CN109847732A - A kind of method and application preparing titanium dioxide nanoplate based on corona treatment - Google Patents
A kind of method and application preparing titanium dioxide nanoplate based on corona treatment Download PDFInfo
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- CN109847732A CN109847732A CN201811389899.5A CN201811389899A CN109847732A CN 109847732 A CN109847732 A CN 109847732A CN 201811389899 A CN201811389899 A CN 201811389899A CN 109847732 A CN109847732 A CN 109847732A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000002055 nanoplate Substances 0.000 title claims abstract description 32
- 238000003851 corona treatment Methods 0.000 title claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 68
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 37
- 239000001257 hydrogen Substances 0.000 claims abstract description 36
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052786 argon Inorganic materials 0.000 claims abstract description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011941 photocatalyst Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 33
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001868 water Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000002135 nanosheet Substances 0.000 claims description 2
- 238000006303 photolysis reaction Methods 0.000 claims description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 claims description 2
- 229960002050 hydrofluoric acid Drugs 0.000 claims 2
- 239000008246 gaseous mixture Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- 239000000243 solution Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000009832 plasma treatment Methods 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 210000002659 acromion Anatomy 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
It is a kind of that the method for titanium dioxide nanoplate and the application in Photocatalyzed Hydrogen Production are prepared based on corona treatment, belong to conductor photocatalysis material preparation technical field.Firstly, preparing titanium dioxide nanoplate using hydro-thermal reaction method using butyl titanate as presoma；Then in the mixed gas (Ar-H of argon gas and hydrogen2), the mixed gas (Ar-H of argon gas, hydrogen and nitrogen2‑N2) or argon gas and oxygen mixed gas (Ar-O2) gas atmosphere under carry out corona treatment, the surface of titanium dioxide nanoplate is modified.When titanium dioxide nanoplate photocatalyst after corona treatment of the present invention, the absorption in visible light region is remarkably reinforced, and the doping of the Lacking oxygen defect, nitrogen formed in treated sample, effectively increases its Photocatalyzed Hydrogen Production activity.
Description
Technical field
The invention belongs to conductor photocatalysis material preparation technical fields, and in particular to one kind is based on corona treatment system
The method and application of standby titanium dioxide nanoplate, the visible light photocatalysis of titanium dioxide nanoplate obtained produce hydrogen activity and obviously increase
By force.
Background technique
With the trend that the serious consumption and environmental pollution of global fossil fuel are got worse, develop it is environmental-friendly, low at
Originally, high performance energy conversion of new generation and storage system are essential.Wherein, solar energy is substantially considered a kind of
Inexhaustible energy, hydrogen are a kind of clean new energy.Realize that solar energy effectively turns to Hydrogen Energy using photocatalysis technology
Change, it is meant that the mankind are possible to permanent to solve the problems, such as environmental pollution and energy shortage.
Titanium dioxide (TiO2) have chemical stability is high, nontoxic, photoelectric conversion efficiency is high, lower-price characteristic,
So become a kind of most important semiconductor light-catalyst, and is widely used in air cleaning, waste water treatment, pollutant process
Equal fields.But the defects of its quantum efficiency is low, the recombination rate of electron-hole pair is high and band gap wide (3.2eV), hinders significantly
The development prospect of titanium dioxide.Currently, plasma technique is considered as a kind of preparing or being modified with high electron temperature and low
The effective means of the material of gas temperature.Plasma technique is that a kind of technique of low energy consumption will not without using any solvent
Chemical waste is generated, is a kind of new technique modified to solid-state material surface.Currently, using plasma technology is to titanium dioxide
The research that titanium is modified processing mainly includes handling (Pylnev, M. to black titanium dioxide metallic plasma；Chang,
W.-H.；Wong,M.-S.,Shel of black titania prepared by sputtering TiO2 target in
H2+ Ar plasma.Applied Surface Science 2018,462,285-290.), pure titinium dioxide nanometer sheet existed
Corona treatment (Kondratowicz, I. are carried out in a kind of atmosphere；Nadolska,M.；S.；M.；-Welenc,M.；Sawczak,M.；Yu,E.H.；Sadowski,W.；K.,Tailoring
properties of reduced graphene oxide by oxygen plasma treatment.Applied
Surface Science 2018,440,651-659.) etc..However, the non-plasma of above-mentioned document treated material
Photocatalyzed Hydrogen Production performance studied.
