CN109876828B - TNT/CdS/TiO2Pt core-shell structure nanotube and preparation method thereof - Google Patents
TNT/CdS/TiO2Pt core-shell structure nanotube and preparation method thereof Download PDFInfo
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Abstract
The invention discloses TNT/CdS/TiO2Pt core-shell structure nanotube and preparation method thereof. The nanotube is sequentially a titanium acid nanotube TNT/CdS quantum dot/TiO from inside to outside2Shell/metal Pt. The method comprises the steps of preparing a titanic acid nanotube carrier (TNT) by a hydrothermal method, preparing CdS quantum dots by a hot injection method, taking the titanic acid nanotube carrier (TNT) as a main body, and growing TiO by adopting an atomic layer deposition technology after loading the CdS quantum dots2Preparing TNT/CdS/TiO by using shell and loaded Pt2Pt core-shell structure nanotube. The core-shell structure composite material prepared by the invention has the advantages of regular structure, ordered electron transfer path, good stability and excellent photocatalytic activity, and has good application in lithium ion batteries, supercapacitors, gas sensing, photocatalysis and the like.
Description
Technical Field
The invention relates to a core-shell structure nanotube and a preparation method thereof, in particular to TNT/CdS/TiO2Pt core-shell structure nanotube and preparation method thereof.
Background
In recent years, human society has faced two major problems of energy shortage and environmental pollution. Since the stage of entering industrialization, the human society has been rapidly increasing in the emission of industrial pollution and the consumption of energy. Therefore, the development of new energy sources which are sustainable, environment-friendly and low in price through the development of science and technology and the innovation of technology has great significance. Solar energy is a pollution-free, sustainable, energy-intensive and ubiquitous source of energy that is considered the most desirable alternative to fossil energy. Today, the conversion of solar energy into other forms of secondary energy (such as electric energy and chemical energy) is the direction of intensive research by scientists. In the chemical energy system, hydrogen energy is increasingly valued by scientists. Because the hydrogen element is rich on the earth, exists in water in large quantity, has the characteristics of high combustion value and high efficiency, and the only product after combustion is water, clean and pollution-free. In addition, the hydrogen has no toxicity, is easy to store and convenient to transport, and is relatively safe to use. Therefore, hydrogen energy is one of the most ideal green pollution-free new energy sources. Therefore, how to convert solar energy into hydrogen energy becomes one of the main research fields of scientists, and hydrogen production by solar photocatalytic water splitting has attracted much attention in recent years in all countries around the world.
In photocatalytic systems of semiconductor materials, TiO2The method has the advantages of low price, no toxicity, high stability, good ultraviolet hydrogen production activity, rich natural storage capacity and the like. The CdS forbidden band is narrow, has strong absorption capacity in a visible light region and high photocatalytic activity, and is widely concerned in the field of photocatalytic research for many years. However, TiO2The problems of large forbidden band width, low solar energy utilization rate, easy recombination of photon-generated carriers and low photocatalysis efficiency exist. CdS is extremely easy to be corroded by light in an aqueous solution, has poor stability and certain toxicity and can cause environmental pollution. To TiO 22The CdS modified by the method has the advantages of improving the visible light response capability, improving the stability of the CdS modified by the method, and having important significance for practical application.
In order to improve the light utilization rate and quantum efficiency, currently, there are several commonly used semiconductor photocatalyst modification techniques, mainly including size quantization, semiconductor compounding, co-catalyst loading, heterojunction formation, and the like. The electronic transmission path can be shortened by the quantization of the catalyst size; the semiconductor compounding method is to utilize two kinds of semiconductor compounding with energy band position matching, and the energy level coupling effect promotes charge separation; the platinum-carrying cocatalyst can form a Schottky potential energy barrier, which is beneficial to capturing electrons; after the heterojunction is formed, a built-in electric field for promoting the electron-hole separation can be generated in the heterojunction. TiO 22Can be well type-II compounded with CdS, and titanic acid nano-tube and TiO with different crystal forms2The heterogeneous phase can be formed, Pt is loaded to provide active sites, the recombination of electrons and holes is inhibited, the quantum efficiency is improved, the absorption range of light is expanded, and the hydrogen production activity and the visible light utilization efficiency are improved.
The existing titanium dioxide, cadmium sulfide and platinum ternary photocatalyst has disordered appearance, structure and recombination position, the electron transfer path is complicated, most of photo-generated electron hole pairs can be recombined, and the quantum efficiency is reduced. Therefore, the reasonable design of the catalyst structure and morphology, the regulation of the electron transfer path and the improvement of the separation efficiency of the electron hole pairs are of great importance.
