CN104289244A - Preparation method for porous g-C3N4/AgBr nanometer composite material - Google Patents
Preparation method for porous g-C3N4/AgBr nanometer composite material Download PDFInfo
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- CN104289244A CN104289244A CN201410469091.3A CN201410469091A CN104289244A CN 104289244 A CN104289244 A CN 104289244A CN 201410469091 A CN201410469091 A CN 201410469091A CN 104289244 A CN104289244 A CN 104289244A
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Abstract
The invention relates to the field of semiconductor materials, and aims to provide a preparation method for a porous g-C3N4/AgBr nanometer composite material. The method comprises the following steps: pouring tripolycyanamide powder into a corundum crucible boat; introducing argon to completely exhaust air in a vacuum tubular furnace; performing heat treatment to obtain lump g-C3N4 for grinding; dispersing g-C3N4 particles into isopropanol; directly putting turbid liquid obtained after ultrasonic treatment into an oven with the temperature of 60 DEG C for drying; dispersing a grinded g-C3N4 sample into ethanol; dispersing the porous g-C3N4 particles into ethanol, and performing ultrasonic treatment for one hour; adding a bromide water solution into ethanol during stirring and continuously stirring for 3 hours; and adding an AgNO3 water solution again to prepare the porous g-C3N4/AgBr nanometer composite material. The method has the beneficial effect that g-C3N4 with a porous structure is prepared by a simple template-free method.
Description
Technical field
The invention relates to field of semiconductor materials, particularly porous g-C
3n
4the preparation method of/AgBr nano composite material.
Background technology
In recent years, class graphitic carbon nitride (g-C
3n
4) receive extensive concern as a kind of novel visible light catalytic material, but its lower specific area and quantum efficiency constrain it further develops.In order to improve its photocatalytic activity, researchers propose a series of method of modifying, such as: element doping, noble metal loading and form hetero-junctions etc. with other semiconductors coupling.But element doping may be introduced defect or reduce oxidation-reduction potential, reduces its catalytic activity on the contrary; Noble metal loading needs expensive metal as raw material, is unfavorable for large-scale production.And form with other semiconductors coupling the photoresponse scope that hetero-junctions not only can regulate semiconductor, but also effectively can suppress the compound of photo-generated carrier, become present modification g-C
3n
4the most popular method.But, for the g-C prepared by solid phase method
3n
4, often have stratiform or block structure, the active site on surface is less, is unfavorable for and other Material cladding, and compound uniformity is difficult to control.Therefore, one method raising simply and effectively g-C is explored
3n
4this field technical barrier urgently to be resolved hurrily is become with the uniformity of other semi-conducting material compound.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, provides a kind of porous g-C
3n
4the preparation method of/AgBr nano composite material.
For solving the problems of the technologies described above, solution of the present invention is:
Porous g-C
3n
4the preparation method of/AgBr nano composite material, comprises the steps:
Steps A: get melamine powder and pour in corundum crucible boat, and inserted vacuum tube furnace; Pass into argon gas the air in vacuum tube furnace is drained, obtain block g-C through heat treatment
3n
4, after grinding, obtain g-C
3n
4particle;
Wherein, heat treatment temperature is 500 DEG C ~ 600 DEG C, and heat treatment time is 2h ~ 10h;
Step B: by g-C
3n
4granular composite, in isopropyl alcohol, carries out ultrasonic process to it; The suspension of gained after ultrasonic process is placed directly in 60 DEG C of baking ovens and carries out drying, and dried powder is ground again; Then ground g-C is got
3n
4sample dispersion, in ethanol, again after ultrasonic process 1h, is put into water-bath and is carried out stirring in water bath;
Under agitation, dropwise add aqueous sulfuric acid, stir after 2h, water-bath heat treatment 4h, then be placed in hydrothermal reaction kettle and carry out hydro-thermal reaction; By gained pelleting centrifugation after hydro-thermal reaction, and wash three times respectively with distilled water and ethanol, in 60 DEG C of baking ovens, carry out drying, obtain porous g-C
3n
4particle;
Wherein, g-C
3n
4the solid content of particle in isopropyl alcohol is 10g/L ~ 20g/L, and in isopropyl alcohol, sonication treatment time is 5h ~ 10h; g-C
3n
4sample solid content is in ethanol 20g/L ~ 30g/L, and the stirring in water bath time is 15h ~ 25h;
Aqueous sulfuric acid concentration is 10g/L ~ 40g/L, and water-bath heat treatment temperature is 60 DEG C ~ 80 DEG C, and hydrothermal temperature is 150 ~ 180 DEG C, and the hydro-thermal reaction time is 16h ~ 24h;
Step C: by porous g-C
3n
4granular composite in ethanol and ultrasonic process 1h, adds bromide solution and continues to stir 3h, then add AgNO in this mixed liquor in whipping process
3the aqueous solution, then continue to stir 6h; The pelleting centrifugation finally will obtained, washs three times respectively with distilled water and ethanol, at 60 DEG C of drying and processings, and obtained porous g-C
3n
4/ AgBr nano composite material;
Wherein, porous g-C
3n
4particle solid content is in ethanol 5g/L ~ 10g/L, and bromide solution concentration is 1g/L ~ 25g/L, AgNO
3concentration of aqueous solution is 0.5g/L ~ 10g/L, and keeps the mol ratio of Br and Ag to be 1:1 ~ 1.2:1.