Summary of the invention
Titanium dioxide is prepared based on corona treatment in view of the defects in the background art, the present invention proposes one kind to receive
The method of rice piece and the application in Photocatalyzed Hydrogen Production.The method of the present invention is simple, short processing time, and obtained titanium dioxide is received
When rice piece is applied to Photocatalyzed Hydrogen Production, its photocatalytic activity can be effectively improved.
Technical scheme is as follows:
A method of titanium dioxide nanoplate is prepared based on corona treatment, which comprises the following steps:
Step 1 prepares titanium dioxide nanoplate using hydro-thermal reaction method；
Step 2, the titanium dioxide nanoplate that step 1 is prepared are placed on the sample stage of plasma-reaction-chamber, so
Plasma reaction chamber carries out vacuumize process afterwards, until the back end vacuum of reaction chamber reaches 10-4~10-6Pa；
Step 3, at room temperature, the mixed gas (Ar-H of argon gas and hydrogen is passed through into reaction chamber2), argon gas, hydrogen and nitrogen
Mixed gas (the Ar-H of gas2-N2) or argon gas and oxygen mixed gas (Ar-O2), until reacting indoor gas atmosphere
Reach 0.8~1.2Pa；
Step 4 keeps being continually fed into for mixed gas, plasma rf power supply is opened, in radio-frequency power supply reaction power
Under conditions of being 2.0~3.0GHz for 1400~1800W, radio-frequency power supply frequency, 15~60min is reacted, is closed after the reaction was completed
Radio-frequency power supply stops being passed through for mixed gas；Take out sample, the titanium dioxide nanoplate after corona treatment can be obtained.
Further, the process of titanium dioxide nanoplate is prepared described in step 1 using hydro-thermal reaction method specifically: firstly,
Butyl titanate is added in hydrofluoric acid, is uniformly mixed, obtains mixed liquor A, wherein the body of butyl titanate and hydrofluoric acid
Product is than being (2~25): 1；Then, mixed liquor A is transferred in the reaction kettle of polytetrafluoroethyllining lining, is lauched at 160~200 DEG C
Thermal response 18~for 24 hours, after the reaction was completed, cooled to room temperature is taken out；Finally, the reaction solution after reaction is centrifugated, obtain
To precipitating deionized water and ethyl alcohol be successively respectively adopted clean 3 times, and the dry 6h at 60~80 DEG C, grinding obtain dioxy
Change titanium nanometer sheet.
Further, in the mixed gas of argon gas described in step 3 and hydrogen, the flow-rate ratio of argon gas and hydrogen is 1:(0.5
~2)；In the mixed gas of the argon gas, hydrogen and nitrogen, the flow-rate ratio of argon gas, hydrogen and nitrogen is 1:(0.5~2): (0.5
~2)；In the mixed gas of the argon gas and oxygen, the flow-rate ratio of argon gas and oxygen is 1:(0.5~2).
The titanium dioxide nanosheet photocatalyst being prepared the present invention also provides the above method is in photolysis water hydrogen
Application.
Compared with prior art, the invention has the benefit that
1, the present invention provides a kind of methods for preparing titanium dioxide nanoplate based on corona treatment, firstly, with titanium
Sour four butyl esters are presoma, prepare titanium dioxide nanoplate using hydro-thermal reaction method, then carry out under different gas atmospheres
Plasma treatment is modified the surface of titanium dioxide nanoplate.Nano titania after corona treatment of the present invention
When piece photocatalyst, the absorption in visible light region is remarkably reinforced, and formed in treated sample Lacking oxygen defect,
The doping of nitrogen effectively increases its Photocatalyzed Hydrogen Production activity.
