CN106732570A - A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst - Google Patents
A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst Download PDFInfo
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- CN106732570A CN106732570A CN201611201568.5A CN201611201568A CN106732570A CN 106732570 A CN106732570 A CN 106732570A CN 201611201568 A CN201611201568 A CN 201611201568A CN 106732570 A CN106732570 A CN 106732570A
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- silver
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- titanium sheet
- preparation
- silver strip
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 150000001875 compounds Chemical class 0.000 title claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052709 silver Inorganic materials 0.000 claims abstract description 44
- 239000004332 silver Substances 0.000 claims abstract description 44
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000010936 titanium Substances 0.000 claims abstract description 40
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 40
- 239000002105 nanoparticle Substances 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000608 laser ablation Methods 0.000 claims abstract description 10
- 239000013307 optical fiber Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000835 fiber Substances 0.000 claims description 9
- 238000002679 ablation Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 239000004408 titanium dioxide Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
Abstract
The invention discloses a kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst, comprise the following steps：(1) titanium sheet and silver strip are cleaned by ultrasonic；(2) titanium sheet after step (1) is cleaned is kept flat in water, with optical fiber pulse laser ablation titanium plate surface, takes out remaining titanium sheet, and titania nanoparticles solution is obtained；(3) to the silver strip kept flat in the titania nanoparticles solution obtained by step (2) after step (1) cleaning, with optical fiber pulse laser ablation silver strip surface, remaining silver strip is taken out, is obtained and is carried silver-colored titania nanoparticles solution；(4) vacuum calcining is carried out again after step (3) gained to be carried the water drying in silver-colored titania nanoparticles solution, obtains final product the silver-colored titanic oxide nano compound photocatalyst of the load.Preparation method of the invention is flexible, it is only necessary to which meeting simple operations computer and tube furnace can just control laser and calcining heat, prepares required nano composite material.
Description
Technical field
The invention belongs to photocatalyst technology field, and in particular to a kind of load silver titanic oxide nano compound photocatalyst
Preparation method.
Background technology
Titanium dioxide optical catalyst is because its catalytic efficiency is higher, stable chemical nature and it is nontoxic the features such as, as most by green grass or young crops
The photochemical catalyst looked at.But, there are two obvious defects in titanium dioxide, limit its further application.On the one hand, electronics is empty
The recombination rate in cave pair is high, causes its quantum yield low, it is difficult to purified concentrations pollutant higher；On the other hand, because its forbidden band compared with
Width, only absorbs ultraviolet light, low to solar energy utilization ratio.In titanium dioxide surface depositing noble metal silver, Xiao Te can be not only formed
The recombination rate of base potential barrier reduction electron hole pair, moreover it is possible to extend the absorption spectrum ranges of titanium dioxide, improve the profit to solar energy
With rate.At present, the method for preparing the silver-colored titanium dioxide nano material of load has photoreduction met hod, hot submersion method and chemical reduction method etc..But
Preparation process is complicated, need chemical addition agent and less stable.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided one kind carries silver-colored titanic oxide nano compound photocatalyst
Preparation method.
Technical scheme is as follows：
A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst, comprises the following steps：
(1) titanium sheet and silver strip are cleaned by ultrasonic, the purity of above-mentioned titanium sheet is more than 99.9%, and the purity of silver strip is more than
99.5%；
(2) titanium sheet after step (1) is cleaned is kept flat in water, with optical fiber pulse laser ablation titanium plate surface, takes out surplus
Remaining titanium sheet, is obtained titania nanoparticles solution, and wherein titanium sheet and the distance of liquid level is 1.5~2.5mm；
(3) to the silver strip after step (1) is cleaned is kept flat in the titania nanoparticles solution obtained by step (2), use
Fiber pulse laser ablation silver strip surface, takes out remaining silver strip, is obtained and carries silver-colored titania nanoparticles solution, wherein silver strip
It is 1.5~2.5mm with the distance of liquid level；
The fiber pulse laser of above-mentioned steps (2) and (3) is wavelength 1064nm, the ND of pulse duration 100ns：YAG
Fiber pulse laser, the focal length of ablation is 325~330mm, be radiated at the spot diameter on titanium sheet and silver strip surface for 0.04~
0.06mm, power is 2.4~2.5W, and pulse recurrence frequency is 19~21kHz, and power density is 6.1~6.2Jcm-2；
(4) vacuum calcining is carried out again after step (3) gained to be carried the water drying in silver-colored titania nanoparticles solution, i.e.,
Obtain the silver-colored titanic oxide nano compound photocatalyst of the load.
