CN102671651A - Method for preparing mesoporous beta-Ga2O3 nanorod photocatalyst by using PEG (polyethylene glycol) as template - Google Patents

Method for preparing mesoporous beta-Ga2O3 nanorod photocatalyst by using PEG (polyethylene glycol) as template Download PDF

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CN102671651A
CN102671651A CN2012101919423A CN201210191942A CN102671651A CN 102671651 A CN102671651 A CN 102671651A CN 2012101919423 A CN2012101919423 A CN 2012101919423A CN 201210191942 A CN201210191942 A CN 201210191942A CN 102671651 A CN102671651 A CN 102671651A
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peg
catalyst
ga2o3
template
beta
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赵伟荣
张静
王琰
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Zhejiang University ZJU
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Abstract

The invention belongs to the technical field of photocatalyst materials and preparation thereof, and aims to provide a method for preparing a mesoporous beta-Ga2O3 nanorod photocatalyst by using PEG (polyethylene glycol) as a template. According to the method, gallium-containing compounds and alkaline matters are used as raw materials, the PEG is used as the template, and a hydrothermal synthesis method is adopted to prepare the mesoporous beta-Ga2O3 nanorod photocatalyst. The invention can effectively control the crystal growth, improve the crystal form structure of the catalyst, increase the specific area of the catalyst, generate abundant oxygen vacancies or gallium-oxygen vacancy pairs, and enhance the photoresponse intensity of the catalyst, thereby enhancing the photocatalytic efficiency of the catalyst. The experiment of decomposing methylbenzene by photocatalytic oxidation indicates that the photocatalytic efficiency of the PEG-modified beta-Ga2O3 is 1.2-10 times of that of the beta-Ga2O3 which is not modified by the PEG. The method has the advantages of simple technique and adjustable parameters, and is easy to operate; and the prepared beta-Ga2O3 nanorod photocatalyst is a monoclinic system with complete and regular crystal form, belongs to a mesoporous material, and has the advantages of high photoresponse capacity and high catalytic performance.

