CN106277050A - A kind of novel light absorbent and preparation method thereof - Google Patents
A kind of novel light absorbent and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of novel light absorbent and preparation method thereof, described light absorbent be chemical formula be Bi9O7.5S6Single-phase compounds, described light absorbent has layer structure, and its structure is [BiS2 -] layer and [Bi2O2 2+] layer forms along the alternately accumulation of [001] direction, wherein Bi is+trivalent, and O is-divalent, and S is-divalent.The light absorbent Bi of the present invention9O7.5S6Being a kind of stable novel lamellar compound with good absorbing properties, it has superior absorbing properties, good photoelectric transformation efficiency, has opto-electronic conversion field and have broad application prospects.
Description
Technical field
The invention belongs to solar energy light absorption Material Field, particularly to a kind of novel lamellar light absorbent and preparation method thereof.
Background technology
Solar energy optical-thermal application be human use's solar energy the most simply, one of approach the most direct, maximally effective, with solar energy
Photovoltaic technology is that the Solar use the supported energy consumption structure to the mankind brings revolutionary change.Therefore, for a long time with
Come, how low-grade solar energy is converted into high-grade heat energy, and solar energy is enriched with, in order to land productivity to greatest extent
With solar energy, become study hotspot.Development can the catalysis material of spectral absorption visible ray (wavelength is 400～700 nanometers) entirely,
It it is the premise realizing high-efficiency solar photocatalytic conversion.In known solar energy light absorption material, the bismuth oxysulfide of stratiform is because of it
The character of some uniquenesses, such as Bi2O2S9Photocatalytic activity, Bi2O2The pyroelectric effect of Se, and hybrid metal oxysulfide
Water-splitting phenomenon etc., of great interest.It is noted that the band gap of oxysulfide is generally less than oxide,
Some is close to optimal band-gap photovoltaic material (～1.5eV), and this also show the photoelectric properties that it is potential.Therefore, by attention collection
In be just particularly important in the research of its photoelectric properties.And the prior synthesizing method of bismuth oxysulfide generally requires through complexity
Mechanical lapping and repeat sintering process for a long time.But, there is research display, the compound of metastable phase and layer structure can be passed through
Hydro-thermal method obtains relatively easily.It practice, hydro-thermal method can be as preparing the important of several oxysulfide under relatively mild conditions
Method, such as BiOCuS and Bi2O2S.Therefore, hydro-thermal method is a kind of effective ways of new sulfur compou nd synthesis.But,
There is presently no and prepare Bi about by hydro-thermal method9O7.5S6Report.
Summary of the invention
The problem existed for prior art, it is an object of the invention to provide a kind of novel light absorbent Bi9O7.5S6And water
Hot preparation method.
Here, on the one hand, the present invention provides a kind of novel light absorbent, described light absorbent be chemical formula be Bi9O7.5S6
Single-phase compounds, described light absorbent has layer structure, and its structure is [BiS2 -] layer and [Bi2O2 2+] [001] direction friendship of layer edge
Forming for accumulation, wherein Bi is+trivalent, and O is-divalent, and S is-divalent.
It is preferred that described light absorbent presents the hexagon of rule, size is at 40～60 microns.
It is preferred that described light absorbent is space group is the crystal of R3m diamond structure, its cell parameter is:
It is preferred that the band gap of described light absorbent is 1.27eV.
It is preferred that described light absorbent is under conditions of applied voltage is 1V, density of photocurrent is the twice of dark current density
Above.
The light absorbent Bi of the present invention9O7.5S6It is a kind of stable novel lamellar compound with good absorbing properties,
It has superior absorbing properties, good photoelectric transformation efficiency, has opto-electronic conversion field and has broad application prospects.
On the other hand, the present invention also provides for the preparation method of above-mentioned light absorbent, comprises the following steps:
A) by Bi source, S source according to mol ratio 1:(0.5～1.5) add and water and ethanol are mixed and stirred for uniformly, obtain mixing molten
Liquid A；
B) adding alkali in gained mixed solution A, make described mixed solution basicity reach more than 5mol/L, stirring makes mixture equal
Even mixing, obtains mixed solution B；
C) mixed solution B is transferred in reactor in 433～513K reaction 1～7 day, by synthetic product wash, ultrasonic,
Obtain described light absorbent.
