CN105372223A - Ag/TiO2 flexible SERS substrate capable of being repeatedly utilized and preparation method thereof - Google Patents
Ag/TiO2 flexible SERS substrate capable of being repeatedly utilized and preparation method thereof Download PDFInfo
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- CN105372223A CN105372223A CN201510693040.3A CN201510693040A CN105372223A CN 105372223 A CN105372223 A CN 105372223A CN 201510693040 A CN201510693040 A CN 201510693040A CN 105372223 A CN105372223 A CN 105372223A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/64—Treatment of refractory metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
Abstract
The invention discloses a preparation method of an Ag/TiO2 flexible SERS substrate capable of being repeatedly utilized. A thin Ti sheet is adopted as a Ti source, a TiO2 nanobelt array with Ti as a substrate is prepared through a hydro-thermal synthesis method, an SERS substrate material of Ag/TiO2 is prepared through a continuous ion deposition method, the Ti sheet can be cut to be of any shape and size according to test requirements, the large-area SERS substrate material can be prepared according to the size of the Ti sheet, and potential industrial production prospects are achieved. In addition, the number of silver nanoparticles on the surface of an Ag/TiO2 film is controllable, the silver nanoparticles are firm and not likely to fall off, an organic tested objected adsorbed on the surface of the material can be degraded and decomposed under the irradiation of a xenon lamp light source, the function of detoxicating the SERS material is achieved, and therefore a sample can be used repeatedly and cyclically.
Description
Technical field
The invention belongs to field of nanometer technology, be specifically related to a kind of Ag/TiO
2flexible, the SERS substrate that can reuse and preparation method thereof.
Background technology
Surface enhanced raman spectroscopy (Surface-enhancedRamanscattering, SERS) be a kind of novel, fast, highly sensitive detection method.Because it can realizing ultralow detection limit, can providing the finger print information of material and not destroying sample when detecting, can reach the advantages such as detection fast and be widely used in Molecular Detection field, therefore develop effective SERS marker material particularly important.Efficient SERS marker material not only will have stronger enhancer, also will have good stability and reappearance simultaneously.People study discovery, and noble-metal-supported semiconductor material, due to the synergy between noble metal and semiconductor, makes material have stronger SERS enhancement effect, therefore can be used as one of optimal selection of SERS marker material.Because titania itself is a kind of important wide band gap semiconducter, there is good optical property and stability, and nontoxic, cheap.Ag modifies TiO
2in compound substance, titania and silver surface are conducive to Charger transfer, thus improve SERS signal, and in addition, Ag modifies TiO
2compound substance is also a kind of common catalysis material.At present, the people multiple Ag/TiO that utilized multiple method or technology to prepare
2, but there is complicated process of preparation in these methods, operating process is restive, or the Nano silver grain of film surface deposition insecure, easily washed out by water or ethanol etc., have a strong impact on subsequent applications, or film is frangible, can the defect of reusing difference.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Ag/TiO
2flexible, the SERS substrate that can reuse and preparation method thereof, to overcome preparation Ag/TiO
2sERS baseplate material SERS substrate process complexity, the difficult control of process, film surface Nano silver grain is insecure, reusing is poor defect.
For realizing above-mentioned technical matters, the invention provides a kind of Ag/TiO
2flexible, can the to reuse preparation method of SERS substrate, comprises the following steps:
(1) by titanium sheet successively with after acetone, EtOH Sonicate cleaning 20 ~ 40min, adopt chemical polishing process, then after repeatedly rinsing with distilled water under nitrogen protection cold wind dry up for subsequent use;
(2) by polished titanium sheet while lean against in autoclave, slowly add concentration be 3.5 ~ 4.5mol/LNaOH aqueous solution to titanium sheet is flooded completely, build autoclave and be placed in air dry oven isothermal reaction 36 ~ 72h at 180 ~ 220 DEG C;
(3) titanium sheet is taken out, after repeatedly rinsing with deionized water, be immersed in the HCl solution 10 ~ 14h of 0.08 ~ 0.12mol/L, again titanium sheet is taken out, repeatedly rinse with deionized water, cold wind dries up, and then in muffle furnace, 380 ~ 420 DEG C of annealing naturally cooled to room temperature after 2.5 ~ 3.5 hours, obtained the TiO of Anatase
2nanobelt;
(4) by TiO
2nanobelt is first immersed in the AgNO that 50mL concentration is 3 ~ 5mmol/L
34 ~ 8min in solution, after taking out, level is dried, then is immersed in the NaBH that 50mL concentration is 1.8 ~ 2.2mmol/L
44 ~ 6min in solution, takes out sample, after clean with deionized water rinsing, naturally dries, obtained Ag/TiO
2nanometer sheet, the charge capacity of Ag controls by soaking number of times.