Description

Prepare mesoporous beta-Ga with PEG as template 2O 3The method of nano-rod photo-catalyst
Technical field
The present invention relates to a kind ofly prepare mesoporous beta-Ga as template with PEG 2O 3The method of nano-rod photo-catalyst belongs to catalysis material and preparing technical field thereof.
Background technology
Ga 2O 3Be a kind of transparent broad stopband metal oxide semiconductor material, have excellent chemical stability, heat endurance, electric conductivity, the characteristics of luminescence, optical energy gap is between 4.2 ~ 4.9eV under the room temperature.The Ga that reports at present 2O 3Have α-, β-, γ-, δ-and ε-Ga 2O 3Deng 5 kinds of different forms.At room temperature, to have the β-Ga of monocline 2O 3The most stable, aspect opto-electronic device, have broad application prospects, can be widely used in Ga and semi-conductive insulating barrier, ultra-violet light-emitting material and gas sensor etc., in addition, β-Ga 2O 3As a kind of catalysis material efficiently, representing superior performance and huge application potential aspect the VOC such as purifying benzene thing.
Prepare β-Ga at present 2O 3Method a lot, mainly contain chemical deposition, sol-gel process, molecular beam epitaxy, pulsed laser deposition, carbothermic method, metal-organic chemical deposition and hydro-thermal method etc.Need high-temperature operation in the said method, to equipment and preparation technology's requirement than higher, preparation and maintenance cost costliness.Hydro-thermal method is as a kind of simple low temperature wet method, and reaction is in autoclave, to carry out, easy control simple to operate, and the equipment precision requirement is not high, at the powder β-Ga of preparation stable homogeneous 2O 3There is special advantages the aspect.Patent publication No. is: CN101993110A, patent is by name: a kind of microwave method prepares β-Ga 2O 3Method, announced that a kind of reaction of carrying out microwave hydrothermal with the micro-wave digestion stove forms the cotton-shaped β-Ga of white crystals 2O 3Method, this method device structure is simple, technological principle is reliable, preparation time is short, efficient is high, operation is prone to row; But the β-Ga of preparation 2O 3Crystallite dimension is big, irregular structure, and specific area is little, has had a strong impact on β-Ga 2O 3Photocatalysis performance and application.
In the process of Preparation of Catalyst, adding template pore-creating is to increase specific surface area of catalyst, improves catalyst microstructure, one of method that the photocatalysis performance of raising catalyst is the most frequently used.PEG is a kind of comparatively cheap surfactant, is widely used in the preparation of metal oxide nano rod and photocatalytic semiconductor material as template.At Hydrothermal Preparation β-Ga 2O 3In the system, the PEG molecule in the solution is adsorbed in the GaOOH nano particle through hydrogen bond, and it is covered, and impels the grain orientation growth that is protected, and forms the pattern of stable homogeneous.And because the PEG molecule self has linear structure and more hydroxyl activity point position, can attract contiguous nanometer rods polymerization through the bridge linking effect between the hydroxyl, final formation has larger-diameter prismatic crystal structure.The PEG molecule and the hydroxyl evaporation that in calcination process, act on material surface produce loose structure; Increased the specific area of catalyst effectively; And abundant oxygen room and gallium-oxygen double-void have been produced; Suppress electronics-hole-recombination effectively, improved the photoinduction intensity and the photocatalysis efficiency of catalyst.The present invention first with PEG as the high mesoporous beta-Ga of template Hydrothermal Preparation stable homogeneous photocatalysis performance 2O 3Nano-rod photo-catalyst.
Summary of the invention
The technical problem that the present invention will solve is, overcomes the shortcoming that prior art exists, and providing a kind of is that template prepares β-Ga that specific area is big, crystal structure is complete, photocatalysis performance is high with PEG 2O 3The new method of photochemical catalyst.
For solving the problems of the technologies described above, solution of the present invention is: prepare mesoporous beta-Ga with PEG as template 2O 3The method of nano-rod photo-catalyst is characterized in that, with contain gallium compound, alkaline matter is a raw material, as template, adopts hydrothermal synthesis method to prepare mesoporous beta-Ga with PEG 2O 3Nano-rod photo-catalyst, it is following that it specifically prepares process:
(1) will contain gallium compound, alkaline matter, PEG, deionized water and mix, stir 1 ~ 4 hour under the room temperature, 100 ~ 300 ℃ of hydrothermal treatment consists 6 ~ 24 hours to dissolving fully;
(2) cooling back suction filtration separates, and spends deionised water earlier 3 ~ 5 times, uses absolute ethanol washing again 3 ~ 5 times, 100 ~ 200 ℃ of dryings 1 ~ 4 hour, grinds and obtains white powder GaOOH;