Disclosure of Invention
The invention aims to provide TNT/CdS/TiO with ordered structure, good stability, high photocatalytic efficiency and simple preparation method2Pt core-shell structure nanotube and preparation method thereof.
TNT/CdS/TiO2The Pt core-shell structure nanotube sequentially comprises a titanic acid nanotube carrier (TNT)/loaded CdS quantum dots/TiO from inside to outside2Shell/supported metal Pt. Growing TiO through loaded CdS quantum dots by using titanic acid nanotube carrier (TNT) as a main body2The shell layer and the supported metal Pt form a composite material. The diameter of the titanic acid nanotube carrier (TNT) is 50-300 nanometers, the diameter of the CdS quantum dot is 4-6 nanometers, and the titanic acid nanotube carrier (TNT) and TiO2The shell layer forming a heterojunction, TiO2The thickness of the shell layer is 1-8 nanometers, and the size of the metal Pt particles is 0.5-3 nanometers.
Preparation of the above TNT/CdS/TiO2The method for preparing the Pt core-shell structure nanotube comprises the following steps:
preparing a titanic acid nanotube carrier (TNT): TiO 2 of commercial products2Adding NaOH (10M) aqueous solution into the mixture, carrying out hydrothermal reaction for 2-4 days at 150 ℃, then carrying out suction filtration and washing with deionized water, stirring the washed solid sample in 0.1-1 mol/L HCL for 2 hours, then carrying out suction filtration and washing with deionized water, and drying the obtained filter cake in a 110 ℃ oven for 6-24 hours. And grinding the dried sample, and then carrying out heat treatment at 300-800 ℃ for 4-8 hours to obtain the titanic acid nanotube carrier.
The concentration of NaOH is 10M/L;
the commercial product TiO2The content of (A) is as follows: 16-64 g/L;
step (2) CdS quantum dot preparation: mixing CdO, 1-octadecene and oleic acid, heating to 260-320 ℃ under the protection of inert gas, then adding tri-n-octylphosphine dissolved with sulfur powder, wherein the molar ratio of CdO to S is 1, and keeping the temperature at 220-320 ℃ for 3-10 minutes. And purifying and separating the cooled product by using normal hexane and acetone for multiple times. Adding mercaptopropionic acid into the purified sample, stirring for 6-24 hours, and then purifying and separating the product obtained after the reaction with the mercaptopropionic acid for multiple times by using water and acetone to obtain the water-soluble CdS quantum dots.
The concentration range of CdO after the CdO, the 1-octadecene and the oleic acid are mixed is 0.1-0.4M;
the concentration range of sulfur powder in the tri-n-octyl phosphorus is 1-8M;
step (3) preparation of the CdS quantum dot and Titanate Nanotube (TNT) composite catalyst:
and (3) mixing the titanic acid nanotube carrier obtained in the step (1) with the CdS quantum dots obtained in the step (2), performing ultrasonic treatment for 0.5-1 hour to fully disperse the titanic acid nanotube carrier, and then performing freeze drying on the ultrasonic treated sample to obtain the TNT/CdS composite catalyst.
The molar ratio of the titanic acid nanotube carrier to the CdS quantum dots is 1-11.
Step (4) TNT/CdS/TiO2Preparation of core-shell catalyst:
putting the TNT/CdS composite catalyst obtained in the step (3) into an atomic layer deposition vacuum chamber for TiO2Depositing an atomic layer to obtain TNT/CdS/TiO2A core-shell catalyst. Deposition of TiO using atomic layer deposition method (ALD)2In the preparation process, high-purity nitrogen or argon is used as a carrier, the flow rate of the carrier is kept to be more than 10sccm, the reaction temperature is more than 50 ℃, the reaction time is more than 1s, the cleaning time of the precursor is more than 3s, and TiO grows on the surface of the TNT/CdS composite catalyst2Circulating the step (4) for 10-80 times to grow TiO2And a protective layer.
The titanium source of the organic titanium comprises titanium tetrachloride, tetradimethylamino titanium or titanium isopropoxide;
step (5) TNT/CdS/TiO2Preparation of Pt core-shell structure catalyst:
TNT/CdS/TiO obtained in the step (4)2Placing the core-shell catalyst in an atomic layer deposition vacuum chamber for Pt atomic layer deposition to obtain TNT/CdS/TiO2Pt core-shell catalyst. When depositing Pt by using an Atomic Layer Deposition (ALD) method, organic Pt and ozone are used as precursors, and the pulse time of the precursorsAnd (3) taking high-purity nitrogen or argon as a carrier, keeping the flow of the carrier to be more than 10sccm, the reaction temperature to be more than 150 ℃ and less than 400 ℃, the reaction time to be more than 1s, and the precursor cleaning time to be more than 3s, and circulating the preparation process for 1-20 times to grow the Pt.