Preferably, described titanium sheet is smooth, and thickness is 0.5mm, and size is 30mm × 10mm.
Preferably, described chemical polishing is HF:HNO in volume ratio
3: H
2carry out in the mixed liquor of O=1:1:4, be polished to till titanium plate surface is bright silver
Preferably, described immersion number of times is 1 ~ 5 time.
Preferably, described annealing heating rate is 3 DEG C/min.
The present invention also provides a kind of Ag/TiO prepared according to said method
2flexible, can to reuse SERS substrate, is prepared from by following steps:
(1) after titanium sheet being used successively acetone, ethanol ultrasonic cleaning 20 ~ 40min, adopt chemical polishing carry out polishing, then after repeatedly rinsing with distilled water under nitrogen protection cold wind dry up for subsequent use;
(2) by polished titanium sheet while lean against in autoclave, slowly add concentration be 3.5 ~ 4.5mol/LNaOH aqueous solution to titanium sheet is flooded completely, build autoclave and be placed in air dry oven isothermal reaction 36 ~ 72h at 180 ~ 220 DEG C;
(3) titanium sheet is taken out, after repeatedly rinsing with deionized water, be immersed in the HCl solution 10 ~ 14h of 0.08 ~ 0.12mol/L, again titanium sheet is taken out, repeatedly rinse with deionized water, cold wind dries up, and then in muffle furnace, 380 ~ 420 DEG C of annealing naturally cooled to room temperature after 2.5 ~ 3.5 hours, obtained the TiO of Anatase
2nanobelt;
(4) by TiO
2nanobelt is first immersed in the AgNO that 50mL concentration is 3 ~ 5mmol/L
34 ~ 8min in solution, after taking out, level is dried, then is immersed in the NaBH that 50mL concentration is 1.5 ~ 2.5mmol/L
44 ~ 6min in solution, takes out sample, after clean with deionized water rinsing, naturally dries, obtained Ag/TiO
2nanometer sheet, the charge capacity of Ag controls by soaking number of times.
Compared with prior art, the beneficial effect acquired by the present invention is: the present invention is that being prepared by the method for Hydrothermal Synthesis with Ti is the TiO of substrate with thin Ti sheet (thickness is for 0.2mm) for Ti source
2nano-band array, prepares Ag/TiO through continuous ionic sedimentation
2sERS backing material, the method preparation technology is simple, and course of reaction easily controls.Meanwhile, according to testing requirement, titanium sheet can be cut into arbitrary shape and size, and large-area SERS backing material can be prepared according to Ti sheet size, have potential industrial production prospect.In addition, Ag/TiO
2the Nano silver grain amount of film surface is controlled, and firmly, difficult drop-off, under the irradiation of xenon source, degradable decomposes and is adsorbed on organic measured object of material surface, SERS material is reached to the function of " removing toxic substances ", thus makes sample can iterative cycles use.
Accompanying drawing explanation
Fig. 1 is TiO prepared by embodiment 1
2nanobelt and Ag/TiO
2nanobelt SEM and TEM schemes.
Fig. 2 is TiO prepared by embodiment 1
2nanobelt and Ag/TiO
2the XRD figure of nanobelt.
Fig. 3 is the Ag/TiO being adsorbed with variable concentrations rhodamine 6G
2nanobelt (S
3) SERS spectrum, the concentration of (a ~ d) rhodamine 6G respectively 10
-5mol/L, 10
-6mol/L, 10
-7mol/L and 10
-8mol/L.