2, the present invention provides a kind of methods for preparing titanium dioxide nanoplate based on corona treatment, have technique letter
It the advantages that single, easy to operate, process cycle is short, can be widely applied in the modification of titanium dioxide optical catalyst.
Detailed description of the invention
The XRD diffracting spectrum (a) for the sample that Fig. 1 is Examples 1 to 3, comparative example 1 obtains, embodiment 1-2 and comparative example 1
The full spectrogram (b) of XPS, the EPR map (c) of embodiment 1-2；
The UV-vis DRS map (a) and forbidden bandwidth figure for the sample that Fig. 2 is Examples 1 to 3, comparative example 1 obtains
(b)；
The scanning electron microscope (SEM) photograph (SEM) and transmission electron microscope picture (TEM) for the sample that Fig. 3 is Examples 1 to 3, comparative example 1 obtains；
Wherein, (a) is the SEM of embodiment 1, (b) is the SEM of embodiment 2, (c) is the SEM of embodiment 3, (d) is the TEM of comparative example 1；
Photocatalyzed Hydrogen Production performance map of the sample that Fig. 4 is Examples 1 to 3, comparative example 1 obtains under visible optical radiation；
Fig. 5 is that the embodiment of the present invention 1~3 is catalyzed the mechanism figure for producing hydrogen under light illumination.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiments.It should be understood that institute
Purpose for embodiment is the content that the present invention is further explained, and cannot be construed to protect the present invention in any sense
The limitation of range.
Embodiment 1
A method of titanium dioxide nanoplate is prepared based on corona treatment, which comprises the following steps:
Step 1 prepares titanium dioxide nanoplate using hydro-thermal reaction method；
1.1 25mL butyl titanate is added in 3mL hydrofluoric acid (concentration 40%), is uniformly mixed, is mixed
Liquid A；
1.2 are transferred to mixed liquor A in the reaction kettle of polytetrafluoroethyllining lining, and hydro-thermal reaction for 24 hours, is reacted at 180 DEG C
After the completion, cooled to room temperature is taken out；
1.3 are centrifugated the reaction solution after reaction, and deionized water and ethyl alcohol cleaning 3 is successively respectively adopted in obtained precipitating
It is secondary, and the dry 6h at 80 DEG C, grinding obtain titanium dioxide nanoplate；
Step 2, the sample stage that the 0.1g titanium dioxide nanoplate that step 1 is prepared is placed in plasma-reaction-chamber
On, then plasma reaction chamber carries out vacuumize process, until the back end vacuum of reaction chamber reaches 10-4Pa；
Step 3, at room temperature, the mixed gas (Ar-H of argon gas and hydrogen is passed through into reaction chamber2), until reacting indoor
Gas atmosphere reaches 1.07Pa, wherein the flow of argon gas is 20sccm, and the flow of hydrogen is 20sccm；
Step 4 keeps being continually fed into for mixed gas, plasma rf power supply is opened, in radio-frequency power supply reaction power
Under conditions of being 2.45GHz for 1600W, radio-frequency power supply frequency, 30min is reacted, closes radio-frequency power supply after the reaction was completed, is stopped mixed
Close being passed through for gas；It takes out sample (grey powder), the titanium dioxide nanoplate after corona treatment can be obtained.
Embodiment 2
Compared with Example 1, difference is the present embodiment: in step 3, at room temperature, argon gas, hydrogen is passed through into reaction chamber
With the mixed gas (Ar-H of nitrogen2-N2), until reacting indoor gas atmosphere reaches 1.07Pa, wherein the flow of argon gas is
30sccm, the flow of hydrogen are 20sccm, and the flow of nitrogen is 40sccm；In step 4, being continually fed into for mixed gas is kept,
Plasma rf power supply is opened, under conditions of radio-frequency power supply reaction power is 1600W, radio-frequency power supply frequency is 2.45GHz,
30min is reacted, radio-frequency power supply is closed after the reaction was completed, stops being passed through for mixed gas；It takes out sample (buff powder)
Titanium dioxide nanoplate after obtaining corona treatment.
