CN105396581B - The method that gold improves branch photocatalytic activity is carried in the middle of a kind of - Google Patents
The method that gold improves branch photocatalytic activity is carried in the middle of a kind of Download PDFInfo
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- CN105396581B CN105396581B CN201510368511.3A CN201510368511A CN105396581B CN 105396581 B CN105396581 B CN 105396581B CN 201510368511 A CN201510368511 A CN 201510368511A CN 105396581 B CN105396581 B CN 105396581B
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- 239000010931 gold Substances 0.000 title claims abstract description 24
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 66
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 57
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000010936 titanium Substances 0.000 claims abstract description 44
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 43
- 229910052751 metal Inorganic materials 0.000 claims abstract description 39
- 239000002184 metal Substances 0.000 claims abstract description 39
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 22
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims abstract description 19
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 5
- 239000002070 nanowire Substances 0.000 description 24
- 239000002253 acid Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- 239000005864 Sulphur Substances 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001258 titanium gold Inorganic materials 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Abstract
The invention discloses a kind of method for effectively improving apparatus derivatorius titanium dioxide nano thread film photocatalytic activity by middle load gold, comprise the following steps：Nitric acid and melamine are added in hydrogen peroxide solution, reaction solution I is obtained；Metallic titanium plate is immersed in reaction solution I, reacted 12 ~ 72 hours；Metal titanium sheet is taken out, is cleaned with deionized water, is dried, is heat-treated 0.5 ~ 5 hour；Addition gold chloride and methanol, obtain reaction solution II in deionized water；Metal titanium sheet after heat treatment is immersed in reaction solution II, after ultraviolet light, then is immersed in sulfuric acid solution, is reacted 12 ~ 72 hours, is cleaned, dried with deionized water, obtain apparatus derivatorius titanium dioxide nano thread film.The present invention is effectively increased nanogold particle and titanium dioxide contact area, is significantly improved the photocatalytic activity of film using the middle method for carrying gold.
Description
Technical field
Carried the present invention relates to a kind of method for improving titanium deoxid film photocatalytic activity, more particularly to a kind of middle gold that carries
The method of high branch structure titanium dioxide nano wire film photocatalytic activity, belongs to field of new materials.
Background technology
It is excellent that titanium deoxid film has that inexpensive, nontoxic, chemical property is stable, catalytic activity is high and can recycle etc.
Point, has a wide range of applications in fields such as photocatalysis, photoelectrocatalysis, solar cell and gas sensors.Common titanium dioxide
Titanium film structure includes nano wire, nano flower, nanometer rods etc..Relative to above-mentioned nanostructured, titanium dioxide branched structure has
Larger specific surface area, is more beneficial for fully contacting with reactant, meanwhile, there is the multiple scattering of light to act on for it, can promote
Light absorbs, and then improve the utilization ratio of light.One-dimensional titanium dioxide apparatus derivatorius has been provided simultaneously with the characteristic and one of branched structure
The excellent electronic conductivity energy of dimension nanometer construction, with unique advantage.
Pure titinium dioxide film is applied to photocatalysis field, and its activity is restricted by two factors：First, it is raw after light is excited
Into electronics and hole easily be combined, quantum efficiency is low；2nd, the energy gap of titanium dioxide is 3.2 eV, corresponding excitation wavelength
For 387 nm, 5% up to the sunshine gross energy on ground can only be absorbed to, it is seen that light utilization ratio is extremely low.In order to improve quantum effect
Rate and visible light utilization efficiency to titanium deoxid film, it is necessary to carry out suitably being modified.Research shows, by nanogold particle and titanium dioxide
Titanium film is compound can to effectively improve its photocatalytic activity.Modified advantage is：First, due to Fermi's energy of titanium dioxide and gold
Level is different, and both form Schottky barrier after contacting, and trap is captured as electronics, can effectively suppress catalytic inner electricity
Son-hole it is compound；2nd, unique surface plasma bulk effect that nanogold particle has, the spectrum that can expand catalyst rings
Scope is answered to visible region.
The content of the invention
Carry gold to improve apparatus derivatorius titanium dioxide nano thread film light by centre it is an object of the invention to provide one kind
The method of catalytic activity.
