dioxide film by continuous wave laser irradiation |
| CN111360146A (en) * | 2020-03-23 | 2020-07-03 | 沈阳航空航天大学 | Device and method for preparing metal film by area expansion under vacuum environment |
| CN111360146B (en) * | 2020-03-23 | 2021-06-15 | 沈阳航空航天大学 | Device and method for preparing metal film by area expansion under vacuum environment |
| CN112663333B (en) * | 2020-11-22 | 2022-03-15 | 南京理工大学 | Method for depositing superfine nano metal powder on surface of fabric |
| CN112663333A (en) * | 2020-11-22 | 2021-04-16 | 南京理工大学 | Method for depositing superfine nano metal powder on surface of fabric |
| CN113922193A (en) * | 2021-10-08 | 2022-01-11 | 山西大学 | Device and method for improving vacuum degree of vacuum system through laser local heating |
| CN113922193B (en) * | 2021-10-08 | 2023-09-22 | 山西大学 | Device and method for improving vacuum degree of vacuum system through laser local heating |
| CN114378054A (en) * | 2021-12-31 | 2022-04-22 | 复旦大学 | Vacuum type three-dimensional scanning laser surface cleaning and collecting device |
| CN114378054B (en) * | 2021-12-31 | 2024-01-23 | 复旦大学 | Vacuum type three-dimensional scanning laser surface cleaning and collecting device |
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Application publication date: 20161123 |