CN106745240A - A kind of square sheet shape BiOCl crystallites and preparation method thereof - Google Patents
A kind of square sheet shape BiOCl crystallites and preparation method thereof Download PDFInfo
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- CN106745240A CN106745240A CN201611059180.6A CN201611059180A CN106745240A CN 106745240 A CN106745240 A CN 106745240A CN 201611059180 A CN201611059180 A CN 201611059180A CN 106745240 A CN106745240 A CN 106745240A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G29/00—Compounds of bismuth
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
Abstract
The invention provides a kind of square sheet shape BiOCl crystallites and preparation method thereof, first with distillation water dissolves KCl, Bi (NO are then slowly added into3)3·5H2O, is stirred at room temperature reaction, obtains precursor liquid, adds water constant volume precursor liquid, precursor liquid is carried out hydro-thermal reaction, washs product after having reacted, dries, that is, obtain square sheet shape BiOCl crystallites.The present invention uses traditional hydro-thermal method, and the square sheet shape BiOCl of pure Tetragonal has been obtained, and the method reaction time is short, flow is few, operating procedure is simple, reaction condition is gentle, cost is relatively low, environmentally safe.Obtained BiOCl crystallites of the invention are Tetragonal, and space structure group is P4/nmm (129), and its pattern, with good light-catalyzed reaction potentiality, is advantageously implemented its application in field of functional materials such as photocatalysis, opto-electronic conversions in corner circle square piece shape.
Description
Technical field
The invention belongs to field of functional materials, it is related to a kind of square sheet shape BiOCl crystallites and preparation method thereof.
Background technology
Bismuth element is located at the Vth main group, period 5, and its common chemical valence is+trivalent.Due to Bi3+Easily polarization deformation,
And the 6s outside electronic structure2Electronics is to being not involved in bonding, therefore 6s2Electronics is to anisotropy.Bismuth based compound have from
The property such as subconductivity, ferroelectricity, ferromagnetic, superconduction, catalysis, wherein BiOX have unique property, such as electrical conductivity high, low energy
Amount band gap, high index of refraction and dielectric constant etc., have a wide range of applications, such as field of electronic materials, electricity in field of functional materials
Solution material, high temperature superconducting materia and photoelectric conversion material etc..
BiOCl is a kind of new photochemical catalyst, and it is that simplest a member is constituted in BiOX family, crystal be by
[Bi2O2] and [Cl] construction unit composition, with layer structure.This layer structure contributes to the photoproduction in photocatalytic process to carry
The transfer of son is flowed, the quantum efficiency of photochemical catalyst is improved.Just because of BiOCl layer structures and suitable energy gap, compared with
Good photocatalytic activity, becomes a kind of very potential catalysis material.
The present Research of nano material shows, the performance of nano material and its pattern, crystalline phase, size, Size Distribution, exposure
Crystal face and synthetic method are closely related.At present, the different BiOCl of pattern is reported in succession, and the microscopic appearance of sample and its
Preparation method is also closely related, there is solvent-thermal method, surfactant assisting ultrasonic method, chemical vapour deposition technique, plasma at present
Body technique, electrochemical process, hydro-thermal method etc..
So far, prepare the work of square sheet shape BiOCl using hydro-thermal method there is not been reported, also without patent and text
Offer and reported that hydro-thermal method prepared square sheet shape BiOCl.
The content of the invention
It is an object of the invention to provide a kind of square sheet shape BiOCl crystallites and preparation method thereof, when the method is reacted
Between it is short, technological process is simple, and obtained BiOCl crystallites are square flake, and even size distribution is preceding with good application
Scape.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of preparation method of square sheet shape BiOCl crystallites, comprises the following steps：
Step 1, KCl is dissolved in deionized water, is stirred, and obtains KCl solution；
Step 2, is (9~13) by the mol ratio of Cl and Bi:(8~11), to addition Bi (NO in KCl solution3)3·5H2O,
Stir, produce white precipitate, continue stirring reaction, obtain precursor liquid；
Step 3, precursor liquid is poured into hydrothermal reaction kettle, 4~12h of hydro-thermal reaction at 175~185 DEG C, after having reacted
Room temperature is naturally cooled to, by product washing, is dried, obtain square sheet shape BiOCl crystallites.
The concentration of KCl solution is 0.3~0.4mol/L in the step 1.
The time of stirring reaction is 30~60min in the step 2.