(3) above-mentioned GaOOH is shifted as in the Muffle furnace,, promptly obtain the mesoporous beta-Ga of stable homogeneous 500 ~ 1000 ℃ of calcinings 1 ~ 6 hour 2O 3Nano-rod photo-catalyst;
Contain in the mixed solution that gallium compound, alkaline matter, PEG, deionized water form in that step (1) is described, the mol ratio of each component is Ga 3+: OH -: PEG: H 2O=1: (10 ~ 30): (0.85 ~ 25.56): (442 ~ 884).
Among the present invention, the described gallium compound that contains is gallium chloride, gallium nitrate or gallium sulfate (being the commercial goods); Described alkaline matter is NaOH, potassium hydroxide or urea.
Among the present invention, the mean molecule quantity of described template PEG is 200 ~ 6000, and density is 1.127g/L.
Among the present invention, the compactedness when carrying out hydrothermal treatment consists (filling the ratio that liquor capacity accounts for autoclave liner volume) is 40 ~ 90%.
Among the present invention, β-Ga that preparation is obtained 2O 3Nano-rod photo-catalyst is monoclinic system (JCPDS:41-1103), and diameter is 200 ~ 300nm, and length is 1.00 ~ 1.20 μ m, and specific area is 7.79 ~ 29.00 m 2/ g, pore-size distribution belong to mesoporous material at 10 ~ 50nm.
With respect to prior art, the invention has the advantages that:
(1) simple, the wide material sources of raw material of the present invention, preparation technology is easy, and condition is prone to control, and technological parameter is adjustable, and energy consumption, cost are low, can realize a large amount of preparations in the short time.
(2) the present invention with PEG as template; Can effectively reduce crystallite dimension, increase the specific area of catalyst, and produce abundant oxygen room or gallium-oxygen double-void; Thereby the recombination rate that has suppressed photo-generated carrier has strengthened the photoresponse intensity and the photocatalysis efficiency of catalyst.
(3) photochemical catalyst of the present invention's preparation has good degradation to VOC such as toluene; Aspect purifying the air of a room, good prospects for application is arranged; And very big application potential is also arranged in opto-electronic device, sensor device, promoted the practicability of photocatalysis technology.
Description of drawings
Fig. 1 is mesoporous beta-Ga of the present invention 2O 3Preparation method's sketch map of nano-rod photo-catalyst.
Fig. 2 be embodiment 1 catalyst with and the XRD figure of presoma GaOOH.
Fig. 3 is the BET figure of the catalyst of embodiment 1.
Fig. 4 is the BJH figure of the catalyst of embodiment 1.
Fig. 5 is the TEM figure of the catalyst of embodiment 2.
Fig. 6 is the SEM figure of the catalyst of embodiment 2.
Fig. 7 is the PL figure of the catalyst of embodiment 2 ~ 4.
Fig. 8 is the PLE figure of the catalyst of embodiment 2 ~ 4.
Fig. 9 is the catalyst degradation toluene result of experiment of embodiment 1 ~ 4.
The specific embodiment
Come further explain of the present invention below in conjunction with accompanying drawing and embodiment, wherein the part preparation condition only is the explanation as typical case, is not to be to qualification of the present invention.
Embodiment 1:
(1) takes by weighing the autoclave that 1.6g gallium nitrate, 1.7g NaOH are put into 100mL, add the PEG200 of 5mL and the deionized water of 35mL again, stir 1 hour under the room temperature, 100 ℃ of hydro-thermal reactions 6 hours to dissolving fully.
(2) cooling back suction filtration separates, and spends deionised water earlier 3 times, uses absolute ethanol washing again 4 times, 100 ℃ of dryings 1 hour, grinds and obtains white powder GaOOH.
(3) above-mentioned GaOOH is transferred in the Muffle furnace, calcined 1 hour for 500 ℃, promptly obtain the mesoporous beta-Ga of stable homogeneous 2O 3Nano-rod photo-catalyst.
Characterize through XRD, gained presoma GaOOH is orthorhombic system (JCPDS:06-0180) after the hydro-thermal, calcining back gained β-Ga 2O 3For monoclinic system (JCPDS:41-1103), see Fig. 2.Characterize prepared β-Ga through BET 2O 3Average pore size be 17.30nm, belong to mesoporous material, see Fig. 3; Specific area is 7.79m 2/ g sees Fig. 4; Average diameter is 300nm, and distribution of lengths is at 1.00 ~ 1.20 μ m.
Embodiment 2:
(1) takes by weighing the autoclave that 1.6g gallium nitrate, 2.64g urea are put into 100mL, add PEG200 and the 45mL deionized water of 20mL again, stir 2 hours under the room temperature, 140 ℃ of hydro-thermal reactions 6 hours to dissolving fully.
(2) cooling back suction filtration separates, and spends deionised water earlier 4 times, uses absolute ethanol washing again 5 times, 200 ℃ of dryings 2 hours, grinds and obtains white powder GaOOH.
(3) above-mentioned GaOOH is shifted as in the Muffle furnace, calcined 2 hours for 800 ℃, promptly obtain the mesoporous beta-Ga of stable homogeneous 2O 3Nano-rod photo-catalyst.
Characterize prepared β-Ga through TEM and SEM 2O 3Be club shaped structure, average diameter is 200nm, and distribution of lengths is at 1.00 ~ 1.05 μ m, and there is the aperture of many Nano grades in catalyst surface, sees Fig. 5 and Fig. 6; Prepared β-Ga 2O 3The specific area of nanometer rods is 29.00m 2/ g, average pore size is 10 nm, belongs to mesoporous material.