According to the invention, a titanic acid nanotube carrier is prepared by a hydrothermal method, CdS quantum dots are prepared by a thermal injection method, titanic acid nanotubes are compounded with the CdS quantum dots, and TiO is deposited by an ALD method2A shell layer, and then Pt is loaded on the core-shell catalyst, thereby obtaining TNT/CdS/TiO2Pt core-shell structure nanotube.
The nanotube prepared by the method can be used for lithium ion batteries, gas catalysis, hydrogen production by photocatalytic water decomposition, photocatalytic pollutant degradation or gas-sensitive sensing.
The invention has the beneficial effects that:
TNT/CdS/TiO2the Pt core-shell structure nanotube is a titanic acid nanotube (TNT)/CdS quantum dot/TiO in sequence from inside to outside2Shell/metal Pt. Core-shell structure design using TiO2Energy level matching with CdS promotes excited electrons to be converted into TiO from CdS2And the Schottky barrier formed by the supported Pt enables electrons to be separated from TiO2Transferring to Pt, thereby realizing the regulation and control of an electron transfer path. At the same time, TiO2The shell structure can effectively prevent the CdS from being corroded by light, and the titanic acid nano tube and the TiO are2The heterojunction formed by the shell layer is beneficial to the separation of photon-generated carriers at the interface, and TiO2The shell layer has small thickness, short electron transmission distance and less photon-generated carrier recombination, and the loaded Pt increases the active sites on the surface of the light reagent, thereby effectively improving the photocatalytic activity and stability of the material under the condition of visible light. Meanwhile, the material can also be used in lithium ion batteries, gas catalysis and gas-sensitive sensing, and the performance of the material is correspondingly improved.
Drawings
FIG. 1 shows the preparation of Titanate Nanotubes (TNT), CdS quantum dots and TNT/CdS/TiO prepared in example 12XRD diffraction pattern of Pt core shell structure nanotube.
FIG. 2 shows TNT/CdS/TiO prepared in example 12Pt nucleusTEM pictures of shell-structured nanotubes.
FIG. 3 shows TNT/CdS/TiO prepared in example 12HAADF-STEM diagram of Pt core-shell structure nanotube. Wherein the carrier is titanic acid nano-tube, and thin TiO can be seen at boundary2And the brighter small dots are loaded cadmium sulfide quantum dots and metal platinum.
FIG. 4 shows the preparation of the Titanate Nanotubes (TNT), TNT/CdS and TNT/CdS/TiO prepared in example 12The solid ultraviolet diffuse reflection spectrum of the Pt core-shell structure nanotube.
FIG. 5 shows the preparation of Titanate Nanotubes (TNT), CdS quantum dots, TNT/CdS and TNT/CdS/TiO in example 12The photocatalytic performance diagram of the Pt core-shell structure nanotube.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited to the following examples.
Example 1
(1) Preparation of Titanate Nanotubes (TNT): 2.5g of commercial TiO2Adding the mixture into 125ml of NaOH (10M) aqueous solution, stirring for 2 hours, pouring the mixture into a reaction kettle, reacting for 4 days in an oven at 150 ℃, washing with deionized water, adding the sample into 250ml of 0.1M HCL, stirring for 2 hours, performing suction filtration, washing with deionized water, and drying the obtained sample in the oven at 110 ℃ for 24 hours. The dried sample was further heat-treated at 600 ℃ for 4 hours to obtain a Titanate Nanotube (TNT).
(2) Preparing CdS quantum dots: 30ml of a mixed solution of 0.4M CdO, 1-octadecene and oleic acid was heated to 320 ℃ under the protection of an inert gas, and then 3ml of tri-n-octylphosphine (S concentration: 4M) in which sulfur powder was dissolved was added to maintain the temperature at 280 ℃ for 5 minutes. And dissolving the cooled product with n-hexane and methanol, precipitating with acetone, centrifuging at 5000r/min for 5min, and repeatedly purifying and separating for multiple times. And adding 1ml of mercaptopropionic acid into the purified sample, stirring for 6 hours, adding acetone, centrifuging for 5 minutes at 5000r/min, dissolving the sample with water, and repeatedly purifying and separating for multiple times to obtain the water-soluble CdS quantum dots.
