CN104828781B - Eggshell-shaped porous Bi4O5Br2Preparation method of nano material - Google Patents
Eggshell-shaped porous Bi4O5Br2Preparation method of nano material Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 102000002322 Egg Proteins Human genes 0.000 claims abstract description 30
- 108010000912 Egg Proteins Proteins 0.000 claims abstract description 30
- 210000003278 egg shell Anatomy 0.000 claims abstract description 30
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 5
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- 239000003643 water by type Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 3
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- 238000005516 engineering process Methods 0.000 abstract description 15
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
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Abstract
The invention discloses an eggshell-shaped porous Bi4O5Br2A method for preparing nano material. The invention adopts two steps of technological processes of ultrasonic chemistry technology and heat treatment to prepare eggshell-shaped porous Bi4O5Br2And (3) nano materials. Soluble bismuth salt, hexadecyl trimethyl ammonium bromide and deionized water are firstly used as raw materialsRaw materials are fully stirred and dissolved and then are subjected to one-pot ultrasonic chemical reaction to prepare a precursor compound; then annealing the precursor compound to prepare eggshell-shaped porous Bi4O5Br2And (3) nano materials. The invention discloses eggshell-shaped porous Bi4O5Br2The nano material is of a hollow hierarchical structure, is similar to an eggshell, has no agglomeration and good dispersibility, the diameter of an opening end is 500-800 nm, the thickness of the shell is about 20nm, a large number of pores are formed on the surface, and the specific surface area is large. The method does not use organic solvent, and the process is clean and friendly; the prepared nano material can be used in the fields of visible light catalysis, antibiosis and the like.
Description
Technical field
It is that to be related to a kind of eggshell state porous specifically the invention belongs to the preparing technical field of inorganic functional material
Bi4O5Br2The preparation method of nano material.
Background technology
Nano material suffers from important work in numerous areas such as nanometer light, electricity, magnetic because of its distinctive function and property
With.The morphological structure of nano material, particle size and its physical and chemical performance are closely related, with the micro- of unique morphology structure
Nano material generally shows superior physical and chemical performance, is increasingly paid much attention to by people.The hollow micro-nano of hierarchy
Rice structural material because having larger specific surface area, relatively low density, excellent permeability and unique photoelectricity and surface property,
Always one of nanometer material science study hotspot.
Ternary bismuthino oxyhalide (BiVOVIXVII, X=Cl, Br, I) and it is the important semi-conducting material of cluster, in photo-thermal, light
Suffer from being widely applied in terms of electricity, sensor, superconduction, solar cell, lithium battery and photochemical catalyst.Due to bismuthino oxyhalogen
The semiconductor energy level bandwidth of compound is typically in the range of between 2.1~2.9eV, with visible response performance, in recent years as visible ray
Catalyst presents excellent performance in terms of degradation of contaminant.Except BiOX chemical combination beyond the region of objective existences, the high-order of some oxygen-enriched poor halogen
Compound, such as Bi12O15Cl6、Bi3O4Cl、Bi4O5Br2、Bi5O7I、Bi7O9I3And Bi24O31Br10Deng because containing different elements
Metering ratio is learned, the energy level bandwidth of semiconductor is effectively have adjusted, thus embodies the things such as light, the electricity of material composition and structure regulating
Physicochemical performance.The ternary oxyhalogen bismuth compound of the different stoichiometric proportions of these high-orders is traditionally prepared, is all logical at high temperature
Cross made from vapour deposition process, temperature is usually above 600 DEG C.Gas phase deposition technology needs complex precise and the instrument of costliness is set
It is standby, some poisonous gases such as HBr etc. is also used as raw material among preparing sometimes.With regard to the oxygen-enriched compound of ternary high-order
Bi4O5Br2For semi-conducting material, Keller etc. first reported its crystal structure, be monoclinic phase, P21(4) space group, structure cell
Parameter is a=14.539S4, b=5.605S1,β=97.75 (7) °, Z=4 (Keller E., Ketterer
J.,V.,Zeitschrift für Kristallographie,2001,216(11):595-599)；Recently,
Semiconductor Bi has been made using hydrothermal technique in Chen etc.4O5Br2Photochemical catalyst, it is seen that it is excellent that photocatalysis experiment shows that catalyst has
Degradable organic pollutant crystal violet (Crystal Violet) dyestuff more performance (Chen, H.L., Lee W.W., Chung,
W.H.,Lin,H.P.,Chen,Y.J.,Jiang,Y.R.,Lin,W.Y.,Chen,C.C,Journal of the Taiwan
Institute of Chemical Engineers,2014,in press).With regard to literature survey, the semiconductor on pure phase
Bi4O5Br2The research of photochemical catalyst is still considerably deficient, therefore, and a kind of simple and direct efficient controllable preparation pure phase of development has uniqueness
The oxygen-enriched compound Bi of ternary of morphological structure4O5Br2Semiconductor light-catalyst is still a challenging job.