Embodiment 3
Compared with Example 1, difference is the present embodiment: in step 3, at room temperature, argon gas and oxygen is passed through into reaction chamber
Mixed gas (the Ar-O of gas2), until reacting indoor gas atmosphere reaches 1.07Pa, wherein the flow of argon gas is 10sccm,
The flow of oxygen is 20sccm；In step 4, being continually fed into for mixed gas is kept, plasma rf power supply is opened, in radio frequency
Under conditions of power supply reaction power is 1600W, radio-frequency power supply frequency is 2.45GHz, 30min is reacted, closes penetrate after the reaction was completed
Frequency power stops being passed through for mixed gas；It takes out sample (off-white powder), the titanium dioxide after corona treatment can be obtained
Titanium nanometer sheet.
Comparative example 1
By step 1 obtains in embodiment 1 titanium dioxide nanoplate as a comparison case 1.
The XRD diffracting spectrum (a) for the sample that Fig. 1 is Examples 1 to 3, comparative example 1 obtains, embodiment 1-2 and comparative example 1
The full spectrogram (b) of XPS, the EPR map (c) of embodiment 1-2.Fig. 1 (a) display, plasma treated sample are still
Anatase titania, but crystallinity has significantly different, and the degree of crystallization of embodiment 1 is remarkably reinforced.Fig. 1 (b) display, embodiment
2 there is nitrogen-doping in plasma treatment procedure.Fig. 1 (c) display, embodiment 1 is in plasma treatment procedure
Introduce a large amount of Lacking oxygen.
The UV-vis DRS map (a) and forbidden bandwidth figure for the sample that Fig. 2 is Examples 1 to 3, comparative example 1 obtains
(b).As shown in Figure 2, the sample that embodiment 1 obtains has very high optical absorption intensity in visible light region and forbidden bandwidth becomes
Narrow, this is allowed in illumination, and the sample that embodiment 1 obtains is easier that electronics transfer occurs；The sample that embodiment 2 obtains is can
There is an acromion in light-exposed region, and forbidden bandwidth broadens；3 sample of embodiment has strongest light absorption energy in UV light region
Power, but it is basic identical with the intensity of comparative example 1 in visible light region.
The scanning electron microscope (SEM) photograph (SEM) and transmission electron microscope picture (TEM) for the sample that Fig. 3 is Examples 1 to 3, comparative example 1 obtains；
Wherein, (a) is the SEM of embodiment 1, (b) is the SEM of embodiment 2, (c) is the SEM of embodiment 3, (d) is the TEM of comparative example 1；
From the figure 3, it may be seen that Examples 1 to 3 sample remains as nanometer sheet pattern, show the corona treatment of room temperature to the pattern of sample not
Can have an impact.
The sample that Examples 1 to 3, comparative example 1 are obtained carries out Photocatalyzed Hydrogen Production activity test in visible optical radiation, specifically
Process are as follows:
(1) Glycerine-Aqueous Solution that dose volume concentration is 10%；
(2) each 20mg of sample that Example 1~3, comparative example 1 obtain respectively, is separately added into the there-necked flask of 4 100mL
It is interior, then the Glycerine-Aqueous Solution of the above-mentioned preparation of 80mL is added thereto respectively；
(3) 0.1% H is added into three-necked flask respectively2PtCl6·H2O solution (10gL-1), it is placed under full light and shines
20min is penetrated, then three-necked flask is sealed using rubber stopper and rubber tube；
(4) it is passed through nitrogen while stirring to remove the gas dissolved in air and water in flask, after 20min, clamps rubber
Leather hose is to prevent gas leakage；
(5) by step 4, treated that three-necked flask is placed under the xenon lamp equipped with visible filter irradiates 1h, irradiates
While keep magnetic agitation to come into full contact with photochemical catalyst with solution, utilize gas chromatograph to measure and generated in three-necked flask
Hydrogen.