The present invention uses the hydrothermal method of simplicity to prepare single-phase Bi9O7.5S6Light absorbent.The preparation method letter of the present invention
Single the most easy, utilize regulation and control parameters, can finally be prepared as stable there is the novel of good absorbing properties by the method
Lamellar compound.
It is preferred that in step a), Bi source is the soluble-salt of Bi element, S source is organic sulfur compound or sulfur simple substance.
It is preferred that in step a), the volume ratio of water and ethanol is 1:(0.5～1.5), in mixed solution A, Bi source
Concentration be 0.8～1.2mol/L.
It is preferred that in step b), described alkali is alkali metal hydroxide.
It is preferred that in step c), the compactedness of reactor is less than 80%.
Accompanying drawing explanation
Fig. 1 a is the Bi prepared by embodiment 19O7.5S6Material morphology SEM schemes；
Fig. 1 b is the Bi prepared by embodiment 19O7.5S6Material high resolution scanning Electronic Speculum figure and SEAD image；
Fig. 2 is the Bi prepared by embodiment 19O7.5S6Material crystal structure schematic diagram；
Fig. 3 is the Bi prepared by embodiment 19O7.5S6Absorbed spectrogram；
Fig. 4 is the Bi prepared by embodiment 19O7.5S6Resistivity of material varies with temperature graph of a relation；
Fig. 5 is the Bi prepared by embodiment 19O7.5S6Material opto-electronic conversion graph of a relation.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
The present invention provides a kind of novel light absorbent, and its chemical formula is Bi9O7.5S6.Fig. 1 a illustrates one example of the present invention
Bi9O7.5S6The SEM figure of material, as it is shown in figure 1, this Bi9O7.5S6Material presents the hexagon of rule, and size exists
40～60 microns, such as 50 microns.Fig. 1 b illustrates the Bi of one example of the present invention9O7.5S6The high resolution scanning of material
Electronic Speculum figure and SEAD image.As shown in Figure 1 b, this Bi9O7.5S6Material be a space group be R3m rhombus
The crystal of structure, its cell parameter is:Fig. 2 illustrates
The Bi of one example of the present invention9O7.5S6The crystal structure schematic diagram of material, as in figure 2 it is shown, crystal structure is mainly by [BiS2]-Layer
[Bi2O2]2+Layer is alternately piled up along [001] direction and is formed obvious layer structure.This structure contains two unique Bi
Atom (Bi1, Bi2), a unique S atom and two unique O atom (O1, O2).Each Bi1 atom and 6
Individual S atom is coordinated, and forms a regular [BiS6] octahedra.Each Bi2 atom all with 4 O1 atoms and three and half
The O2 site occupied forms coordination, and a pair obvious lone pair electrons is arranged at each Bi2 atom top.Each O1 atom
All with 4 Bi2 Atomic coordinates form a tetrahedral structure.At Bi9O7.5S6In, Bi is+trivalent, and O is-divalent, S is-
Divalent.
The Bi of the present invention9O7.5S6Material has superior absorbing properties, good photoelectric transformation efficiency.Fig. 3 illustrates this
The Bi of one example of invention9O7.5S6The abosrption spectrogram of material, as it is shown on figure 3, its band gap is 1.27eV, meets solar energy
The optimal band gap of battery light absorbent.Fig. 4 illustrates the Bi of one example of the present invention9O7.5S6The resistivity of material varies with temperature pass
System's figure, it is known that this Bi9O7.5S6Material is typical semi-conducting material.Fig. 5 illustrates the Bi of one example of the present invention9O7.5S6Material
The opto-electronic conversion graph of a relation of material, under conditions of applied voltage is 1V, compared to 4.3 μ A/cm2Dark current density, photoelectricity
Current density is obviously improved, and has reached 9 μ A/cm2, the photoelectric conversion performance of its excellence is described.
The Bi of the present invention9O7.5S6Material can be prepared by hydro-thermal method.Specifically, as example, following step can be included
Suddenly.