The content of the invention
It is an object of the invention to for the oxygen-enriched compound Bi of current ternary4O5Br2Nano material and its technology of preparing it is tight
Weight is not enough, and there is provided a kind of porous Bi of eggshell state4O5Br2The simple preparation method of nano material, its technique is simple, and raw material is easy to get, into
This is low, and yield is high, and obtained nano material has huge in terms of using visible ray or solar radiation photocatalytic degradation environmental contaminants
Big application prospect.
The purpose of the present invention is achieved by the following technical solution.
The technical scheme is that porous to prepare using sonochemistry technology and heat treatment two-step process process
Bi4O5Br2Nano material.Wherein sonochemistry process is with soluble bismuth salt, cetyl trimethylammonium bromide (CTAB) and gone
Ionized water is raw material, through the reaction of " one pot " sonochemistry after being sufficiently stirred for dissolving, and a kind of precursor compound is made and (is named as
BOBP)；Again by this precursor compound BOBP by annealing, so that the porous Bi of eggshell state is made4O5Br2Nano material.Its
Concrete technology step is described as follows：
S1 weighs the water bismuth nitrate Bi (NO of 0.4mmol five3)3·5H2The stirring of O deionized waters is hydrolyzed into Sol A；
S2 weighs a certain amount of cetyl trimethylammonium bromide (CTAB) and solution B, five water nitre is configured to deionized water
The mol ratio of sour bismuth and CTAB is 1:1~1:2；
S3 weighs 10mmol complexing agents thiocarbamide (Tu) and is configured to solution C with deionized water again；
Solution B addition Sol A under agitation, is added to A, B mixed reaction solution by S4 in, then by solution C successively
In, overall solution volume is 60mL, continues to stir 10 minutes；
Mixed reaction solution is transferred in 100mL blue cover glass bottle by S5, is placed in the ultrasonic cleaner for filling running water
In, the temperature setting of ultra sonic bath is between 60~90 DEG C, and ultrasound wave irradiation time control after reaction terminates, took at 20~60 minutes
Go out and naturally cool to room temperature, filtering precipitate is washed 2~3 times with water and absolute ethyl alcohol respectively, it is 60 to put the precipitate in temperature
Heated 6~10 hours in DEG C baking oven, it is precursor B OBP to collect purple product；
It is small that precursor B OBP in air atmosphere is heated 1~2 by S6 in temperature in the Muffle furnace between 450~480 DEG C
When, that is, obtain the porous Bi of eggshell state of the present invention4O5Br2Nano material.
In above-mentioned technical proposal, the porous Bi of described eggshell state4O5Br2Nano material is hollow hierarchy, similar egg
Shelly, soilless sticking, good dispersion, port diameter is between 500~800nm, and thickness of the shell is about the presence of substantial amounts of hole on 20nm, surface
Gap, there is larger specific surface area.
The mol ratio of five water bismuth nitrates and CTAB in the step S2 is 1:1.375.
Bath temperature in the step S5 is 80 DEG C；The ultrasound wave irradiation time is 30 minutes.
Annealing temperature in the step S6 is 460 DEG C, and the heat time is 2 hours.
The preparation technology equipment is simple, and environment temperature is low, easy to operate, reproducible；Do not use organic solvent, environment
Close friend's cleaning；Product yield is high, good crystallinity；Raw material is easy to get, with low cost, suitable industrialized production.