Embodiment 3:
(1) takes by weighing the autoclave that 0.71g gallium chloride, 2.64g urea are put into 100mL, add PEG1000 and the 45mL deionized water of 20mL again, stir 3 hours under the room temperature, 200 ℃ of hydro-thermal reactions 12 hours to dissolving fully.
(2) cooling back suction filtration separates, and spends deionised water earlier 5 times, uses absolute ethanol washing again 3 times, 150 ℃ of dryings 3 hours, grinds and obtains white powder GaOOH.
(3) above-mentioned GaOOH is shifted as in the Muffle furnace,, can obtain the mesoporous beta-Ga of stable homogeneous 800 ℃ of calcinings 5 hours 2O 3Nanometer rods.
Prepared β-Ga 2O 3The specific area of nanometer rods is 20.62 m 2/ g, distribution of lengths is at 1.00 ~ 1.10 μ m, and average diameter is 260nm, and average pore size is 50nm, belongs to mesoporous material.
Embodiment 4:
(1) takes by weighing the autoclave that 1.88g gallium sulfate, 7.41g potassium hydroxide are put into 100mL, add PEG6000 and the 70mL deionized water of 20mL again, stir 4 hours under the room temperature, 300 ℃ of hydro-thermal reactions 24 hours to dissolving fully.
(2) cooling back suction filtration separates, and spends deionised water earlier 4 times, uses absolute ethanol washing again 5 times, 200 ℃ of dryings 4 hours, grinds and obtains white powder GaOOH.
(3) above-mentioned GaOOH is shifted as in the Muffle furnace, calcined 6 hours for 1000 ℃, can obtain the mesoporous beta-Ga of stable homogeneous 2O 3Nanometer rods.
Prepared β-Ga 2O 3The specific area of nanometer rods is 25.40 m 2/ g, distribution of lengths is at 1.00 ~ 1.10 μ m, and average diameter is 220nm, and average pore size is 35nm, belongs to mesoporous material.
Characterize through PL, embodiment 2 ~ 4 prepared catalyst all have tangible PL signal, and the PL peak intensity all is higher than the sample of modifying without PEG, show the β-Ga that modifies through PEG 2O 3Produced abundant oxygen room or gallium-oxygen double-void, improved the separating effect in electronics and hole effectively, the β-Ga that wherein modifies through PEG200 2O 3The PL peak the strongest, the photoinduction effect is best, sees Fig. 7.PLE collection of illustrative plates by the prepared catalyst of embodiment 2 ~ 4 can know that the adding of PEG has obviously improved β-Ga in the reaction system 2O 3Optical property, tangible blue shift has taken place in the position at PL peak, shows that the adding of PEG in the system can enlarge β-Ga 2O 3Energy gap, significantly improve the photoresponse intensity of catalyst, the β-Ga that wherein modifies through PEG200 2O 3The PLE peak is the strongest, and the photoinduction effect is best, sees Fig. 8.
Sample to embodiment 1 ~ 4 carries out the photocatalytic activity test
The cylindrical reactor of being processed by quartz glass is adopted in experiment, diameter 12.6cm, and high 13cm, volume are 1.2L, and lid is to be done by quartz material to process, and adopts the ground sealing with reactor, and contact-making surface is coated with one deck vacuum grease, with anti-gas-leak.As target contaminant, the uviol lamp of 254nm that with power is 8W is as light source with toluene.Adopt four embodiment of the present invention to carry out photocatalytic degradation toluene test, and and β-Ga of modifying without PEG 2O 3Make comparisons.Take by weighing the 0.05g catalyst and place on the glass surface ware of 12.5mm, drip a small amount of absolute ethyl alcohol, evenly be coated with completely whole surface, remove ethanol 80 ℃ of oven dry, cooling is placed on reactor, sealing.Extract a certain amount of toluene saturated gas (reagent bottle that fills toluene is done 40 ℃ of waters bath with thermostatic control processing) with 100 μ L injectors; Squeeze into reactor through injection port, leave standstill 30min, make that the absorption-desorption of toluene reaches balance in the system; Open uviol lamp then, carry out the photocatalytic degradation experiment.Every separated 10min sampling detects with GC, thereby confirms the concentration of toluene.
Fig. 9 has provided in 60min, the degrade efficiency chart of toluene of five kinds of catalyst, can find out the β-Ga that modifies through PEG 2O 3Photocatalysis performance all improve, be the β-Ga that modifies without PEG approximately 2O 31.2 ~ 10 times.Prepared β-the Ga of embodiment 2 wherein 2O 3Photocatalysis efficiency the highest, basic degraded is fully in 30min.
Although the present invention is described in each specific embodiment; But those skilled in the art will readily understand that the present invention is not limited to foregoing description; It can be changed or improve by multiple other modes, and does not break away from spirit and the scope of illustrating in the claim of the present invention.Everyly belong to the row that conspicuous variation that technical scheme of the present invention amplifies out or change still are in protection scope of the present invention.