In the present invention, the grinding technics adopted in described steps A is ball-milling technology, and these process conditions are: ratio of grinding media to material 30: 1, ball milling speed 200 turns/min, Ball-milling Time 4h.
In the present invention, the bromide adopted in described step C is at least one in softex kw, sodium bromide, KBr.
Operation principle of the present invention: first the present invention adopts ultrasonic process g-C
3n
4powder sample, utilizes that ultrasonic wave amount can reduce its particle size, grain thickness is thinning, improves its follow-up hydrothermal and compound uniformity; Then with the g-C after ultrasonic process
3n
4sample is raw material, take sulfuric acid solution as modifier, by high temperature hydro-thermal, under protonation, makes g-C
3n
4dissolution of partial fiber surface, thus prepare the g-C with loose structure
3n
4, and by after hydrothermal treatment consists, g-C
3n
4surface-active point obtains and significantly promotes.Finally, the g-C after hydrothermal treatment consists is utilized
3n
4surface has loose structure, a large amount of active site and with positive electricity, Br-uniform adsorption can be made in its surface, thus prepare equally distributed porous g-C
3n
4/ AgBr nano composite material.
Compared with prior art, the invention has the beneficial effects as follows:
1, a kind of simple g-C without template synthesis with loose structure is proposed
3n
4, avoid conventional template legal system for porous g-C
3n
4complicated processes;
2, g-C is solved
3n
4the problems such as specific area is low, surface-active point is few and difficult and compound is uneven with other Material cladding, impel AgBr particle at porous g-C
3n
4surface in situ homoepitaxial, is conducive to the photocatalytic activity improving compound system.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail:
Porous g-C
3n
4the preparation method of/AgBr nano composite material, comprises the following steps:
Steps A: first weigh melamine powder and pour in corundum crucible boat, and inserted vacuum tube furnace; Pass into argon gas the air in vacuum tube furnace is drained, obtain block g-C through heat treatment
3n
4, by block for gained g-C
3n
4carry out ball milling: this ball-milling technology condition is: ratio of grinding media to material 30: 1, ball milling speed 200 turns/min, Ball-milling Time 4h, obtain g-C after grinding
3n
4particle;
Wherein, heat treatment temperature is 500 DEG C ~ 600 DEG C, and heat treatment time is 2h ~ 10h.