Brief description of the drawings
Fig. 1 is the porous Bi of the eggshell state of the embodiment of the present invention 14O5Br2The X-ray powder diffraction analysis of porous nanometer material
(XRD) spectrogram；
Fig. 2 is the porous Bi of the eggshell state of the embodiment of the present invention 14O5Br2The low power field scan electron microscope of nano material
(SEM) photo；
Fig. 3 is the porous Bi of the eggshell state of the embodiment of the present invention 14O5Br2The high power field scan electron microscope of nano material
(SEM) photo；
Fig. 4 is the porous Bi of the eggshell state of the embodiment of the present invention 14O5Br2Transmission electron microscope (TEM) photo of nano material.
Embodiment
Make further detailed complete description to technical scheme below by way of specific embodiment.Following reality
It is that the present invention is further illustrated to apply example, and is not limited the scope of the invention.
Embodiment 1
The porous Bi of eggshell state of the present invention4O5Br2Nano material is prepared using sonochemistry technology and heat treatment two-step process
Obtain, its concrete technology step is as follows：
S1 weighs the water bismuth nitrate Bi (NO of 1.940g five3)3·5H2O is hydrolyzed into Sol A with the stirring of 10mL deionized waters；
S2 weighs 0.2001g cetyl trimethylammonium bromides (CTAB) and solution B, five water is configured to 20mL deionized waters
Bismuth nitrate and CTAB mol ratio are 1:1.375；
S3 weighs 0.7612g thiocarbamides (Tu) and is configured to solution C with 30mL deionized waters again；
Solution B addition Sol A under agitation, is added to A, B mixed reaction solution by S4 in, then by solution C successively
In, continue to stir 10 minutes；
Mixed reaction solution is transferred in 100mL blue cover glass bottle by S5, is placed in the ultrasonic cleaner for filling running water
In, the temperature of ultra sonic bath is at 80 DEG C, and the ultrasound wave irradiation time, after reaction terminates, taking-up naturally cooled to room temperature, filters at 30 minutes
Sediment, is washed 2~3 times with water and absolute ethyl alcohol respectively, is put the precipitate in temperature to be heated 8 hours in 60 DEG C of baking ovens, is received
It is precursor B OBP to collect purple product；
S6 heating 2 hours in 460 DEG C of Muffle furnaces in air atmosphere by precursor B OBP, that is, obtain the eggshell of the present invention
The porous Bi of shape4O5Br2Nano material.
Referring to accompanying drawing 1, the porous Bi of eggshell state made from the method as described in embodiment 14O5Br2The X-ray of nano material
Powder diffraction analysis (XRD) spectrogram.All diffraction crystal faces of spectral line peak position and JCPDF standard cards (37-3699) are one by one in figure
Correspondence, is designated as the Bi of monoclinic phase4O5Br2Crystal, space group P21/ 4, lattice constant
β=97.6 °.Impure diffraction maximum is not found, illustrates that it is pure Bi to be made4O5Br2Crystal, diffraction maximum has obvious widthization,
Show that particle diameter is smaller.
Referring to accompanying drawing 2, the porous Bi of eggshell state made from the method as described in embodiment 14O5Br2The low power of nano material
ESEM (SEM) photo.As can be seen from the figure the porous Bi of eggshell state4O5Br2Nano material yield is high, in opening hemispherical,
Good dispersion, soilless sticking, particle diameter distribution is uniform.
Referring to accompanying drawing 3, the porous Bi of eggshell state made from the method as described in embodiment 14O5Br2The high power of nano material
ESEM (SEM) photo.As can be seen from the figure the porous Bi of eggshell state4O5Br2Nano material is hollow hierarchy, end
Mouth diameter is between 500~800nm, and thickness of the shell is about there is hole on 20nm, surface.
Referring to accompanying drawing 4, the porous Bi of eggshell state made from the method as described in embodiment 14O5Br2The transmission electricity of nano material
Mirror (TEM) photo.What light and shade was met each other, which speculate, which also show particle, has hollow property, and further demonstrate on particle surface
There is more great pore structure, there is larger specific surface area.
