CN103920512A - Preparation method of noble-metal-modified fluorine-boron-codoped TiO2 nano-particle - Google Patents

Preparation method of noble-metal-modified fluorine-boron-codoped TiO2 nano-particle Download PDF

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CN103920512A
CN103920512A CN201410148268.XA CN201410148268A CN103920512A CN 103920512 A CN103920512 A CN 103920512A CN 201410148268 A CN201410148268 A CN 201410148268A CN 103920512 A CN103920512 A CN 103920512A
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tio
fluorine boron
boron codope
preparation
nanometer sheet
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许海峰
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Suzhou University
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Abstract

The invention discloses a preparation method of a noble-metal-modified fluorine-boron-codoped TiO2 nano-particle. The preparation method has the advantages that the photocatalytic activity of the noble-metal-modified fluorine-boron-codoped TiO2 nano-particle is high; by loading the noble metal atoms, the separation efficiency of an electron hole pair can be improved, the combination of the electron hole pair can be restrained, a catalytic effect is improved, the surface hydrophobicity can be further improved, and adhered degradation products are easy to clean.

Description

A kind of noble metal decorated fluorine boron codope TiO 2the preparation of nano particle
Technical field
The present invention relates generally to nano material and field of nanometer technology, relates in particular to a kind of noble metal decorated fluorine boron codope TiO 2the preparation of nano particle.
Background technology
Nano titanium oxide, owing to having good photocatalysis performance, has broad application prospects at aspects such as antibacterial and deodouring, sewage disposal, air cleanings, TiO 2being N-type semiconductor metal oxide, having the advantages such as oxidation activity is good, stability is strong, nontoxic in allied substances, is the friendly shaped material of a kind of green environment.Prepare and have higher catalytic activity and can be by the nano titanium dioxide photocatalyst of excited by visible light, be forward position and the important directions of photocatalysis research always; Synthetic and the repercussion study of novel nano photocatalysis material of titanium dioxide; development along with global process of industrialization; problem of environmental pollution is day by day serious; environmental protection and sustainable development become the matter of utmost importance that the mankind must consider, photocatalysis technology is the emerging research field having grown up since nearly 30 years as a representative of Green Chemistry.
Large quantity research shows, various poisonous and hazardous pollutants in water and air, and the various alkane that discharge in Chemical Manufacture, fragrant hydrocarbons and their derivates, halides, polycyclic aromatic hydrocarbon and heterocyclic compound etc. greatly can be by photocatalytic degradations.Poisonous, harmful, the difficult organic research of decomposing in industrial wastewater that is used for degrading of the application of pure pollution-free and inexhaustible luminous energy and photochemical catalyst that environmental protection combines and consersion unit is had to far-reaching strategic importance, and conductor photocatalysis material also becomes the emphasis of scientists study.
Summary of the invention
The object of the invention is just to provide the fluorine boron codope TiO that a kind of Pt modifies 2the preparation of nano particle.
The present invention is achieved by the following technical solutions:
A kind of noble metal decorated fluorine boron codope TiO 2the preparation of nano particle, comprises the following steps:
(1) preparation of basic nanometer sheet:
Fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) noble metal decorated fluorine boron codope TiO 2the preparation of nano particle:
The fluorine boron codope TiO of A, Pt metal-modified 2the preparation of nano particle:
Get a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet, ultrasonic being scattered in 300mL ultra-pure water, then adds a certain amount of Platinous Potassium Chloride, makes TiO 2mass ratio 100:1～5 of nanometer sheet and Platinous Potassium Chloride, stir the lower 120w of use low pressure mercury lamp, apart from liquid level 30cm, illumination 4h, after centrifugation, with distilled water flushing, then, the baking oven inner drying of 60～80 ℃ 4～6 hours, obtain the fluorine boron codope TiO that described Pt modifies 2nano particle;
The fluorine boron codope TiO that B, Ag modify 2the preparation of nano particle:
The ethanol that measures 30ml adds to be poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, measures a certain amount of silver nitrate, uses magnetic stirrer 20 minutes, measures a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet, makes fluorine boron codope, (001) crystal face expose TiO 2mass ratio 100:1～5 of nanometer sheet and silver nitrate, continue to stir 15 minutes, and then 200 ℃ of constant temperature is 18 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 3～5 times 80 ℃ of freeze-day with constant temperature 10 hours; After the product centrifugation obtaining washing are dry, obtain the fluorine boron codope TiO that Ag modifies 2nano particle.
Advantage of the present invention is:
The fluorine boron codope TiO that Pt of the present invention modifies 2the photocatalytic activity of nano particle is high, due to load precious metal atom, its fermi level is significantly lower than semiconductor, therefore very easily enrichment on these metallics of light induced electron, hole is retained in semiconductor, metal nanoparticle can provide activated centre for surface light catalytic reaction as co-catalyst simultaneously, and separative efficiency and the inhibition electron hole pair that can improve electron hole pair are compound, strengthen catalytic effect.
Accompanying drawing explanation
Fig. 1 is that fluorine boron codope of the present invention, (001) crystal face expose TiO 2the fluorine boron codope TiO that nano material and Pt modify 2the XRD collection of illustrative plates of nano material;
Fig. 2 is the fluorine boron codope TiO that Pt of the present invention modifies 2the SEM figure of nano material;
Fig. 3 is the fluorine boron codope TiO that Pt of the present invention modifies 2the TEM figure of nano material;
Fig. 4 is the fluorine boron codope TiO that Pt of the present invention modifies 2the XPS spectrum figure of nano material, abscissa is that ordinate is relative intensity in conjunction with energy;