Step B: by g-C
3n
4granular composite, in isopropyl alcohol, carries out ultrasonic process to it; The suspension of gained after ultrasonic process is placed directly in 60 DEG C of baking ovens and carries out drying, and dried powder is ground again; Then ground g-C is got
3n
4sample dispersion, in ethanol, again after ultrasonic process 1h, is put into water-bath and is carried out stirring in water bath;
Under the condition stirred, dropwise add finite concentration aqueous sulfuric acid, stir after 2h, water-bath heat treatment 4h, then be placed in hydrothermal reaction kettle and carry out hydro-thermal reaction; By gained pelleting centrifugation after hydro-thermal reaction, and wash three times respectively with distilled water and ethanol, in 60 DEG C of baking ovens, carry out drying, obtain porous g-C
3n
4particle;
Wherein, g-C
3n
4the solid content of particle in isopropyl alcohol is 10g/L ~ 20g/L, and in isopropyl alcohol, sonication treatment time is 5h ~ 10h; g-C
3n
4sample solid content is in ethanol 20g/L ~ 30g/L, and the stirring in water bath time is 15h ~ 25h; Aqueous sulfuric acid concentration is 10g/L ~ 40g/L, and water-bath heat treatment temperature is 60 DEG C ~ 80 DEG C, and hydrothermal temperature is 150 ~ 180 DEG C, and the hydro-thermal reaction time is 16h ~ 24h.
Step C: by porous g-C
3n
4granular composite is in ethanol and ultrasonic process 1h; In whipping process, add bromide solution and continue to stir 3h; Slowly AgNO is added again in this mixed liquor
3the aqueous solution, then continue to stir 6h; The pelleting centrifugation finally will obtained, washs three times respectively with distilled water and ethanol, at 60 DEG C of drying and processings, and obtained porous g-C
3n
4/ AgBr nano composite material;
Wherein, porous g-C
3n
4particle solid content is in ethanol 5g/L ~ 10g/L, and bromide solution concentration is 1g/L ~ 25g/L, AgNO
3concentration of aqueous solution is 0.5g/L ~ 10g/L, and keeps the mol ratio of Br and Ag to be 1:1 ~ 1.2:1.
The following examples can make professional and technical personnel's comprehend the present invention of this specialty, but do not limit the present invention in any way.Successfully porous g-C is obtained respectively by 8 embodiments
3n
4the preparation method of/AgBr nano composite material, the test data in each embodiment sees the following form 1.
Table 1 embodiment tables of data
Finally, it is also to be noted that enumerate above be only specific embodiments of the invention son.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (3)
1. porous g-C
3n
4the preparation method of/AgBr nano composite material, is characterized in that, comprises the steps:
Steps A: get melamine powder and pour in corundum crucible boat, and inserted vacuum tube furnace; Pass into argon gas the air in vacuum tube furnace is drained, obtain block g-C through heat treatment
3n
4, after grinding, obtain g-C
3n
4particle;
Wherein, heat treatment temperature is 500 DEG C ~ 600 DEG C, and heat treatment time is 2h ~ 10h;
Step B: by g-C
3n
4granular composite, in isopropyl alcohol, carries out ultrasonic process to it; The suspension of gained after ultrasonic process is placed directly in 60 DEG C of baking ovens and carries out drying, and dried powder is ground again; Then ground g-C is got
3n
4sample dispersion, in ethanol, again after ultrasonic process 1h, is put into water-bath and is carried out stirring in water bath;
Under agitation, dropwise add aqueous sulfuric acid, stir after 2h, water-bath heat treatment 4h, then be placed in hydrothermal reaction kettle and carry out hydro-thermal reaction; By gained pelleting centrifugation after hydro-thermal reaction, and wash three times respectively with distilled water and ethanol, in 60 DEG C of baking ovens, carry out drying, obtain porous g-C
3n
4particle;
Wherein, g-C
3n
4the solid content of particle in isopropyl alcohol is 10g/L ~ 20g/L, and in isopropyl alcohol, sonication treatment time is 5h ~ 10h; g-C
3n
4sample solid content is in ethanol 20g/L ~ 30g/L, and the stirring in water bath time is 15h ~ 25h; Aqueous sulfuric acid concentration is 10g/L ~ 40g/L, and water-bath heat treatment temperature is 60 DEG C ~ 80 DEG C, and hydrothermal temperature is 150 ~ 180 DEG C, and the hydro-thermal reaction time is 16h ~ 24h;
Step C: by porous g-C
3n
4granular composite in ethanol and ultrasonic process 1h, adds bromide solution and continues to stir 3h, then add AgNO in this mixed liquor in whipping process
3the aqueous solution, then continue to stir 6h; The pelleting centrifugation finally will obtained, washs three times respectively with distilled water and ethanol, at 60 DEG C of drying and processings, and obtained porous g-C
3n
4/ AgBr nano composite material;
Wherein, porous g-C
3n
4particle solid content is in ethanol 5g/L ~ 10g/L, and bromide solution concentration is 1g/L ~ 25g/L, AgNO
3concentration of aqueous solution is 0.5g/L ~ 10g/L, and keeps the mol ratio of Br and Ag to be 1:1 ~ 1.2:1.