Embodiment 2
The porous Bi of eggshell state of the present invention4O5Br2Nano material is prepared using sonochemistry technology and heat treatment two-step process
Obtain, its concrete technology step is as follows：
S1 weighs the water bismuth nitrate Bi (NO of 1.940g five3)3·5H2O is hydrolyzed into Sol A with the stirring of 10mL deionized waters；
S2 weighs 0.1455g cetyl trimethylammonium bromides (CTAB) and solution B, five water is configured to 20mL deionized waters
Bismuth nitrate and CTAB mol ratio are 1:1；
S3 weighs 0.7610g thiocarbamides (Tu) and is configured to solution C with 30mL deionized waters again；
Solution B addition Sol A under agitation, is added to A, B mixed reaction solution by S4 in, then by solution C successively
In, continue to stir 10 minutes；
Mixed reaction solution is transferred in 100mL blue cover glass bottle by S5, is placed in the ultrasonic cleaner for filling running water
In, the temperature of ultra sonic bath is at 60 DEG C, and the ultrasound wave irradiation time, after reaction terminates, taking-up naturally cooled to room temperature, filters at 40 minutes
Sediment, is washed 2~3 times with water and absolute ethyl alcohol respectively, is put the precipitate in temperature to be heated 10 hours in 60 DEG C of baking ovens, is received
It is precursor B OBP to collect purple product；
S6 heating 1 hour in 480 DEG C of Muffle furnaces in air atmosphere by precursor B OBP, that is, obtain the ternary of the present invention
Oxygen-enriched semiconductor Bi4O5Br2Porous nanometer material.
Bi made from method as described in embodiment 24O5Br2Nano material, is in be similar to " egg shell " shape with SEM observations
Hollow sphere structure.
Embodiment 3
The porous Bi of eggshell state of the present invention4O5Br2Nano material is prepared using sonochemistry technology and heat treatment two-step process
Obtain, its concrete technology step is as follows：
S1 weighs the water bismuth nitrate Bi (NO of 1.942g five3)3·5H2O is hydrolyzed into Sol A with the stirring of 10mL deionized waters；
S2 weighs 0.2910g cetyl trimethylammonium bromides (CTAB) and solution B, five water is configured to 20mL deionized waters
Bismuth nitrate and CTAB mol ratio are 1:2；
S3 weighs 0.7612g thiocarbamides (Tu) and is configured to solution C with 30mL deionized waters again；
Solution B addition Sol A under agitation, is added to A, B mixed reaction solution by S4 in, then by solution C successively
In, continue to stir 10 minutes；
Mixed reaction solution is transferred in 100mL blue cover glass bottle by S5, is placed in the ultrasonic cleaner for filling running water
In, the temperature of ultra sonic bath is at 90 DEG C, and the ultrasound wave irradiation time, after reaction terminates, taking-up naturally cooled to room temperature, filters at 20 minutes
Sediment, is washed 2~3 times with water and absolute ethyl alcohol respectively, is put the precipitate in temperature to be heated 8 hours in 60 DEG C of baking ovens, is received
It is precursor B OBP to collect purple product；
S6 heating 1.5 hours in 460 DEG C of Muffle furnaces in air atmosphere by precursor B OBP, that is, obtain the three of the present invention
The oxygen-enriched semiconductor Bi of member4O5Br2Porous nanometer material.
Bi made from method as described in embodiment 34O5Br2Nano material, is in be similar to " egg shell " shape with SEM observations
Hollow sphere structure.
Embodiment 4
The porous Bi of eggshell state of the present invention4O5Br2Nano material is prepared using sonochemistry technology and heat treatment two-step process
Obtain, its concrete technology step is as follows：
S1 weighs the water bismuth nitrate Bi (NO of 1.940g five3)3·5H2O is hydrolyzed into Sol A with the stirring of 10mL deionized waters；
S2 weighs 0.2001g cetyl trimethylammonium bromides (CTAB) and solution B, five water is configured to 20mL deionized waters
Bismuth nitrate and CTAB mol ratio are 1:1.375；
S3 weighs 0.7612g thiocarbamides (Tu) and is configured to solution C with 30mL deionized waters again；
Solution B addition Sol A under agitation, is added to A, B mixed reaction solution by S4 in, then by solution C successively
In, continue to stir 10 minutes；
Mixed reaction solution is transferred in 100mL blue cover glass bottle by S5, is placed in the ultrasonic cleaner for filling running water
In, the temperature of ultra sonic bath is at 80 DEG C, and the ultrasound wave irradiation time, after reaction terminates, taking-up naturally cooled to room temperature, filters at 60 minutes
Sediment, is washed 2~3 times with water and absolute ethyl alcohol respectively, is put the precipitate in temperature to be heated 6 hours in 60 DEG C of baking ovens, is received
It is precursor B OBP to collect purple product；
S6 heating 1.5 hours in 480 DEG C of Muffle furnaces in air atmosphere by precursor B OBP, that is, obtain the three of the present invention
The oxygen-enriched semiconductor Bi of member4O5Br2Porous nanometer material.