The present invention carries the method that gold improves apparatus derivatorius titanium dioxide nano thread film photocatalytic activity, its feature middle
It is, comprises the following steps：
1) it is addition nitric acid and melamine in 30% hydrogen peroxide solution to mass percent concentration, mixes to obtain reaction solution
I, wherein concentration of nitric acid are 0.34~0.45 mol/L, and melamine concentration is 0.016~0.024 mol/L；
2) metal titanium sheet is immersed in reaction solution I, reacted 12 ~ 72 hours at 60 ~ 90 DEG C；
3) by step 2）The metal titanium sheet of gained is cleaned with deionized water, is dried, and is then heat-treated at 240 ~ 280 DEG C
0.5 ~ 5 hour；
4）Addition gold chloride and methanol in deionized water, mixes to obtain reaction solution II, wherein the concentration of gold chloride be 5.2 ×
10-6~3.4 × 10-4Mol/L, methanol concentration is 0.2 × 10-3~1.28 mol/Ls；
5）By step 3）The metal titanium sheet of gained is immersed in reaction solution II, ultraviolet light 1 ~ 20 minute；
6) by step 5）The metal titanium sheet of gained is cleaned with deionized water, dried, and is placed in 60 ~ 90 DEG C of hot water, is used sulfuric acid
PH value is adjusted to 1.0 ~ 3.0, reaction is taken out after 12~72 hours, with deionized water rinsing, is dried.
The device have the advantages that being：
The present invention is introduced using the middle method for carrying gold that is, in apparatus derivatorius titanium dioxide nano thread membrane-film preparation process
Nanogold particle, effectively increases nanogold particle and titanium dioxide contact area, so as to significantly improve the photocatalysis of film
Activity.With first obtaining branched structure titanium dioxide nano thread film and compared with the routine techniques of rear bearing gold, film of the invention exists
Under ultraviolet light and visible ray significantly higher photocatalytic activity is shown during rhodamine B in degradation water.
Brief description of the drawings
Fig. 1 is the high power Flied emission scanning electron microscopy of apparatus derivatorius titanium dioxide nano thread film prepared by embodiment 1
Mirror photo；
Fig. 2 is the low power Flied emission scanning electron microscopy of apparatus derivatorius titanium dioxide nano thread film prepared by embodiment 1
Mirror photo；
Fig. 3 is the section high power Flied emission scanning electron of apparatus derivatorius titanium dioxide nano thread film prepared by embodiment 1
Microphotograph；
Fig. 4 is the X-ray diffractogram of each stage acquisition sample in the preparation process of embodiment 1, and wherein curve (a) is step
2）Obtain the X-ray diffractogram of sample；Curve (b) is step 3）Obtain the X-ray diffractogram of sample；Curve (c) final sample
X-ray diffractogram；A is anatase in figure, and R is rutile, and H is hydrogen metatitanic acid, and Ti is titanium-base, and S is uhligite；
Fig. 5 is the transmission electron microscope photo of apparatus derivatorius titanium dioxide nano thread film prepared by embodiment 1；
Fig. 6 carries golden sample and the golden sample of middle load photocatalytic degradation water under ultraviolet light not carry golden sample, common process
Middle rhodamine B concentration is with light application time change curve；
Fig. 7 is the corresponding pseudo-first-order dynamics fitting results of Fig. 6；
Fig. 8 carries golden sample and the golden sample of middle load photocatalytic degradation water under visible light not carry golden sample, common process
Middle rhodamine B concentration is with light application time change curve；
Fig. 9 is the corresponding pseudo-first-order dynamics fitting results of Fig. 8.
Embodiment
The present invention is expanded on further below in conjunction with the drawings and specific embodiments.But gold is carried in the middle of the present invention to improve branch
The method of structure titanium dioxide nano wire film is not limited solely to following embodiments.
Embodiment 1
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.45 mol/L, and melamine concentration is 0.016 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 48 hours at 80 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 260 DEG C at heat
Reason 1 hour, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II, wherein gold chloride concentration is 4.2 × 10 in deionized water-5
Mol/L, methanol concentration is 0.16 mol/L.
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity22 points of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 80 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 2.0, reaction is taken out after 48 hours, with deionized water rinsing, dries.
SEM high powers, low power and the section high power figure difference of sample made from this example are as shown in Figure 1,2 and 3, it can be seen that
Metal titanium sheet surface is uniformly distributed apparatus derivatorius titanium dioxide nano thread film, a diameter of 100~250nm of nanometer branch array
Between, length is about 1 micron, and membrane middle layer thickness is about 0.8 micron.Fig. 5 branch titanium dioxide transmission electron microscopy shines
Piece shows that the Au nanoparticle sizes supported are about 8 ~ 12 nanometers, are embedded between nano wire trunk and branch, with titanium dioxide
It is in close contact, forms heterojunction structure.As shown in figure 4, the nano-wire array that step 2 is obtained is hydrogen metatitanic acid；At step 3 heat
Hydrogen metatitanic acid diffraction maximum disappears after reason, the relatively low anatase diffraction maximum of intensity occurs；Anatase diffraction maximum becomes behind step 4,5,6
By force, while there is rutile and a small amount of uhligite diffraction maximum.It is less due to carrying gold amount, the diffraction of gold is not observed in figure
Peak.