(3) Preparing a CdS quantum dot and Titanate Nanotube (TNT) composite catalyst: and (3) mixing the sample obtained in the step (1) with the sample obtained in the step (2), performing ultrasonic treatment for 0.5 hour to fully disperse the sample, and then performing freeze drying on the sample to obtain the TNT/CdS composite catalyst.
(4)TNT/CdS/TiO2Preparation of core-shell catalyst: putting the sample obtained in the step (3) in an atomic layer deposition vacuum chamber for TiO2Atomic layer deposition, when the vacuum degree reaches the experimental requirement, introducing a precursor: titanium tetraisopropoxide and water, the pulse time of a precursor is 1s, in the preparation process, high-purity argon (99.999%) is used as a carrier gas, and the carrier gas flow is as follows: 50sccm, the reaction temperature is 150 ℃, the reaction time is 8s, the precursor cleaning time is 20s, and TiO grows on the surface of the TNT/CdS composite catalyst2The TiO is grown by circulating the preparation process for 80 times2Protecting the layer to obtain TNT/CdS/TiO2A core-shell catalyst.
(5)TNT/CdS/TiO2Preparation of Pt core-shell structure catalyst: putting the sample obtained in the step (4) in an atomic layer deposition vacuum chamber, and performing Pt atomic layer deposition to obtain TNT/CdS/TiO2Pt core-shell catalyst. When depositing Pt by using an atomic layer deposition method (ALD), trimethyl (methylcyclopentadienyl) platinum (IV) and ozone are used as precursors, the pulse time of the precursors is 1s, high-purity argon (99.999%) is used as a carrier gas in the preparation process, and the carrier gas flow rate is as follows: 10sccm, the reaction temperature is 280 ℃, the reaction time is 10s, the precursor cleaning time is 20s, the preparation process is circulated for 10 times to grow Pt, and the TNT/CdS/TiO is obtained2Pt core-shell structure nanotube.
Examples 2 to 5
Examples 2 to 5 were prepared in the same manner as in example 1 except that TiO was carried out in step (4)2The cycle number of the atomic layer deposition is changed from 80 to 10, 20, 40 and 60 respectively.
The test results of the materials obtained in the above examples are specifically described below.
(1) X-ray diffraction analysis (XRD)
FIG. 1 shows the preparation of Titanate Nanotubes (TNT), CdS quantum dots and TNT/CdS/TiO prepared in example 12XRD pattern of Pt core-shell structure nanotube. As can be seen from FIG. 1, TNT/CdS/TiO was prepared2The XRD of the Pt core-shell structure nanotube has characteristic peaks of TNT and CdS at the same time, and the successful compounding of the TNT and the CdS is proved.
(2) Perspective electron microscopy analysis (TEM)
FIG. 2 shows TNT/CdS/TiO prepared for example 12TEM picture of Pt core-shell structure nanotube.
(3) High angle annular dark field image (HAADF-STEM)
FIG. 3 shows TNT/CdS/TiO prepared in example 12HAADF-STEM diagram of Pt core-shell structure nanotube. Wherein the carrier is titanic acid nano-tube, and thin TiO can be seen at boundary2And the brighter small dots are loaded cadmium sulfide quantum dots and metal platinum.
(4) Solid UV diffuse reflectance analysis
FIG. 4 Titanic acid nanotubes (TNT), TNT/CdS and TNT/CdS/TiO prepared in example 12The solid ultraviolet diffuse reflection spectrum of the Pt core-shell structure nanotube. TNT/CdS/TiO can be obtained from the graph2The absorption of the Pt core-shell structure nanotube in a visible light range is widened and enhanced compared with that of a titanic acid nanotube (TNT) and TNT/CdS, and the photocatalytic performance of the composite material is favorably improved.
(5) Characterization of photocatalytic Properties
FIG. 5 shows the preparation of Titanate Nanotubes (TNT), CdS quantum dots, TNT/CdS and TNT/CdS/TiO in example 12The comparison graph of the photocatalytic hydrogen production performance of the Pt core-shell structure nanotube shows that the TNT/CdS/TiO of the invention2The photocatalytic performance of the Pt core-shell structure nanotube is obviously higher than that of a titanic acid nanotube (TNT), a CdS quantum dot and TNT/CdS.
Claims (4)
1. TNT/CdS/TiO2The Pt core-shell structure nanotube is characterized by sequentially comprising a titanic acid nanotube carrier/loaded CdS quantum dot/TiO from inside to outside2Shell/supported metal Pt; growing TiO through loaded CdS quantum dots by using titanic acid nanotube carrier as main body2The shell layer and the loaded metal Pt form a composite material; the diameter of the titanic acid nanotube carrier is 50-300 nanometers, the diameter of the CdS quantum dot is 4-6 nanometers, and the titanic acid nanotube carrier and TiO2The shell layer forming a heterojunction, TiO2The thickness of the shell layer is 1-8 nanometers, and the size of the metal Pt particles is 0.5-3 nanometers.