2. preparation method according to claim 1, is characterized in that, the grinding technics adopted in described steps A is ball-milling technology, and these process conditions are: ratio of grinding media to material 30: 1, ball milling speed 200 turns/min, Ball-milling Time 4h.
3. preparation method according to claim 1, is characterized in that, the bromide adopted in described step C is at least one in softex kw, sodium bromide, KBr.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217598A (en) * | 2015-10-10 | 2016-01-06 | 浙江大学 | A kind of take sucrose as the preparation method that carbon source prepares carbon nanotube |
| CN105665733A (en) * | 2015-11-24 | 2016-06-15 | 鲁东大学 | Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode |
| CN106970031A (en) * | 2017-03-08 | 2017-07-21 | 浙江工业大学 | Flexible carbonitride/reduced graphene electronics composite and its preparation and application |
| CN107876074A (en) * | 2017-10-20 | 2018-04-06 | 浙江大学 | g‑C3N4The preparation method of nano particle/flower-shaped BiOI composites |
| CN108355702A (en) * | 2018-03-23 | 2018-08-03 | 辽宁大学 | A kind of bigger serface carbon defects graphite phase carbon nitride photochemical catalyst and its preparation method and application |
| CN108927201A (en) * | 2018-08-06 | 2018-12-04 | 合肥学院 | A kind of AgBr/g-C3N4The preparation method and application of composite granule |
| CN111071999A (en) * | 2019-11-20 | 2020-04-28 | 嘉兴学院 | Synthesis method of mesoporous graphite-like carbon nitride nanosheet with low metal content |
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| CN102836734A (en) * | 2012-09-20 | 2012-12-26 | 华东理工大学 | Method for preparing AgX@g-C3N4 composite photocatalytic material |
| CN103418415A (en) * | 2013-08-22 | 2013-12-04 | 南昌航空大学 | Method for using ultrasonic mixing to prepare Ag-g-C3N4/TiO2 photocatalyst |
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| SIZHAN WU,ET AL.: "Processing graphitic carbon nitride for improved photocatalytic activity", 《MATERIALSSCIENCE IN SEMICONDUCTOR PROCESSING》, vol. 24, 19 March 2014 (2014-03-19), XP029020790, DOI: doi:10.1016/j.mssp.2014.02.049 * |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217598A (en) * | 2015-10-10 | 2016-01-06 | 浙江大学 | A kind of take sucrose as the preparation method that carbon source prepares carbon nanotube |
| CN105665733A (en) * | 2015-11-24 | 2016-06-15 | 鲁东大学 | Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode |
| CN106970031A (en) * | 2017-03-08 | 2017-07-21 | 浙江工业大学 | Flexible carbonitride/reduced graphene electronics composite and its preparation and application |
| CN106970031B (en) * | 2017-03-08 | 2019-05-31 | 浙江工业大学 | Flexible carbonitride/reduced graphene electronics composite material and its preparation and application |
| CN107876074A (en) * | 2017-10-20 | 2018-04-06 | 浙江大学 | g‑C3N4The preparation method of nano particle/flower-shaped BiOI composites |
| CN107876074B (en) * | 2017-10-20 | 2020-02-18 | 浙江大学 | g-C3N4Preparation method of nanoparticle/flower-shaped BiOI composite material |
| CN108355702A (en) * | 2018-03-23 | 2018-08-03 | 辽宁大学 | A kind of bigger serface carbon defects graphite phase carbon nitride photochemical catalyst and its preparation method and application |
| CN108927201A (en) * | 2018-08-06 | 2018-12-04 | 合肥学院 | A kind of AgBr/g-C3N4The preparation method and application of composite granule |
| CN111071999A (en) * | 2019-11-20 | 2020-04-28 | 嘉兴学院 | Synthesis method of mesoporous graphite-like carbon nitride nanosheet with low metal content |
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Application publication date: 20150121 |