Before the step 3 is carried out, first to deionized water is added in A mL precursor liquids, the volume constant volume for making precursor liquid is B
ML, wherein A:B=(30~38):45.
Precursor liquid is poured into hydrothermal reaction kettle in the step 3, the filling rate of hydrothermal reaction kettle is 75~80%.
With absolute ethyl alcohol and deionized water washing reaction product in the step 3, then dry 10 at 70~80 DEG C~
12h。
Square sheet shape BiOCl crystallites, the BiOCl obtained in the preparation method of described square sheet shape BiOCl crystallites
The crystal formation of crystallite is Tetragonal, and along the growth of (102) high preferred orientation, its space structure group is P4/nmm (129)；The BiOCl crystallites
Pattern be fillet square piece shape, its length be 3.5~4.5um, width be 2~3um, thickness be 0.5~0.6um.
Relative to prior art, beneficial effects of the present invention are：
The preparation method of the square sheet shape BiOCl crystallites that the present invention is provided, first obtains KCl with deionized water dissolving KCl
Solution, is then slowly added to Bi (NO thereto3)3·5H2O, is stirred at room temperature reaction, obtains precursor liquid, finally makes precursor liquid
Hydro-thermal reaction is carried out, product is washed after having reacted, is dried, that is, obtain square sheet shape BiOCl crystallites.The present invention is used
Traditional hydro-thermal method, has been obtained the square sheet shape BiOCl crystallites of pure Tetragonal, the method has that the reaction time is short, flow is few,
Operating procedure is simple, reaction condition is gentle, cost is relatively low, advantages of environment protection, is a kind of succinct, green BiOCl crystallites
Preparation method.
The present invention is successfully prepared square sheet shape BiOCl crystallites, and obtained its pattern of BiOCl crystallites is in corner circle side
Sheet, surface is smooth, is uniformly dispersed, soilless sticking phenomenon, and size distribution ranges are narrow, is conducive to it in use and other
The uniform mixing of material, enables its performance to unify to play, and reaches the purpose of its effective use.And it is of the invention obtained
BiOCl crystallites are pure phase, and crystallinity is high and physically well develops, and is advantageously implemented the advantage performance of its active crystal face.The present invention
Obtained BiOCl crystallites are Tetragonal, and space structure group is P4/nmm (129), with good light-catalyzed reaction potentiality, is conducive to
Realize its application in field of functional materials such as photocatalysis, opto-electronic conversions.
Brief description of the drawings
Fig. 1 is the XRD diffracting spectrums of square sheet shape BiOCl crystallites prepared by the present invention；
Fig. 2 is the SEM figures of square sheet shape BiOCl crystallites prepared by the present invention.
Specific embodiment
The present invention is described further with currently preferred specific embodiment below in conjunction with the accompanying drawings, raw material is analysis
It is pure.
Embodiment 1：
Step 1,9mmol KCl are dissolved in 30mL deionized waters, are stirred, and obtain the KCl that concentration is 0.3mol/L
Solution；
Step 2,8mmol Bi (NO are slowly added in the 30mL KCl solution to step 1 preparation3)3·5H2O, stirring is equal
It is even, white precipitate generation is had in solution, continue strong stirring reaction 30min, obtain precursor liquid；
Step 3, to addition 15mL deionized waters in the 30mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
80%, the hydro-thermal reaction 6h at 180 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 12h, the side of obtaining by the product after washing at 70 DEG C
Shape flake BiOCl crystallites.
Embodiment 2：
Step 1,9.9mmol KCl are dissolved in 30mL deionized waters, are stirred, and it is 0.33mol/L's to obtain concentration
KCl solution；
Step 2,9.3mmol Bi (NO are slowly added in the 30mL KCl solution to step 1 preparation3)3·5H2O, stirring is equal
It is even, white precipitate generation is had in solution, continue strong stirring reaction 35min, obtain precursor liquid；
Step 3, to addition 15mL deionized waters in the 30mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
80%, the hydro-thermal reaction 8h at 180 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 10h, the side of obtaining by the product after washing at 70 DEG C
Shape flake BiOCl crystallites.
Embodiment 3：
Step 1,11.9mmol KCl are dissolved in 35mL deionized waters, are stirred, and it is 0.34mol/L's to obtain concentration
KCl solution；
Step 2,9.9mmol Bi (NO are slowly added in the 35mL KCl solution to step 1 preparation3)3·5H2O, stirring is equal
It is even, white precipitate generation is had in solution, continue strong stirring reaction 40min, obtain precursor liquid；
Step 3, to addition 10mL deionized waters in the 35mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
80%, the hydro-thermal reaction 12h at 180 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 11h, the side of obtaining by the product after washing at 75 DEG C
Shape flake BiOCl crystallites.