2. TNT/CdS/TiO according to claim 12The preparation method of the Pt core-shell structure nanotube is characterized by comprising the following steps:
step (1) preparation of a titanic acid nanotube carrier: TiO 2 of commercial products2Adding the mixture into NaOH aqueous solution, carrying out hydrothermal reaction for 2-4 days at 150 ℃, then carrying out suction filtration and washing with deionized water, stirring the washed solid sample in 0.1-1 mol/LHCL for 2 hours, then carrying out suction filtration and washing with deionized water, and drying the obtained filter cake in a 110 ℃ drying oven for 6-24 hours; grinding the dried sample, and then carrying out heat treatment at 300-800 ℃ for 4-8 hours to obtain a titanic acid nanotube carrier;
step (2) CdS quantum dot preparation: mixing CdO, 1-octadecene and oleic acid, heating to 260-320 ℃ under the protection of inert gas, then adding tri-n-octylphosphine dissolved with sulfur powder, wherein the molar ratio of CdO to S is 1, and keeping the temperature at 220-320 ℃ for 3-10 minutes; purifying and separating the cooled product by using normal hexane and acetone for multiple times; adding mercaptopropionic acid into the purified sample, stirring for 6-24 hours, and then purifying and separating a product obtained after the reaction with the mercaptopropionic acid for multiple times by using water and acetone to obtain water-soluble CdS quantum dots;
step (3) preparation of the CdS quantum dot and titanate nanotube composite catalyst:
mixing the titanic acid nanotube carrier obtained in the step (1) with the CdS quantum dots obtained in the step (2), performing ultrasonic treatment for 0.5-1 hour to fully disperse the titanic acid nanotube carrier, and then performing freeze drying on an ultrasonic sample to obtain a TNT/CdS composite catalyst;
step (4) TNT/CdS/TiO2Preparation of core-shell catalyst:
putting the TNT/CdS composite catalyst obtained in the step (3) into an atomic layer deposition vacuum chamber for TiO2Depositing an atomic layer to obtain TNT/CdS/TiO2A core-shell catalyst; deposition of TiO using atomic layer deposition methods2In the preparation process, organic titanium and water are used as precursors, the pulse time of the precursors is more than 5ms, and high-purity nitrogen is used in the preparation processGas or argon is used as a carrier, the flow of the carrier is kept to be more than 10sccm, the reaction temperature is more than 50 ℃ and less than 400 ℃, the reaction time is more than 1s, the precursor cleaning time is more than 3s, and TiO grows on the surface of the TNT/CdS composite catalyst2Circulating the step (4) for 10-80 times to grow TiO2A protective layer;
step (5) TNT/CdS/TiO2Preparation of Pt core-shell structure catalyst:
TNT/CdS/TiO obtained in the step (4)2Placing the core-shell catalyst in an atomic layer deposition vacuum chamber for Pt atomic layer deposition to obtain TNT/CdS/TiO2Pt core-shell catalyst; when the atomic layer deposition method is used for depositing Pt, organic Pt and ozone are used as precursors, the pulse time of the precursors is more than 5ms, high-purity nitrogen or argon is used as a carrier, the carrier flow is kept to be more than 10sccm, the reaction temperature is more than 150 ℃ and less than 400 ℃, the reaction time is more than 1s, the precursor cleaning time is more than 3s, and the preparation process is circulated for 1-20 times to grow Pt.
3. TNT/CdS/TiO according to claim 22The preparation method of the Pt core-shell structure nanotube is characterized by comprising the following steps:
the concentration of NaOH in the step (1) is 10 m/L;
the commercial TiO in the step (1)2The content of (A) is as follows: 16-64 g/L;
the CdO concentration range of the mixed CdO, 1-octadecene and oleic acid in the step (2) is 0.1-0.4M;
the concentration range of sulfur powder in the tri-n-octylphosphine obtained in the step (2) is 1-8M;
the molar ratio of the titanic acid nanotube carrier and the CdS quantum dots in the step (3) is 1-11;
the titanium source of the organic titanium in the step (4) comprises titanium tetrachloride, titanium tetradimethylamide or titanium isopropoxide.
4. TNT/CdS/TiO according to claim 12The Pt core-shell structure nanotube can be used in lithium ion batteries, hydrogen production by photocatalytic water decomposition, pollutant photocatalytic degradation or gas-sensitive sensing。
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