Sample made from this example carries golden sample to be middle, it is same in addition under conditions of lack step 4, the 5 samples notes obtained
Not carry golden sample, it is same under conditions of step is adjusted to 1,2,3,6,4,5, golden step 4 will be carried, 5 branch knot is adjusted to
The sample obtained after structure growth carries rhodamine in golden sample, these three sample photocatalytic degradation water of contrast test for common process
The efficiency of B molecules；Specific method is as follows：
(1) ultraviolet catalytic performance：With 2.5 × 2.5 cm2Film is 5.0mW/cm in light intensity2To 25 under ultraviolet light
The catalytic degradation speed of 0.005 mM/l of rhodamine B of milliliter is characterized.
(2) visible light catalytic performance：With 2.5 × 2.5 cm2Film is 180mW/cm in light intensity2To 25 under radiation of visible light
The catalytic degradation speed of 0.005 mM/l of rhodamine B of milliliter is characterized.
Photocatalysis test includes the continuous magnetic force that carries out in dark absorption in 30 minutes and photocatalysis in 60 minutes, degradation process and stirred
Mix, every sampling in 15 minutes once.
Photocatalytic degradation rhodamine B meets pseudo-first order reaction kinetics：
ln(c/c 0 )=kt
Wherein, c0Degraded initial substrate concentration is represented, c represents that light-catalyzed reaction carries out the dense of reaction substrate after a period of time
Degree, k is reaction rate constant,tFor the time.
The change of target degradate concentrations is by UV-1800PC types ultraviolet-uisible spectrophotometer at its principal absorption wavelength
The change of corresponding absorbance is measured, and draws photocatalytic degradation curve, and carry out pseudo-first-order dynamics fitting.Three kinds of samples
Photocatalysis performance figure and its pseudo-first-order dynamics of the product under ultraviolet light are fitted respectively as shown in Figure 6 and Figure 8, in visible ray
Under then as shown in figures 7 and 9.
As can be seen that common process is carried after gold, Luo Dan in apparatus derivatorius titanium dioxide nano thread film photocatalytic degradation water
The efficiency of bright B molecules is greatly improved.The photocatalysis under ultraviolet light, visible ray can be obtained according to pseudo-first-order dynamics fitting result anti-
Answer rate constants k not carry the 2.80 of golden sample respectively, 3.55 times.After the technical scheme announced using the present invention, in conventional work
Skill is carried on the basis of gold, and the photocatalytic activity of apparatus derivatorius titanium dioxide nano thread film is further improved.By pseudo-first-order
Dynamics fitting result understands that light-catalyzed reaction rate constants k is respectively that common process carries golden sample under ultraviolet light, visible ray
1.98,1.09 times.
Embodiment 2
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.45 mol/L, and melamine concentration is 0.016 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 48 hours at 80 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 260 DEG C at heat
Reason 1 hour, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II in deionized water；Wherein gold chloride concentration 3.4 × 10-4Rub
You/liter, 1.28 mM/ls of methanol concentration；
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity21 point of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 80 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 2.0, reaction is taken out after 48 hours, with deionized water rinsing, dries.
Embodiment 3
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.45 mol/L, and melamine concentration is 0.016 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 12 hours at 90 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 260 DEG C at heat
Reason 1 hour, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II, wherein gold chloride concentration is 5.2 × 10 in deionized water-6
Mol/L, methanol concentration is 0.2 × 10-3Mol/L.
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity220 points of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 80 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 2.0, reaction is taken out after 48 hours, with deionized water rinsing, dries.
Embodiment 4
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.45 mol/L, and melamine concentration is 0.016 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 72 hours at 60 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 240 DEG C at heat
Reason 5 hours, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II, wherein gold chloride concentration is 4.2 × 10 in deionized water-5
Mol/L, methanol concentration is 0.16 mol/L.
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity22 points of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 80 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 2.0, reaction is taken out after 48 hours, with deionized water rinsing, dries.