By the reaction raw materials containing Bi, S according to mol ratio 1:(0.5～1.5) add and water and ethanol are mixed and stirred for uniformly,
Obtain mixed solution.Wherein, Bi source can be the soluble-salt of this element, such as Bi (NO3)2、BiCl3.S source is can be organic
Sulfide or sulfur simple substance, wherein organic sulfur compound for example, CN2H4S、CH3CH2SH.The volume ratio of water and ethanol can be 1:
(0.5～1.5).In the mixed solution obtained, the concentration in Bi source can be 0.8～1.2mol/L.
Adding alkali in above-mentioned mixed solution, make described solution basicity reach more than 5mol/L, stirring makes mixture uniformly mix
Close.The alkali used can be alkali metal hydroxide, such as, can be any one in alkali metal hydroxide, or any two
Plant above combination.
After said mixture is cooled to room temperature, it is transferred in reactor, preferably makes compactedness be less than 80%, at 433-
After 513K baking oven reacts 1-7 days, reactor is cooled to room temperature, and release.
Synthetic sample such as deionized water is cleaned, and in ultrasonic oscillator, carries out supersound process, obtain product.
Preferably, it is also possible to the product obtained is dried in 50-60 DEG C.In the preparation process in accordance with the present invention, can be the simplest
Ground regulation and control various process parameters, such as reaction temperature, response time, materials ratio, ultrasonic time etc., thus regulate and control the knot of product
Structure and performance.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
A) by reaction raw materials Bi (NO3)2And CN2H4S mixes according to mol ratio 1:1, and grinds uniformly in mortar；
B) above-mentioned mixed-powder is transferred in beaker, by volume 1:1, by H2O and CH3CH2On the mixed solution of OH adds
State in beaker, so that Bi (NO3)2Concentration be 1mol/L, mix homogeneously on magnetic stirring apparatus；
C) state 1:2 in mass ratio in mixed liquor directly up and add KOH and LiOH solid, make solution basicity reach more than 5M,
Mixture is made uniformly to mix under continuous stirring；
D) after said mixture is cooled to room temperature, being transferred in reactor, compactedness is less than 80%, in 433-513K baking oven
After reacting 1-7 days, reactor is cooled to room temperature, and release；
E) synthetic sample deionized water is cleaned, and in ultrasonic oscillator, carry out supersound process, obtain Lycoperdon polymorphum Vitt with metal light
The little granule crystal sample in pool, final sample is dried in 60 DEG C of baking ovens.
As seen in figure la and lb, the Bi gone out by water heat transfer9O7.5S5Sample, presents the hexagon of rule, chi
Very little at 50 microns.Single crystal X-ray diffraction test result display Bi9O7.5S sample be a space group be R-3m rhombus
The crystal of structure, its cell parameter is:Such as Fig. 2 institute
Show, Bi9O7.5The crystal structure of S sample is mainly by [BiS2]-Layer and [Bi2O2]2+Layer is alternately piled up along [001] direction and is formed substantially
Layer structure.This structure contains two unique Bi atoms (Bi1, Bi2), and a unique S atom and two are solely
Special O atom (O1, O2).Each Bi1 atom and 6 S atom coordinations, form a regular [BiS6] octahedra.
The O2 site that each Bi2 atom all occupies with 4 O1 atoms and three and half forms coordination, and each Bi2 atom top
There is a pair obvious lone pair electrons in portion.Each O1 atom and 4 Bi2 Atomic coordinates form a tetrahedral structure.Figure
3 show that the band gap of sample is 1.27eV, meet the optimal band gap of solaode light absorbent.Fig. 4 shows that this material is for typical case
Semi-conducting material.Fig. 5 then gives the photoresponse test result of this material, under conditions of applied voltage is 1V, compares
In 4.3 μ A/cm2Dark current density, density of photocurrent is obviously improved, and has reached 9 μ A/cm2, illustrate that it is excellent
Photoelectric conversion performance.
Embodiment 2
A) by reaction raw materials Bi (NO3)2And CN2H4S mixes according to mol ratio 1:1, and grinds uniformly in mortar；
B) above-mentioned mixed-powder is transferred in beaker, by volume 1:1, by H2O and CH3CH2On the mixed solution of OH adds
State in beaker, so that Bi (NO3)2Concentration be 1mol/L, mix homogeneously on magnetic stirring apparatus；
C) state addition KOH solid in mixed liquor directly up, make solution basicity reach more than 5M, make mixture under continuous stirring
Uniformly mixing；
D) after said mixture is cooled to room temperature, being transferred in reactor, compactedness is less than 80%, anti-in 433-513K baking oven
After answering 1-7 days, reactor is cooled to room temperature, and release；
E) synthetic sample deionized water is cleaned, and in ultrasonic oscillator, carry out supersound process, obtain Lycoperdon polymorphum Vitt with metal light
The little granule crystal sample in pool, final sample is dried in 60 DEG C of baking ovens.