Fig. 4 sample S
3as the circulation degradation results of SERS substrate.
Embodiment
Below in conjunction with specific embodiment, the technical solution of the present invention is further explained illustrates, but is not limited to following examples.
Embodiment 1
(1) be 0.2mm by thickness, area is that the titanium sheet of 30mm × 10mm flattens; to use in acetone, ethanol after ultrasonic cleaning 30min successively; adopt chemical polishing to carry out polishing, after the Ti sheet distilled water after polishing rinses repeatedly, cold wind dries up for subsequent use under nitrogen protection.Chemical polishing adopts infusion process, is HF:HNO in volume ratio
3: H
2carry out in the mixed liquor of O=1:1:4, be polished to titanium plate surface oxide layer and all dissolve, till bright silver; (2) by polished titanium sheet while leaning against volume is in the teflon-lined autoclave of 100ml, the NaOH aqueous solution slowly adding the 4mol/L prepared, to titanium sheet being flooded completely, is built and to be placed in air dry oven isothermal reaction 48h at 200 DEG C; (3) with tweezers, sample is carefully taken out, after repeatedly rinsing with deionized water, be immersed in the HCl solution 12h of 0.1mol/L, to remove impurity and the Na ion of sample surfaces, then sample tweezers are taken out, repeatedly rinse well with deionized water, cold wind dries up, then be placed in 400 DEG C of annealing in muffle furnace and, after 3 hours, naturally cool to room temperature, obtain the TiO of Anatase
2nanobelt (TiO
2nBs) sample, is labeled as S
0; (4) continuous ionic layer adsorption reaction method (SILAR) is adopted to prepare the Ag/TiO of Ag charge capacity
2nBs.By the TiO prepared
2nBs sample is first immersed in the AgNO that 50mL concentration is 4mmol/L
36min in solution, after taking out, level is dried, then to be immersed in 50mL concentration be 5min in the NaBH4 solution of 2mmol/L.Due to NaBH
4there is stronger reductibility, will the Ag on TiO2NBs surface be adsorbed on rapidly
+be reduced into simple substance Ag.Take out sample, after clean with deionized water rinsing, naturally dry, then repeat immersion process twice, the Ag/TiO of acquisition
2nBs identified as samples is designated as S
3, namely soak the sample of 3 times.
In order to inquire into the pattern of synthesized product, to obtained TiO
2nanobelt and Ag/TiO
2nanobelt (S
3) do scanning electron microscope and transmission electron microscope test, result is as shown in Figure 1.Fig. 1 a is the TiO etched in the substrate of Ti sheet
2the SEM figure of nano-band array, as can be seen from Fig., the roomy of nanobelt is about 400nm, and length is approximately 5 μm; Fig. 1 b figure is Ag/TiO
2by figure, the SEM figure of nanobelt, finds out that Ag nano particle uniform deposition is on nanobelt surface, and TiO
2the pattern of nanobelt remains intact; Fig. 1 c is Ag/TiO
2the TEM photo of nanobelt, its pattern and Fig. 1 b very identical, the domain size distribution of Ag nano particle is between 10 ~ 30nm.
X-ray diffraction (XRD) is one of characterization method that crystalline material is conventional, is commonly used to crystalline form and the crystallization degree of exosyndrome material.Fig. 2 is obtained TiO
2nanobelt and Ag/TiO
2nanobelt (S
3) XRD figure, TiO as can be seen from Fig.
2nanobelt and Ag/TiO
2the TiO of nanobelt
2be Anatase.