Photocatalyzed Hydrogen Production performance map of the sample that Fig. 4 is Examples 1 to 3, comparative example 1 obtains under visible optical radiation；By
Fig. 4 is it is found that the Photocatalyzed Hydrogen Production activity for the sample that Examples 1 to 3 obtains is above comparative example 1.
Fig. 5 is that the embodiment of the present invention 1~3 is catalyzed the mechanism figure for producing hydrogen under light illumination；The photocatalytic activity of 1 sample of embodiment
Mainly due to the presence of Lacking oxygen, embodiment 2 is then due to foring impurity energy level, the case where forbidden bandwidth broadens for enhancing
Under still have the photocatalytic activity of opposite enhancing, the photocatalytic activity of 3 sample of embodiment enhancing is due to having the activity electricity increased
Son.
It should be pointed out that specific embodiment described above can make those skilled in the art that this hair be more fully understood
It is bright, but do not limit the invention in any way.Therefore, it will be appreciated by those skilled in the art that still can be carried out to the present invention
Modification or equivalent replacement；And all do not depart from the technical solution and its improvement of spirit and technical spirit of the invention, it should all
Cover in the scope of protection of the patent of the present invention.
Claims (4)
1. a kind of method for preparing titanium dioxide nanoplate based on corona treatment, which comprises the following steps:
Step 1 prepares titanium dioxide nanoplate using hydro-thermal reaction method；
Step 2, the titanium dioxide nanoplate that step 1 is prepared are placed on the sample stage of plasma-reaction-chamber, then right
Plasma-reaction-chamber carries out vacuumize process, until the back end vacuum of reaction chamber reaches 10-4~10-6Pa；
Step 3, at room temperature, the mixed gas of argon gas and hydrogen, the gaseous mixture of argon gas, hydrogen and nitrogen are passed through into reaction chamber
The mixed gas of body or argon gas and oxygen, until reacting indoor gas atmosphere up to 0.8~1.2Pa；
Step 4 keeps being continually fed into for mixed gas, opens plasma rf power supply, is in radio-frequency power supply reaction power
Under conditions of 1400~1800W, radio-frequency power supply frequency are 2.0~3.0GHz, 15~60min is reacted, closes penetrate after the reaction was completed
Frequency power stops being passed through for mixed gas；It takes out, the titanium dioxide nanoplate after corona treatment can be obtained.
2. the method according to claim 1 for preparing titanium dioxide nanoplate based on corona treatment, which is characterized in that
The process of titanium dioxide nanoplate is prepared described in step 1 using hydro-thermal reaction method specifically: firstly, hydrogen is added in butyl titanate
It in fluoric acid, is uniformly mixed, obtains mixed liquor A, wherein the volume ratio of butyl titanate and hydrofluoric acid is (2~25): 1；So
Afterwards, mixed liquor A is transferred in the reaction kettle of polytetrafluoroethyllining lining, the hydro-thermal reaction 18~for 24 hours at 160~200 DEG C, reaction
After the completion, cooled to room temperature is taken out；Finally, the reaction solution after reaction is centrifugated, obtained precipitating is successively adopted respectively
It is cleaned 3 times with deionized water and ethyl alcohol, and the dry 6h at 60~80 DEG C, grinding obtain titanium dioxide nanoplate.
3. the method according to claim 1 for preparing titanium dioxide nanoplate based on corona treatment, which is characterized in that
In the mixed gas of argon gas described in step 3 and hydrogen, the flow-rate ratio of argon gas and hydrogen is 1:(0.5~2)；The argon gas, hydrogen
In the mixed gas of gas and nitrogen, the flow-rate ratio of argon gas, hydrogen and nitrogen is 1:(0.5~2): (0.5~2)；The argon gas and
In the mixed gas of oxygen, the flow-rate ratio of argon gas and oxygen is 1:(0.5~2).