Embodiment 4：
Step 1,11.4mmol KCl are dissolved in 30mL deionized waters, are stirred, and it is 0.38mol/L's to obtain concentration
KCl solution；
Step 2,8.9mmol Bi (NO are slowly added in the 30mL KCl solution to step 1 preparation3)3·5H2O, stirring is equal
It is even, white precipitate generation is had in solution, continue strong stirring reaction 50min, obtain precursor liquid；
Step 3, to addition 15mL deionized waters in the 30mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
80%, the hydro-thermal reaction 12h at 180 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 12h, the side of obtaining by the product after washing at 80 DEG C
Shape flake BiOCl crystallites.
Embodiment 5
Step 1,13mmol KCl are dissolved in 37mL deionized waters, are stirred, and it is 0.35mol/L's to obtain concentration
KCl solution；
Step 2,10.1mmol Bi (NO are slowly added in the 37mL KCl solution to step 1 preparation3)3·5H2O, stirring
Uniformly, white precipitate generation is had in solution, continues strong stirring reaction 55min, obtain precursor liquid；
Step 3, to addition 8mL deionized waters in the 37mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
80%, the hydro-thermal reaction 8h at 180 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 11.5h by the product after washing at 80 DEG C, obtains
Square sheet shape BiOCl crystallites.
Embodiment 6
Step 1,12.4mmol KCl are dissolved in 31mL deionized waters, are stirred, and it is 0.4mol/L's to obtain concentration
KCl solution；
Step 2,10mmol Bi (NO are slowly added in the 31mL KCl solution to step 1 preparation3)3·5H2O, stirring is equal
It is even, white precipitate generation is had in solution, continue strong stirring reaction 60min, obtain precursor liquid；
Step 3, to addition 14mL deionized waters in the 31mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
80%, the hydro-thermal reaction 10h at 180 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 12h, the side of obtaining by the product after washing at 75 DEG C
Shape flake BiOCl crystallites.
Embodiment 7
Step 1,12.2mmol KCl are dissolved in 38mL deionized waters, are stirred, and it is 0.32mol/L's to obtain concentration
KCl solution；
Step 2,11mmol Bi (NO are slowly added in the 38mL KCl solution to step 1 preparation3)3·5H2O, stirring is equal
It is even, white precipitate generation is had in solution, continue strong stirring reaction 45min, obtain precursor liquid；
Step 3, to addition 7mL deionized waters in the 38mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
75%, the hydro-thermal reaction 11h at 175 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 10.5h by the product after washing at 78 DEG C, obtains
Square sheet shape BiOCl crystallites.
Embodiment 8
Step 1,11.5mmol KCl are dissolved in 32mL deionized waters, are stirred, and it is 0.36mol/L's to obtain concentration
KCl solution；
Step 2,10.5mmol Bi (NO are slowly added in the 32mL KCl solution to step 1 preparation3)3·5H2O, stirring
Uniformly, white precipitate generation is had in solution, continues strong stirring reaction 48min, obtain precursor liquid；
Step 3, to addition 13mL deionized waters in the 32mL precursor liquids that step 2 is obtained, the volume constant volume for making precursor liquid is
45mL；
Step 4, the precursor liquid after step 3 constant volume is put into hydrothermal reaction kettle, it is ensured that the filling rate of hydrothermal reaction kettle is
78%, the hydro-thermal reaction 4h at 185 DEG C.Room temperature is naturally cooled to after having reacted, respectively with deionized water and washes of absolute alcohol
Product, until the supernatant after washing is in neutrality, then dries 11.5h by the product after washing at 72 DEG C, obtains
Square sheet shape BiOCl crystallites.
Fig. 1 is the XRD diffracting spectrums of square sheet shape BiOCl crystallites prepared by the present invention, it can be seen that being obtained
BiOCl crystallites be pure Tetragonal BiOCl (JCPDS NO.06-0249), space structure group is P4/nmm (129), along (102)
High preferred orientation grow, and (101), (002), (110), (111), (003), (112), (200), (201), (110), (211),
(104), the diffraction maximum of the crystal face such as (212), (114), (005), (220) substantially, illustrates that its crystallization is all right.