Fig. 5 is that fluorine boron codope of the present invention, (001) crystal face expose TiO 2the fluorine boron codope TiO that nano material and Pt modify 2nano material is the degradation effect comparison diagram to methyl orange under visible ray;
Fig. 6 is that fluorine boron codope of the present invention, (001) crystal face expose TiO 2the fluorine boron codope TiO that nano material and Ag modify 2the XRD collection of illustrative plates of nano material;
Fig. 7 is the fluorine boron codope TiO that Ag of the present invention modifies 2the SEM figure of nano material;
Fig. 8 is the fluorine boron codope TiO that Ag of the present invention modifies 2the TEM figure of nano material;
Fig. 9 is the fluorine boron codope TiO that Ag of the present invention modifies 2the XPS spectrum figure of nano material, abscissa is that ordinate is relative intensity in conjunction with energy;
Figure 10 is that fluorine boron codope of the present invention, (001) crystal face expose TiO 2the fluorine boron codope TiO that nano material and Ag modify 2nano material is the degradation effect comparison diagram to methyl orange under visible ray.
The specific embodiment
Embodiment 1
(1) fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) the fluorine boron codope TiO that Pt modifies 2the preparation of nano particle:
Get the above-mentioned fluorine boron codope of 0.3g, (001) crystal face exposure TiO 2nanometer sheet, ultrasonic being scattered in 300mL ultra-pure water, then add a certain amount of Platinous Potassium Chloride 0.01g, stir the lower 120w of use low pressure mercury lamp, apart from liquid level 30cm, illumination 4h, uses distilled water flushing after centrifugation, then the baking oven inner drying of 80 ℃ 4 hours, obtain the support type fluorine boron codope TiO containing Pt 2nano particle.
Embodiment 2
(1) fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) the fluorine boron codope TiO that Pt modifies 2the preparation of nano particle:
Get the above-mentioned fluorine boron codope of 0.2g, (001) crystal face exposure TiO 2nanometer sheet, ultrasonic being scattered in 300mL ultra-pure water, then adds a certain amount of Platinous Potassium Chloride 0.007g, under stirring, under 120w low pressure mercury lamp, carry out illumination 4h, after centrifugation, with distilled water flushing, then, the baking oven inner drying of 80 ℃ 4 hours, obtain the support type fluorine boron codope TiO containing Pt 2nano particle.
Embodiment 3
(1) fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) the fluorine boron codope TiO that Pt modifies 2the preparation of nano particle:
Get the above-mentioned fluorine boron codope of 0.2g, (001) crystal face exposure TiO 2nanometer sheet, ultrasonic being scattered in 300mL ultra-pure water, then add a certain amount of Platinous Potassium Chloride 0.005g, stir the lower 120w of use low pressure mercury lamp, apart from liquid level 30cm, illumination 4h, uses distilled water flushing after centrifugation, then the baking oven inner drying of 75 ℃ 4 hours, obtain the support type fluorine boron codope TiO containing Pt 2nano particle.
Embodiment 4
(1) fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) the fluorine boron codope TiO that Ag modifies 2the preparation of nano particle:
The ethanol that measures 30ml adds to be poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, measures silver nitrate 0.004g, uses magnetic stirrer 20 minutes, measures a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet 0.2g, continue to stir 15 minutes, and then 200 ℃ of constant temperature is 18 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 3 times 80 ℃ of freeze-day with constant temperature 10 hours; After the product centrifugation obtaining washing are dry, obtain the fluorine boron codope TiO that Ag modifies 2nano-particle complex.
Embodiment 5
(1) fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) the fluorine boron codope TiO that Ag modifies 2the preparation of nano particle:
The ethanol that measures 30ml adds to be poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, measures silver nitrate 0.005g, uses magnetic stirrer 20 minutes, measures a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet 0.18g, continue to stir 15 minutes, and then 200 ℃ of constant temperature is 18 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 3～5 times 80 ℃ of freeze-day with constant temperature 10 hours; After the product centrifugation obtaining washing are dry, obtain the fluorine boron codope TiO that Ag modifies 2nano-particle complex.
Embodiment 6
(1) fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) the fluorine boron codope TiO that Ag modifies 2the preparation of nano particle:
The ethanol that measures 30ml adds to be poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, measures silver nitrate 0.005g, uses magnetic stirrer 20 minutes, measures a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet 0.25g, continue to stir 15 minutes, and then 200 ℃ of constant temperature is 18 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 3～5 times 80 ℃ of freeze-day with constant temperature 10 hours; After the product centrifugation obtaining washing are dry, obtain the fluorine boron codope TiO that Ag modifies 2nano-particle complex.
Comparative example
Fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet.
Experiment material and method
By contrasting respectively the TiO of fluorine boron codope, the exposure of (001) crystal face 2the fluorine boron codope TiO that nanometer sheet and Pt, Ag modify 2nano particle studies to the degradation rate of Methyl Orange in Wastewater the fluorine boron codope TiO that Pt modifies 2nano particle is to TiO 2the impact of photocatalysis performance.
Reaction is used 350W high-pressure sodium lamp as light source, apart from liquid level 10cm, 0.04g photocatalysis sample is put into the methyl orange solution that 50ml concentration is 15mg/L, mixed liquor constantly stirs, every 20min, get 3ml solution, with 5000 revs/min of centrifuges, remove the catalyst in solution, clear liquid judges its residual concentration by ultraviolet-visual spectrometer test absorption maximum light rate.
Experimental result
Experimental result, as shown in Fig. 5,10, can be found out, the TiO exposing than fluorine boron codope, (001) crystal face 2nanometer sheet, the fluorine boron codope TiO that Pt, Ag modify 2nano particle significantly promotes for the degradation capability of methyl orange, confirms that it has good Photocatalytic Degradation Property.