In a preferred embodiment of the invention, the step (1) is：Titanium sheet and silver strip are first placed in deionized water
25~35min of middle ultrasonic cleaning, then it is placed in 25~35min of ultrasonic cleaning in absolute ethyl alcohol.
In a preferred embodiment of the invention, in the step (2) distance of titanium sheet and liquid level for 1.8~
2.2mm。
In a preferred embodiment of the invention, in the step (3) distance of silver strip and liquid level for 1.8~
2.2mm。
In a preferred embodiment of the invention, the focal length of the fiber pulse laser of the step (2) and (3) is
329mm, it is 0.05mm to be radiated at the spot diameter on titanium sheet and silver strip surface, and power is 2.43W, and pulse recurrence frequency is 20kHz,
Power density is 6.11Jcm-2。
In a preferred embodiment of the invention, the drying temperature of the step (4) is 50~60 DEG C.
In a preferred embodiment of the invention, the vacuum calcining in the step (4) is true at 430~460 DEG C
Sky 1.8~2.2h of calcining, the heating-up time is 40~45min, and room temperature is naturally cooled to after vacuum calcining.
Beneficial effects of the present invention：
1st, preparation method of the invention is flexible, it is only necessary to which meeting simple operations computer and tube furnace can just control laser
And calcining heat, prepare required nano composite material；And the size of particle, component ratio etc. can enter by changing parameter
Row regulation.
2nd, preparation method of the invention need not add chemistry agent, and prepared product has purity very high, without it
His pollutant.
3rd, preparation method of the invention will not produce the accessory substance of adverse environment and human body own health.Prepared by the method
Load silver titanic oxide nano compound photocatalyst mainly have two advantages：1) by loading silver, can be in silver and titanium dioxide
Contact area forms Schottky barrier, prevents the compound of electron hole pair, improves light-catalysed performance.2) compared to pure dioxy
Change titanium and only absorb ultraviolet light, carrying silver-colored titanium dioxide can not only absorb ultraviolet light, moreover it is possible to absorb visible ray, greatly improve to too
The utilization rate of positive energy.
Brief description of the drawings
Fig. 1 is the EDX figures of the silver-colored titanium dioxide of load prepared by the embodiment of the present invention 1.
Fig. 2 is the TEM figures of the silver-colored titanium dioxide of load prepared by the embodiment of the present invention 1.
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure of the silver-colored titanium dioxide of load prepared by the embodiment of the present invention 1.
Specific embodiment
Technical scheme is further detailed and described below by way of specific embodiment.
Embodiment 1
A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst, comprises the following steps：
(1) titanium sheet and silver strip are first placed in 25~35min of ultrasonic cleaning in deionized water, then are placed in ultrasound in absolute ethyl alcohol
25~35min of cleaning；Above-mentioned titanium sheet purity is 99.99%, and size is 20mm × 20mm × 2mm, and above-mentioned silver strip purity is
99.8%, size is Φ 15mm × 2mm；
(2) titanium sheet after step (1) is cleaned is kept flat in the deionized water of 3.5mL, with optical fiber pulse laser ablation titanium
Piece surface, takes out remaining titanium sheet, is obtained titania nanoparticles solution, wherein the distance of titanium sheet and liquid level for 1.8~
2.2mm；
(3) to the silver strip after step (1) is cleaned is kept flat in the titania nanoparticles solution obtained by step (2), use
Fiber pulse laser ablation silver strip surface, takes out remaining silver strip, is obtained and carries silver-colored titania nanoparticles solution, wherein silver strip
It is 1.8~2.2mm with the distance of liquid level；
The fiber pulse laser of above-mentioned steps (2) and (3) is wavelength 1064nm, the ND of pulse duration 100ns：YAG
Fiber pulse laser, the focal length of ablation is 329mm, and it is 0.05mm to be radiated at the spot diameter on titanium sheet and silver strip surface, and power is
2.43W, pulse recurrence frequency is 20kHz, and power density is 6.11Jcm-2, laser scanning region is length of side 15mm × 15mm's
Square, speed is 1000mms-1, the time is 60min；
(4) carry step (3) gained after the water in silver-colored titania nanoparticles solution is dried in 50~60 DEG C is carried out again
Vacuum calcining, obtains final product the silver-colored titanic oxide nano compound photocatalyst of the load；Above-mentioned vacuum calcining is in 450 DEG C of vacuum calcinings
2h, the heating-up time is 45min, and room temperature is naturally cooled to after vacuum calcining.