Bi made from method as described in embodiment 44O5Br2Nano material, is in be similar to " egg shell " shape with SEM observations
Hollow sphere structure.
Claims (4)
1. a kind of porous Bi of eggshell state4O5Br2The preparation method of nano material, it is characterised in that comprise the following steps：
S1:Weigh the stirring of the water bismuth nitrate deionized waters of 0.4mmol five and be hydrolyzed into Sol A；
S2:Weigh CTAB and be configured to solution B with deionized water, five water bismuth nitrates and CTAB mol ratio are 1:1~1:2；
S3:Weigh 10mmol complexing agent thiocarbamides and be configured to solution C with deionized water；
S4:Under agitation, first solution B addition Sol A is added in A, B mixed reaction solution in, then by solution C, it is molten
Liquid cumulative volume is 60mL, continues to stir 10 minutes；
S5:Mixed reaction solution is transferred in 100mL blue cover glass bottle, blue cover glass bottle is placed in ultrasonic cleaner,
The temperature setting of ultra sonic bath is 60~90 DEG C, and ultrasound wave irradiation time control was at 20~60 minutes, after reaction terminates, and took out nature cold
But to room temperature, filtering precipitate is washed 2~3 times with water and absolute ethyl alcohol respectively, puts the precipitate in the baking oven that temperature is 60 DEG C
Middle heating 6~10 hours, collects the precursor B OBP of purple；
S6:Precursor B OBP is made annealing treatment 1~2 hour in Muffle furnace, it is 450~480 DEG C to control furnace temperature, products obtained therefrom is
For the porous Bi of eggshell state4O5Br2Nano material.
2. the porous Bi of a kind of eggshell state according to claim 14O5Br2The preparation method of nano material, it is characterised in that
The mol ratio of five water bismuth nitrates and CTAB in step S2 is 1:1.375.
3. the porous Bi of a kind of eggshell state according to claim 14O5Br2The preparation method of nano material, it is characterised in that
The temperature of ultra sonic bath is 80 DEG C in step S5, and the ultrasound wave irradiation time is 30 minutes.
4. the porous Bi of a kind of eggshell state according to claim 14O5Br2The preparation method of nano material, it is characterised in that
Annealing temperature in step S6 is 460 DEG C, and the heat time is 2 hours.
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| CN106582726A (en) * | 2016-09-30 | 2017-04-26 | 南京大学 | Bi4o5Br2 hollow sphere and preparation method using micro-emulsion as template |
| CN109603865A (en) * | 2019-01-28 | 2019-04-12 | 合肥学院 | A kind of bismuth metal/bismuth oxybromide composite nano materials and preparation method thereof |
| CN109702186A (en) * | 2019-01-28 | 2019-05-03 | 合肥学院 | A kind of bismuth metal nanometer shell material and preparation method thereof |
| CN111701601A (en) * | 2020-06-05 | 2020-09-25 | 南阳师范学院 | Bi4O5Br2Preparation method of self-assembled hollow flower ball and photocatalytic reduction of CO2Application of aspects |
| CN112570030A (en) * | 2020-12-29 | 2021-03-30 | 天津理工大学 | Bi4O5Br2Preparation method and application of/Fe-MIL composite material photocatalyst |
| CN113998734B (en) * | 2021-11-09 | 2024-01-26 | 淮阴师范学院 | Bi 5 O 7 Preparation method of Br nanosheets |
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| US8383021B1 (en) * | 2008-11-13 | 2013-02-26 | Sandia Corporation | Mixed-layered bismuth-oxygen-iodine materials for capture and waste disposal of radioactive iodine |
| CN104226339A (en) * | 2014-09-18 | 2014-12-24 | 玉林师范学院 | Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof |
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