Claims (1)

1. a noble metal decorated fluorine boron codope TiO 2the preparation of nano particle, is characterized in that comprising the following steps:
(1) preparation of basic nanometer sheet:
Fluorine boron codope, (001) crystal face expose TiO 2nanometer sheet preparation:
The ethanolic solution that measures volume and be 30ml is precursor liquid, slowly adds the 15wt%TiCl of 1ml 3solution, generates uniform suspension for 5 minutes by magnetic stirrer; The solution preparing in above-mentioned steps is poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, then dripped the 40wt%HBF of 0.5ml 4solution in reactor inner bag, 210 ℃ of constant temperature 12 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 4 times 80 ℃ of freeze-day with constant temperature 10 hours; The product obtaining is through 450 ℃ of subsequent heat treatment after 3 hours, and grind into powder, obtains having fluorine boron codope, (001) crystal face that crystallization degree is higher simultaneously and expose TiO 2nanometer sheet;
(2) noble metal decorated fluorine boron codope TiO 2the preparation of nano particle:
The fluorine boron codope TiO that A, Pt modify 2the preparation of nano particle:
Get a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet, ultrasonic being scattered in 300mL ultra-pure water, then adds a certain amount of Platinous Potassium Chloride, makes TiO 2mass ratio 100:1～5 of nanometer sheet and Platinous Potassium Chloride, stir the lower 120w of use low pressure mercury lamp, apart from liquid level 30cm, illumination 4h, after centrifugation, with distilled water flushing, then at the baking oven inner drying 4-6 hour of 60～80 ℃, obtain the fluorine boron codope TiO that described Pt modifies 2nano particle;
The fluorine boron codope TiO that B, Ag modify 2the preparation of nano particle:
The ethanol that measures 30ml adds to be poured in the polytetrafluoroethylene (PTFE) autoclave inner bag that volume is 50ml, measures a certain amount of silver nitrate, uses magnetic stirrer 20 minutes, measures a certain amount of above-mentioned fluorine boron codope, (001) crystal face exposure TiO 2nanometer sheet, makes fluorine boron codope, (001) crystal face expose TiO 2mass ratio 100:1～5 of nanometer sheet and silver nitrate, continue to stir 15 minutes, and then 200 ℃ of constant temperature is 18 hours; The solidliquid mixture obtaining carries out solid-liquid centrifugation, with ethanol washing 3～5 times 80 ℃ of freeze-day with constant temperature 10 hours; After the product centrifugation obtaining washing are dry, obtain the fluorine boron codope TiO that Ag modifies 2nano particle.
CN201410148268.XA 2014-04-14 2014-04-14 Preparation method of noble-metal-modified fluorine-boron-codoped TiO2 nano-particle Pending CN103920512A (en)

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CN105772039A (en) * 2016-05-10 2016-07-20 宿州学院 Fluorine and boron co-doped TiO2 nano-plate with crystal planes (001) and oxygen vacancy, method for preparing fluorine and boron co-doped TiO2 nano-plate and application thereof
CN105817238A (en) * 2016-03-22 2016-08-03 宿州学院 Preparation method of (001) crystal face and fluorine boron codoped TiO2 nanosheet modified by precious metal and provided with oxygen vacancy

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CN105817238A (en) * 2016-03-22 2016-08-03 宿州学院 Preparation method of (001) crystal face and fluorine boron codoped TiO2 nanosheet modified by precious metal and provided with oxygen vacancy
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CN105772039B (en) * 2016-05-10 2018-08-21 宿州学院 A kind of (001) crystal face fluorine boron codope TiO with Lacking oxygen2The Preparation method and use of nanometer sheet

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Application publication date: 20140716