Embodiment 3
A) by reaction raw materials Bi (NO3)2Mix according to mol ratio 1:1 with S, and grind uniformly in mortar；
B) above-mentioned mixed-powder is transferred in beaker, by volume 1:1, by H2O and CH3CH2On the mixed solution of OH adds
State in beaker, so that Bi (NO3)2Concentration be 1mol/L, mix homogeneously on magnetic stirring apparatus；
C) state 1:2 in mass ratio in mixed liquor directly up and add KOH and LiOH solid, make solution basicity reach more than 5M,
Mixture is made uniformly to mix under continuous stirring；
D) after said mixture is cooled to room temperature, being transferred in reactor, compactedness is less than 80%, anti-in 433-513K baking oven
After answering 1-7 days, reactor is cooled to room temperature, and release；
E) synthetic sample deionized water is cleaned, and in ultrasonic oscillator, carry out supersound process, obtain Lycoperdon polymorphum Vitt with metal light
The little granule crystal sample in pool, final sample is dried in 60 DEG C of baking ovens.
Embodiment 4
A) by reaction raw materials Bi (NO3)2Mix according to mol ratio 1:1 with S, and grind uniformly in mortar；
B) above-mentioned mixed-powder is transferred in beaker, by volume 1:1, by H2O and CH3CH2On the mixed solution of OH adds
State in beaker, so that Bi (NO3)2Concentration be 1mol/L, mix homogeneously on magnetic stirring apparatus；
C) state addition KOH solid in mixed liquor directly up, make solution basicity reach more than 5M, make mixture under continuous stirring
Uniformly mixing；
D) after said mixture is cooled to room temperature, being transferred in reactor, compactedness is less than 80%, anti-in 433-513K baking oven
After answering 1-7 days, reactor is cooled to room temperature, and release；
E) synthetic sample deionized water is cleaned, and in ultrasonic oscillator, carry out supersound process, obtain Lycoperdon polymorphum Vitt with metal light
The little granule crystal sample in pool, final sample is dried in 60 DEG C of baking ovens.
Embodiment 5
Prepare above-mentioned single-phase light absorbent Bi9O7.5S6Hydrothermal synthesis method, with specific reference to embodiment 1, difference be use
NaOH substitutes KOH.
Embodiment 6
Prepare above-mentioned single-phase light absorbent Bi9O7.5S6Hydrothermal synthesis method, with specific reference to embodiment 2, difference be use
NaOH substitutes KOH.
Embodiment 7
Prepare above-mentioned single-phase light absorbent Bi9O7.5S6Hydrothermal synthesis method, with specific reference to embodiment 3, difference be use
NaOH substitutes KOH.
Embodiment 8
Prepare above-mentioned single-phase light absorbent Bi9O7.5S6Hydrothermal synthesis method, with specific reference to embodiment 4, difference be use
NaOH substitutes KOH.
The invention provides a kind of stratiform single-phase light absorbent Bi9O7.5S6, invention also provides the special of this light absorbent
High temperature hydrothermal preparing process.This material is a kind of novel lamellar light absorbing material, and optical band gap is 1.27eV.This material has
Having superior absorbing properties, good photoelectric transformation efficiency, manufacture method is the most simple simultaneously, is beneficial to every ginseng
Number, has opto-electronic conversion field and has broad application prospects.
Claims (10)
1. a light absorbent, it is characterised in that described light absorbent be chemical formula be Bi9O7.5S6Single-phase compounds, described light absorbent has layer structure, and its structure is [BiS2 -] layer and [Bi2O2 2+] layer forms along the alternately accumulation of [001] direction, wherein Bi is+trivalent, and O is-divalent, and S is-divalent.
Light absorbent the most according to claim 1, it is characterised in that described light absorbent presents the hexagon of rule, and size is at 40～60 microns.