Embodiment 5
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.34 mol/L, and melamine concentration is 0.016 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 48 hours at 80 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 280 DEG C at heat
Reason 0.5 hour, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II, wherein gold chloride concentration is 4.2 × 10 in deionized water-5
Mol/L, methanol concentration is 0.16 mol/L.
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity22 points of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 80 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 2.0, reaction is taken out after 48 hours, with deionized water rinsing, dries.
Embodiment 6
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.45 mol/L, and melamine concentration is 0.024 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 48 hours at 80 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 260 DEG C at heat
Reason 1 hour, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II, wherein gold chloride concentration is 4.2 × 10 in deionized water-5
Mol/L, methanol concentration is 0.16 mol/L.
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity22 points of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 60 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 1.0, reaction is taken out after 12 hours, with deionized water rinsing, dries.
Embodiment 7
Step 1 preparation of nano line reaction solution
Addition nitric acid and melamine in mass percent concentration is 30% hydrogen peroxide solution, mix to obtain reaction solution I,
Wherein concentration of nitric acid is 0.45 mol/L, and melamine concentration is 0.016 mol/L；
Step 2 prepares nano-wire array
Clean metal titanium sheet is immersed in reaction solution I, reacted 48 hours at 80 DEG C.
Step 3 nano wire intermediate heat-treatment
Metal titanium sheet deionized water obtained by step 2 is cleaned in ultrasonic wave, dried, then at 260 DEG C at heat
Reason 1 hour, 5 DEG C/min of heating rate, furnace cooling.
Step 4, which is prepared, carries golden reaction solution
Addition gold chloride and methanol, mix to obtain reaction solution II, wherein gold chloride concentration is 4.2 × 10 in deionized water-5
Mol/L, methanol concentration is 0.16 mol/L.
Gold is carried in the middle of step 5
Metal titanium sheet obtained by step 3 is immersed in reaction solution II, is 5mW/cm with intensity22 points of ultraviolet light
Clock.
Step 6 nano wire branch growth
Metal titanium sheet obtained by step 5 is cleaned with deionized water, dried, is placed in 90 DEG C of hot water, uses sulphur acid for adjusting pH
It is worth 3.0, reaction is taken out after 72 hours, with deionized water rinsing, dries.
Claims (1)
1. the method that gold improves apparatus derivatorius titanium dioxide nano thread film photocatalytic activity is carried in the middle of a kind of, it is characterised in that
Comprise the following steps：
1) it is addition nitric acid and melamine in 30% hydrogen peroxide solution to mass percent concentration, mixes to obtain reaction solution I, its
Middle concentration of nitric acid is 0.34~0.45 mol/L, and melamine concentration is 0.016~0.024 mol/L；
2) metal titanium sheet is immersed in reaction solution I, reacted 12 ~ 72 hours at 60 ~ 90 DEG C；
3) by step 2）The metal titanium sheet of gained is cleaned with deionized water, is dried, and 0.5 ~ 5 is then heat-treated at 240 ~ 280 DEG C
Hour；
4）Addition gold chloride and methanol, mix to obtain reaction solution II, the wherein concentration of gold chloride is 5.2 × 10 in deionized water-6
~3.4 × 10-4Mol/L, methanol concentration is 0.2 × 10-3~1.28 mol/Ls；
5）By step 3）The metal titanium sheet of gained is immersed in reaction solution II, ultraviolet light 1 ~ 20 minute；
6) by step 5）The metal titanium sheet of gained is cleaned with deionized water, dried, and is placed in 60 ~ 90 DEG C of hot water, is adjusted with sulfuric acid
PH value is to 1.0 ~ 3.0, and reaction is taken out after 12~72 hours, with deionized water rinsing, dries.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350346A (en) * | 2011-08-09 | 2012-02-15 | 福州大学 | Preparation method of visible light catalyst with surface plasmon effect and application thereof |
| CN102557130A (en) * | 2012-02-22 | 2012-07-11 | 浙江大学 | Method for preparing titanium dioxide nanoflower array film |
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| US20100167914A1 (en) * | 2008-12-29 | 2010-07-01 | Vive Nano, Inc. | Nano-scale catalysts |
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| CN102350346A (en) * | 2011-08-09 | 2012-02-15 | 福州大学 | Preparation method of visible light catalyst with surface plasmon effect and application thereof |
| CN102557130A (en) * | 2012-02-22 | 2012-07-11 | 浙江大学 | Method for preparing titanium dioxide nanoflower array film |
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