By the Ag/TiO of preparation
2nanobelt (S
3) as SERS substrate, detectability test is carried out to rhodamine 6G probe molecule.Concentration is respectively 10 with deionized water accurate formulation
-5, 10
-6, 10
-7with 10
-8the solution of mol/L, by sample S
3be cut into the fritter that several sizes are identical, being immersed in 3h in the rhodamine 6G solution of above-mentioned variable concentrations respectively makes probe molecule and Nano silver grain have good absorption, then take out, dry, use the SERS performance of micro laser Raman spectroscopy tester to sample to test.Raman test condition is: optical maser wavelength is 532nm, and laser power is 1.5mW, and micro-multiplying power is 20 times, and spectral resolution is 2cm
-1, integral time is 10s, sweep limit 150 ~ 1800cm
-1.Fig. 3 is the Ag/TiO being adsorbed with variable concentrations rhodamine 6G
2the SERS spectrum of nanobelt, as can be seen from the figure, along with rhodamine 6G concentration reduces gradually, measured Raman signal is more and more weak, when the concentration of rhodamine 6G is 10
-8during mol/L, the Raman peaks of probe molecule rhodamine 6G can also be detected, the Ag/TiO synthesized by explanation
2nanobelt has lower detectability in rhodamine 6G detects, and has fabulous SERS active.
By the used sample S of above-mentioned test SERS detectability
3put into surface plate, drip a small amount of deionized water, xenon lamp surveys its Raman data after irradiating 1h, and (identified as samples is designated as S
3-1), result as shown in Figure 4.As can be seen from the figure, 1649cm is only had
-1there is faint signal in position, shows that the rhodamine 6G dye molecule of sample is almost complete by photocatalytic degradation.Sample is taken out after drying and instill 10 again
-6the rhodamine 6G of mol/L repeats above-mentioned SERS and tests, and after 10 cyclic processes, finds that its Raman strengthens ability and significantly do not weaken that (identified as samples is designated as S
3-2) high stability of this system as SERS substrate, is described.Therefore, Ag/TiO
2nanobelt has good photocatalytic activity and can reusing, is also a kind of well marker material simultaneously.
Embodiment 2
(1) by titanium sheet successively with after acetone, EtOH Sonicate cleaning 40min, adopt chemical polishing process, then after repeatedly rinsing with distilled water under nitrogen protection cold wind dry up for subsequent use; (2) by polished titanium sheet while lean against in autoclave, slowly add concentration be 4.5mol/LNaOH aqueous solution to titanium sheet is flooded completely, build autoclave and be placed in air dry oven isothermal reaction 40h at 220 DEG C; (3) take out titanium sheet, after repeatedly rinsing with deionized water, be immersed in the HCl solution 14h of 0.12mol/L, titanium sheet taken out, repeatedly rinse with deionized water, cold wind dries up again, then in muffle furnace, 420 DEG C of annealing naturally cooled to room temperature after 3.5 hours, obtained the TiO of Anatase
2nanobelt; (4) by TiO
2nanobelt is first immersed in the AgNO that 50mL concentration is 5mmol/L
34min in solution, after taking out, level is dried, then is immersed in the NaBH that 50mL concentration is 2.2mmol/L
44min in solution, takes out sample, and after clean with deionized water rinsing, naturally dry, then repeat immersion process 4 times, the Ag/TiO2NBs identified as samples of acquisition is designated as S
5, namely soak the sample of 5 times.
Embodiment 3
(1) by titanium sheet successively with after acetone, EtOH Sonicate cleaning 20min, adopt chemical polishing process, then after repeatedly rinsing with distilled water under nitrogen protection cold wind dry up for subsequent use; (2) by polished titanium sheet while lean against in autoclave, slowly add concentration be 3.5mol/LNaOH aqueous solution to titanium sheet is flooded completely, build autoclave and be placed in air dry oven isothermal reaction 56h at 180 DEG C; (3) take out titanium sheet, after repeatedly rinsing with deionized water, be immersed in the HCl solution 10h of 0.08mol/L, titanium sheet taken out, repeatedly rinse with deionized water, cold wind dries up again, then in muffle furnace, 380 DEG C of annealing naturally cooled to room temperature after 2.5 hours, obtained the TiO of Anatase
2nanobelt; (4) by TiO
2nanobelt is first immersed in the AgNO that 50mL concentration is 3mmol/L
38min in solution, after taking out, level is dried, then is immersed in the NaBH that 50mL concentration is 1.8mmol/L
46min in solution, takes out sample, after clean with deionized water rinsing, naturally dries, the Ag/TiO of acquisition
2nBs identified as samples is designated as S
1, namely soak the sample of 1 time.