Light absorbent the most according to claim 1 and 2, it is characterised in that described light absorbent is that space group isR-3 mThe crystal of diamond structure, its cell parameter is:a= b=4.0685 (1),c=31.029 (5), V=444.83。
Light absorbent the most according to any one of claim 1 to 3, it is characterised in that the band gap of described light absorbent is 1.27eV.
Light absorbent the most according to any one of claim 1 to 4, it is characterised in that described light absorbent is under conditions of applied voltage is 1V, and density of photocurrent is more than the twice of dark current density.
6. the preparation method of the light absorbent according to any one of a claim 1 to 5, it is characterised in that comprise the following steps:
A) by Bi source, S source according to mol ratio 1:(0.5～1.5) add and water and ethanol are mixed and stirred for uniformly, obtain mixed solution A；
B) adding alkali in gained mixed solution A, make described mixed solution basicity reach more than 5mol/L, stirring makes mixture uniformly mix, obtains mixed solution B；
C) mixed solution B is transferred in reactor in 433～513K reaction 1～7 day, by synthetic product wash, ultrasonic, obtain described light absorbent.
Preparation method the most according to claim 6, it is characterised in that in step a), Bi source is the soluble-salt of Bi element, and S source is organic sulfur compound or sulfur simple substance.
8., according to the preparation method described in claim 6 or 7, it is characterised in that in step a), the volume ratio of water and ethanol is 1:(0.5～1.5), in mixed solution A, the concentration in Bi source is 0.8～1.2mol/L.
9., according to the preparation method according to any one of claim 6 to 8, it is characterised in that in step b), described alkali is alkali metal hydroxide.
10., according to the preparation method according to any one of claim 6 to 9, it is characterised in that in step c), the compactedness of reactor is less than 80%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888031A (en) * | 2019-03-04 | 2019-06-14 | 哈尔滨工业大学（深圳） | A kind of preparation method and photodetector of bismuth oxygen sulphur two-dimensional material |
| CN111943264A (en) * | 2020-06-12 | 2020-11-17 | 南京工业大学 | Preparation method and application of gilding nano flaky material with excellent photoelectric property |
| CN112588303A (en) * | 2020-11-23 | 2021-04-02 | 安徽大学 | Preparation method of selenium-bismuth oxide nanosheet and heterojunction type photoelectrode based on preparation method |
| CN113117702A (en) * | 2021-04-20 | 2021-07-16 | 济南大学 | Preparation and application of composite photocatalyst based on bismuth oxysulfide upconversion material |
| CN117263241A (en) * | 2023-09-19 | 2023-12-22 | 重庆工商大学 | Preparation method and application of bismuth oxysulfide ultrathin nanosheets |
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| CN103320089A (en) * | 2013-05-10 | 2013-09-25 | 张悦雯 | Nanometer light absorption material |
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| CN103320089A (en) * | 2013-05-10 | 2013-09-25 | 张悦雯 | Nanometer light absorption material |
Non-Patent Citations (1)
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| SHA MENG ET AL.: ""Synthesis，crystal structure，and photoelectric properties of a new layered bismuth oxysulfide"", 《INORGANIC CHEMISTRY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888031A (en) * | 2019-03-04 | 2019-06-14 | 哈尔滨工业大学（深圳） | A kind of preparation method and photodetector of bismuth oxygen sulphur two-dimensional material |
| CN111943264A (en) * | 2020-06-12 | 2020-11-17 | 南京工业大学 | Preparation method and application of gilding nano flaky material with excellent photoelectric property |
| CN111943264B (en) * | 2020-06-12 | 2023-07-14 | 南京工业大学 | Preparation method and application of gilded nano sheet material with excellent photoelectric property |
| CN112588303A (en) * | 2020-11-23 | 2021-04-02 | 安徽大学 | Preparation method of selenium-bismuth oxide nanosheet and heterojunction type photoelectrode based on preparation method |
| CN113117702A (en) * | 2021-04-20 | 2021-07-16 | 济南大学 | Preparation and application of composite photocatalyst based on bismuth oxysulfide upconversion material |
| CN117263241A (en) * | 2023-09-19 | 2023-12-22 | 重庆工商大学 | Preparation method and application of bismuth oxysulfide ultrathin nanosheets |
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