Fig. 2 is the SEM figures of square sheet shape BiOCl crystallites prepared by the present invention, it can be seen that obtained
BiOCl crystallite shapes are regular, and surface is smooth, be uniformly dispersed, soilless sticking phenomenon, and are corner circle square sheet shape.Square piece
3.5~4.5um is about, about 2~3um wide, thickness is about 0.5~0.6um.
The present invention uses traditional hydro-thermal method, and the square sheet shape BiOCl crystallites of pure Tetragonal, the method reaction has been obtained
Time is short, flow is few, operating procedure is simple, reaction condition is gentle, cost is relatively low, environmentally safe.Obtained side of the invention
The crystallinity of shape flake BiOCl crystallites is high and physically well develops, and size distribution ranges are narrow, are advantageously implemented its active crystal face
Advantage performance, while be conducive to its in use with the uniform mixing of other materials, its performance is unified
Play, reach the purpose of its effective use.There is obtained square sheet shape BiOCl crystallites of the invention good light-catalyzed reaction to dive
Power, is advantageously implemented its application in field of functional materials such as photocatalysis, opto-electronic conversions.
One embodiment of the present invention is the foregoing is only, is not all of or unique implementation method, this area is common
Any equivalent conversion that technical staff is taken technical solution of the present invention by reading description of the invention, is the present invention
Claim covered.
Claims (7)
1. a kind of preparation method of square sheet shape BiOCl crystallites, it is characterised in that comprise the following steps：
Step 1, KCl is dissolved in deionized water, is stirred, and obtains KCl solution；
Step 2, is (9~13) by the mol ratio of Cl and Bi:(8~11), to addition Bi (NO in KCl solution3)3·5H2O, stirring
Uniformly, white precipitate is produced, continues stirring reaction, obtain precursor liquid；
Step 3, precursor liquid is poured into hydrothermal reaction kettle, 4~12h of hydro-thermal reaction at 175~185 DEG C, natural after having reacted
Room temperature is cooled to, by product washing, is dried, obtain square sheet shape BiOCl crystallites.
2. the preparation method of square sheet shape BiOCl crystallites according to claim 1, it is characterised in that：In the step 1
The concentration of KCl solution is 0.3~0.4mol/L.
3. the preparation method of square sheet shape BiOCl crystallites according to claim 1, it is characterised in that：In the step 2
The time of stirring reaction is 30~60min.
4. the preparation method of square sheet shape BiOCl crystallites according to claim 1, it is characterised in that：The step 3 is entered
Before row, first to deionized water is added in A mL precursor liquids, the volume constant volume for making precursor liquid is B mL, wherein A:B=(30~38):
45。
5. the preparation method of square sheet shape BiOCl crystallites according to claim 1, it is characterised in that：In the step 3
Precursor liquid is poured into hydrothermal reaction kettle, the filling rate of hydrothermal reaction kettle is 75~80%.
6. the preparation method of square sheet shape BiOCl crystallites according to claim 1, it is characterised in that：In the step 3
With absolute ethyl alcohol and deionized water washing reaction product, then dry 10~12h at 70~80 DEG C.
7. square obtained in the preparation method of the square sheet shape BiOCl crystallites according to any one in claim 1-6
Laminar BiOCl crystallites, it is characterised in that：The crystal formation of the BiOCl crystallites is Tetragonal, and along the growth of (102) high preferred orientation, it is empty
Between structure group be P4/nmm (129)；The pattern of the BiOCl crystallites is fillet square piece shape, and its length is 3.5~4.5um, and width is
2~3um, thickness is 0.5~0.6um.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483494A (en) * | 2018-02-27 | 2018-09-04 | 南京信息工程大学 | A kind of nanometer thin sheet BiOI and the purposes as electrode material |
| CN108940323A (en) * | 2018-07-09 | 2018-12-07 | 王子韩 | A kind of preparation method and applications of BiOBr nanometer rods |
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| CN102910673A (en) * | 2012-10-19 | 2013-02-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing BiOCl micro-flower nanometer photocatalysis material |
| CN104069876A (en) * | 2014-06-24 | 2014-10-01 | 华中师范大学 | Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483494A (en) * | 2018-02-27 | 2018-09-04 | 南京信息工程大学 | A kind of nanometer thin sheet BiOI and the purposes as electrode material |
| CN108940323A (en) * | 2018-07-09 | 2018-12-07 | 王子韩 | A kind of preparation method and applications of BiOBr nanometer rods |
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Application publication date: 20170531 |