Fig. 1 is the EDX figures for carrying silver-colored titanic oxide nano compound photocatalyst manufactured in the present embodiment.As can be seen from the figure
The presence of silver, titanium and oxygen element, this is consistent with the silver-colored titanic oxide nano compound photocatalyst of the load for preparing.
Fig. 2 is the TEM figures for carrying silver-colored titanic oxide nano compound photocatalyst manufactured in the present embodiment.The chart is bright many
Size only has several nanometers, and the deeper silver nano-grain of color is deposited on above titanium dioxide granule.
Fig. 3 is the UV-vis absorption spectrum for carrying silver-colored titanic oxide nano compound photocatalyst manufactured in the present embodiment
Figure.The figure clearly shows that the silver-colored titanium dioxide of load can not only absorb ultraviolet light, it is also possible to absorb the visible ray of 400nm wave bands.
Those of ordinary skill in the art understand, when technical scheme changes in following ranges, remain able to
To technique effect same as the previously described embodiments or close, protection scope of the present invention is still fallen within：
A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst, comprises the following steps：
(1) titanium sheet and silver strip are cleaned by ultrasonic, the purity of above-mentioned titanium sheet is more than 99.9%, and the purity of silver strip is more than
99.5%；
(2) titanium sheet after step (1) is cleaned is kept flat in water, with optical fiber pulse laser ablation titanium plate surface, takes out surplus
Remaining titanium sheet, is obtained titania nanoparticles solution, and wherein titanium sheet and the distance of liquid level is 1.5~2.5mm；
(3) to the silver strip after step (1) is cleaned is kept flat in the titania nanoparticles solution obtained by step (2), use
Fiber pulse laser ablation silver strip surface, takes out remaining silver strip, is obtained and carries silver-colored titania nanoparticles solution, wherein silver strip
It is 1.5~2.5mm with the distance of liquid level；
The fiber pulse laser of above-mentioned steps (2) and (3) is wavelength 1064nm, the ND of pulse duration 100ns：YAG
Fiber pulse laser, the focal length of ablation is 325~330mm, be radiated at the spot diameter on titanium sheet and silver strip surface for 0.04~
0.06mm, power is 2.4~2.5W, and pulse recurrence frequency is 19~21kHz, and power density is 6.1~6.2Jcm-2；
(4) vacuum calcining is carried out again after step (3) gained to be carried the water drying in silver-colored titania nanoparticles solution, i.e.,
Obtain the silver-colored titanic oxide nano compound photocatalyst of the load；Above-mentioned drying temperature is 50~60 DEG C, and above-mentioned vacuum calcining is 430
~460 DEG C of 1.8~2.2h of vacuum calcining, the heating-up time is 40~45min, and room temperature is naturally cooled to after vacuum calcining.
The above, only presently preferred embodiments of the present invention, therefore can not according to this limit the scope of present invention implementation, i.e.,
The equivalence changes made according to the scope of the claims of the present invention and description and modification, all should still belong in the range of the present invention covers.