4. the titanium dioxide nanosheet photocatalyst that any one of claims 1 to 3 the method obtains is in photolysis water hydrogen
Application.
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| CN110589883A (en) * | 2019-09-23 | 2019-12-20 | 安徽师范大学 | Two-dimensional layered titanium dioxide nano material rich in oxygen holes, preparation method and application thereof |
| CN110624535A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | Black bismuth tungstate photocatalyst as well as preparation method and application thereof |
| CN110653004A (en) * | 2019-09-05 | 2020-01-07 | 上海化工研究院有限公司 | Catalyst for trapping and catalyzing VOCs degradation and preparation method and application thereof |
| CN111013560A (en) * | 2019-12-26 | 2020-04-17 | 西南石油大学 | Oxygen-deficient titanium dioxide catalyst, preparation method and application thereof |
| CN112387264A (en) * | 2020-11-16 | 2021-02-23 | 西南石油大学 | TiO based on plasma treatment2Method of modifying TiO2Photocatalyst and application |
| CN113764687A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | A bifunctional electrocatalyst for an air electrode of a high-efficiency zinc-air battery is disclosed: ultra-thin ternary nanosheet FePSe treated by plasma3Preparation and use of |
| CN114684864A (en) * | 2022-04-15 | 2022-07-01 | 东南大学 | Preparation method and application of transition metal oxide electrode material |
-
2018
- 2018-11-21 CN CN201811389899.5A patent/CN109847732A/en active Pending
Non-Patent Citations (5)
| Title |
|---|
| XIANGCHEN KONG ET AL: ""Defect enhances photocatalytic activity of ultrathin TiO2 (B) nanosheets for hydrogen production by plasma engraving method"", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
| 向全军: ""二氧化钛基光催化材料的微结构调控与性能增强"", 《中国博士学位论文全文数据库》 * |
| 唐伟忠: "《薄膜材料制备原理、技术及应用》", 31 January 2003 * |
| 崔玉民等: "《二氧化钛光催化技术》", 31 December 2010, 中国书籍出版社 * |
| 徐淑艳: "《钛硼碳氮系硬质薄膜制备、结构及性能》", 31 December 2017, 东北林业大学出版社 * |
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| CN110273165A (en) * | 2019-07-24 | 2019-09-24 | 台州学院 | A kind of method that lower temperature plasma technology prepares oxygen defect type bismuth tungstate optoelectronic pole |
| CN110653004A (en) * | 2019-09-05 | 2020-01-07 | 上海化工研究院有限公司 | Catalyst for trapping and catalyzing VOCs degradation and preparation method and application thereof |
| CN110624535A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | Black bismuth tungstate photocatalyst as well as preparation method and application thereof |
| CN110589883A (en) * | 2019-09-23 | 2019-12-20 | 安徽师范大学 | Two-dimensional layered titanium dioxide nano material rich in oxygen holes, preparation method and application thereof |
| CN111013560A (en) * | 2019-12-26 | 2020-04-17 | 西南石油大学 | Oxygen-deficient titanium dioxide catalyst, preparation method and application thereof |
| CN111013560B (en) * | 2019-12-26 | 2022-05-10 | 西南石油大学 | Oxygen-deficient titanium dioxide catalyst, preparation method and application thereof |
| CN113764687A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | A bifunctional electrocatalyst for an air electrode of a high-efficiency zinc-air battery is disclosed: ultra-thin ternary nanosheet FePSe treated by plasma3Preparation and use of |
| CN112387264A (en) * | 2020-11-16 | 2021-02-23 | 西南石油大学 | TiO based on plasma treatment2Method of modifying TiO2Photocatalyst and application |
| CN112387264B (en) * | 2020-11-16 | 2022-02-08 | 西南石油大学 | TiO based on plasma treatment2Method of modifying TiO2Photocatalyst and application |
| CN114684864A (en) * | 2022-04-15 | 2022-07-01 | 东南大学 | Preparation method and application of transition metal oxide electrode material |
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