It should be noted last that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (6)
1. an Ag/TiO
2flexible, can the to reuse preparation method of SERS substrate, is characterized in that comprising the following steps:
(1) by titanium sheet successively with after acetone, EtOH Sonicate cleaning 20 ~ 40min, adopt chemical polishing process, then after repeatedly rinsing with distilled water under nitrogen protection cold wind dry up for subsequent use;
(2) by polished titanium sheet while lean against in autoclave, slowly add concentration be 3.5 ~ 4.5mol/LNaOH aqueous solution to titanium sheet is flooded completely, build autoclave and be placed in air dry oven isothermal reaction 36 ~ 72h at 180 ~ 220 DEG C;
(3) titanium sheet is taken out, after repeatedly rinsing with deionized water, be immersed in the HCl solution 10 ~ 14h of 0.08 ~ 0.12mol/L, again titanium sheet is taken out, repeatedly rinse with deionized water, cold wind dries up, and then in muffle furnace, 380 ~ 420 DEG C of annealing naturally cooled to room temperature after 2.5 ~ 3.5 hours, obtained the TiO of Anatase
2nanobelt;
(4) by TiO
2nanobelt is first immersed in the AgNO that 50mL concentration is 3 ~ 5mmol/L
34 ~ 8min in solution, after taking out, level is dried, then is immersed in the NaBH that 50mL concentration is 1.8 ~ 2.2mmol/L
44 ~ 6min in solution, takes out sample, after clean with deionized water rinsing, naturally dries, obtained Ag/TiO
2nanometer sheet, the charge capacity of Ag controls by soaking number of times.
2. Ag/TiO according to claim 1
2flexible, can the to reuse preparation method of SERS substrate, it is characterized in that: described titanium sheet is smooth, thickness is 0.2mm, and size is 30mm × 10mm.
3. Ag/TiO according to claim 1
2flexible, can the to reuse preparation method of SERS substrate, is characterized in that: described chemical polishing is HF:HNO in volume ratio
3: H
2carry out in the mixed liquor of O=1:1:4, be polished to till titanium plate surface is bright silver.
4. Ag/TiO according to claim 1
2flexible, can the to reuse preparation method of SERS substrate, is characterized in that: described immersion number of times is 1 ~ 5 time.
5. Ag/TiO according to claim 1
2flexible, can the to reuse preparation method of SERS substrate, is characterized in that: described annealing heating rate is 3 DEG C/min.
6. the Ag/TiO for preparing of method according to claim 1
2flexible, can to reuse SERS substrate, is characterized in that being prepared from by following steps:
(1) after titanium sheet being used successively acetone, ethanol ultrasonic cleaning 20 ~ 40min, adopt chemical polishing carry out polishing, then after repeatedly rinsing with distilled water under nitrogen protection cold wind dry up for subsequent use;
(2) by polished titanium sheet while lean against in autoclave, slowly add concentration be 3.5 ~ 4.5mol/LNaOH aqueous solution to titanium sheet is flooded completely, build autoclave and be placed in air dry oven isothermal reaction 40 ~ 56h at 180 ~ 220 DEG C;
(3) titanium sheet is taken out, after repeatedly rinsing with deionized water, be immersed in the HCl solution 10 ~ 14h of 0.08 ~ 0.12mol/L, again titanium sheet is taken out, repeatedly rinse with deionized water, cold wind dries up, and then in muffle furnace, 380 ~ 420 DEG C of annealing naturally cooled to room temperature after 2.5 ~ 3.5 hours, obtained the TiO of Anatase
2nanobelt;
(4) by TiO
2nanobelt is first immersed in the AgNO that 50mL concentration is 3 ~ 5mmol/L
34 ~ 8min in solution, after taking out, level is dried, then is immersed in the NaBH that 50mL concentration is 1.8 ~ 2.2mmol/L
44 ~ 6min in solution, takes out sample, after clean with deionized water rinsing, naturally dries, obtained Ag/TiO
2nanometer sheet, the charge capacity of Ag controls by soaking number of times.
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