Claims (5)

1. prepare mesoporous beta-Ga with PEG as template 2O 3The method of nano-rod photo-catalyst is characterized in that, be with contain gallium compound, alkaline matter is a raw material, as template, adopts hydrothermal synthesis method to prepare mesoporous beta-Ga with PEG 2O 3Nano-rod photo-catalyst, it is following that it specifically prepares process:
(1) will contain gallium compound, alkaline matter, PEG, deionized water and mix, stir 1 ~ 4 hour under the room temperature, 100 ~ 300 ℃ of hydrothermal treatment consists 6 ~ 24 hours to dissolving fully;
(2) cooling back suction filtration separates, and spends deionised water earlier 3 ~ 5 times, uses absolute ethanol washing again 3 ~ 5 times, 100 ~ 200 ℃ of dryings 1 ~ 4 hour, grinds and obtains white powder GaOOH;
(3) above-mentioned GaOOH is shifted as in the Muffle furnace,, promptly obtain the mesoporous beta-Ga of stable homogeneous 500 ~ 1000 ℃ of calcinings 1 ~ 6 hour 2O 3Nano-rod photo-catalyst;
Contain in the mixed solution that gallium compound, alkaline matter, PEG, deionized water form in that step (1) is described, the mol ratio of each component is Ga 3+: OH -: PEG: H 2O=1: (10 ~ 30): (0.85 ~ 25.56): (442 ~ 884).
2. method according to claim 1 is characterized in that, the described gallium compound that contains is gallium chloride, gallium nitrate or gallium sulfate; Described alkaline matter is NaOH, potassium hydroxide or urea.
3. method according to claim 1 is characterized in that, the mean molecule quantity of described template PEG is 200 ~ 6000, and density is 1.127g/L.
4. method according to claim 1 is characterized in that, the compactedness when carrying out hydrothermal treatment consists, and promptly filling the ratio that liquor capacity accounts for autoclave liner volume is 40 ~ 90%.
5. method according to claim 1 is characterized in that, β-Ga that preparation is obtained 2O 3Nano-rod photo-catalyst is monoclinic system (JCPDS:41-1103), and diameter is 200 ~ 300nm, and length is 1.00 ~ 1.20 μ m, and specific area is 7.79 ~ 29.00 m 2/ g, pore-size distribution belong to mesoporous material at 10 ~ 50nm.
CN2012101919423A 2012-06-07 2012-06-07 Method for preparing mesoporous beta-Ga2O3 nanorod photocatalyst by using PEG (polyethylene glycol) as template Pending CN102671651A (en)

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CN102974379A (en) * 2012-11-05 2013-03-20 南京大学 Method for preparing nitrogen-doped photo-catalytic material containing gallium oxide at low temperature
CN106076373A (en) * 2016-06-20 2016-11-09 广西大学 A kind of Ag/AgBr/Ga2o3heterojunction structure catalysis material and preparation method thereof
CN106517109A (en) * 2016-10-21 2017-03-22 南开大学 A preparing method of gallium nitride nanorods
CN107180882A (en) * 2017-05-23 2017-09-19 哈尔滨工业大学 A kind of preparation method of beta-oxidation gallium nano-array
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CN109796040A (en) * 2019-03-26 2019-05-24 湖南科技大学 A kind of GaOOH, Zn2+The preparation method of monodimension nanometer material
CN110935445A (en) * 2019-11-11 2020-03-31 中国科学院金属研究所 PdGa for selective hydrogenation of acetyleneX/Ga2O3Preparation method and application of catalyst
CN113816417A (en) * 2021-10-20 2021-12-21 西北大学 Black gallium oxide nano-particles and preparation method thereof
CN114086238A (en) * 2021-11-03 2022-02-25 吉林大学 Gamma-Ga2O3Or Cu doped gamma-Ga2O3Nanocrystalline and preparation method and application thereof
CN114408970A (en) * 2022-01-25 2022-04-29 重庆邮电大学 Preparation method of hollow mesoporous carbon-doped gallium sesquioxide nanospheres and product thereof
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WEIRONG ZHAO ET AL.: "Synthesis of mesoporous β-Ga2O3 nanorods using PEG as template: Preparation, characterization and photocatalytic properties", 《JOURNAL OF HAZARDOUS MATERIALS》 *

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CN106076373A (en) * 2016-06-20 2016-11-09 广西大学 A kind of Ag/AgBr/Ga2o3heterojunction structure catalysis material and preparation method thereof
CN106076373B (en) * 2016-06-20 2018-05-22 广西大学 A kind of Ag/AgBr/Ga2O3Heterojunction structure catalysis material and preparation method thereof
CN106517109A (en) * 2016-10-21 2017-03-22 南开大学 A preparing method of gallium nitride nanorods
CN107180882A (en) * 2017-05-23 2017-09-19 哈尔滨工业大学 A kind of preparation method of beta-oxidation gallium nano-array
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Application publication date: 20120919