Claims (7)
1. a kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst, it is characterised in that：Comprise the following steps：
(1) titanium sheet and silver strip are cleaned by ultrasonic, the purity of above-mentioned titanium sheet is more than 99.9%, and the purity of silver strip is more than
99.5%；
(2) titanium sheet after step (1) is cleaned is kept flat in water, with optical fiber pulse laser ablation titanium plate surface, is taken out remaining
Titanium sheet, is obtained titania nanoparticles solution, and wherein titanium sheet and the distance of liquid level is 1.5~2.5mm；
(3) to the silver strip after step (1) is cleaned is kept flat in the titania nanoparticles solution obtained by step (2), optical fiber is used
Pulse laser ablation silver strip surface, takes out remaining silver strip, is obtained and carries silver-colored titania nanoparticles solution, wherein silver strip and liquid
The distance in face is 1.5~2.5mm；
The fiber pulse laser of above-mentioned steps (2) and (3) is wavelength 1064nm, the ND of pulse duration 100ns：YAG optical fiber
Pulse laser, the focal length of ablation is 325~330mm, and it is 0.04~0.06mm to be radiated at the spot diameter on titanium sheet and silver strip surface,
Power is 2.4~2.5W, and pulse recurrence frequency is 19~21kHz, and power density is 6.1~6.2Jcm-2；
(4) vacuum calcining is carried out again after step (3) gained to be carried the water drying in silver-colored titania nanoparticles solution, obtains final product institute
State the silver-colored titanic oxide nano compound photocatalyst of load.
2. preparation method as claimed in claim 1, it is characterised in that：The step (1) is：Titanium sheet and silver strip are first placed in
It is cleaned by ultrasonic 25~35min in ionized water, then is placed in 25~35min of ultrasonic cleaning in absolute ethyl alcohol.
3. preparation method as claimed in claim 1, it is characterised in that：Titanium sheet and the distance of liquid level are 1.8 in the step (2)
~2.2mm.
4. preparation method as claimed in claim 1, it is characterised in that：Silver strip and the distance of liquid level are 1.8 in the step (3)
~2.2mm.
5. preparation method as claimed in claim 1, it is characterised in that：Jiao of the fiber pulse laser of the step (2) and (3)
Away from being 329mm, it is 0.05mm to be radiated at the spot diameter on titanium sheet and silver strip surface, and power is 2.43W, and pulse recurrence frequency is
20kHz, power density is 6.11Jcm-2。
6. preparation method as claimed in claim 1, it is characterised in that：The drying temperature of the step (4) is 50~60 DEG C.
7. preparation method as claimed in claim 1, it is characterised in that：Vacuum calcining in the step (4) be 430~
460 DEG C of 1.8~2.2h of vacuum calcining, the heating-up time is 40~45min, and room temperature is naturally cooled to after vacuum calcining.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611201568.5A CN106732570A (en) | 2016-12-22 | 2016-12-22 | A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611201568.5A CN106732570A (en) | 2016-12-22 | 2016-12-22 | A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst |
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|---|---|
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Family
ID=58897427
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| CN201611201568.5A Pending CN106732570A (en) | 2016-12-22 | 2016-12-22 | A kind of preparation method for carrying silver-colored titanic oxide nano compound photocatalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110093617A (en) * | 2019-05-24 | 2019-08-06 | 山东省科学院激光研究所 | A kind of titanium silk cleaning method and the titanium silk cleaned using this method |
| CN114538506A (en) * | 2022-03-07 | 2022-05-27 | 四川大学 | Preparation of high catalytic performance nano TiO by liquid phase pulse laser ablation2Method for producing granules |
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| CN103272592A (en) * | 2013-05-08 | 2013-09-04 | 陕西科技大学 | Preparation method of one-dimensional silver-loaded titanium dioxide nanorod photocatalyst |
| CN105603492A (en) * | 2016-01-29 | 2016-05-25 | 武汉理工大学 | Method for electrochemically depositing silver nanoparticles in titanium dioxide nanotube array |
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2016
- 2016-12-22 CN CN201611201568.5A patent/CN106732570A/en active Pending
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| CN103272592A (en) * | 2013-05-08 | 2013-09-04 | 陕西科技大学 | Preparation method of one-dimensional silver-loaded titanium dioxide nanorod photocatalyst |
| CN103272592B (en) * | 2013-05-08 | 2015-09-02 | 陕西科技大学 | One dimension carries the preparation method of silver-colored titanium dioxide nano-rod photo-catalyst |
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Non-Patent Citations (3)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093617A (en) * | 2019-05-24 | 2019-08-06 | 山东省科学院激光研究所 | A kind of titanium silk cleaning method and the titanium silk cleaned using this method |
| CN114538506A (en) * | 2022-03-07 | 2022-05-27 | 四川大学 | Preparation of high catalytic performance nano TiO by liquid phase pulse laser ablation2Method for producing granules |
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Application publication date: 20170531 |