CN109052455A - A kind of preparation method of non-toxic stable perovskite - Google Patents
A kind of preparation method of non-toxic stable perovskite Download PDFInfo
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- CN109052455A CN109052455A CN201811181959.4A CN201811181959A CN109052455A CN 109052455 A CN109052455 A CN 109052455A CN 201811181959 A CN201811181959 A CN 201811181959A CN 109052455 A CN109052455 A CN 109052455A
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- C01G19/00—Compounds of tin
- C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
Abstract
Present invention discloses a kind of preparation methods of non-toxic stable perovskite, include the following steps, S1, weigh reaction raw materials, and reaction raw materials are put into heating reaction in organic solvent and are stirred 2 ~ 12 hours；S2, cleaning solvent is added into the reaction product of S1 and stands 3 ~ 5 minutes；S3, the reaction product of S2 is filtered, removes its solvent portions and obtains sediment, 3 ~ 5 cleanings then are carried out to sediment using cleaning solvent；S4, will be completed in S3 cleaning after sediment place with baking oven in dry 5 ~ 8 hours, obtain final product.Preparation method of the invention, which avoids, adds reactant in existing solution preparation at high temperature and prepares the operating procedure of precursor solution, not only simplifies reaction process, while also avoiding the special installation demand in solid reaction method and reaction atmosphere requirement.
Description
Technical field
The present invention relates to a kind of preparation methods of perovskite, in particular to a kind of nothing applied to solar battery
Poison stablizes the preparation method of perovskite, belongs to field of photoelectric technology.
Background technique
Over the past decades, the development of perovskite is made remarkable achievements, currently, the electricity of the perovskite based on lead
Pond device efficiency has been over 20%.However, the toxicity of the perovskite material in traditional technology based on lead greatlys restrict it
Further commercial applications are therefore, extremely urgent for the research of nontoxic perovskite material.
In recent years, it is based on Sn2+Perovskite because of its green non-poisonous characteristic, obtained the favor of numerous researchers.Currently,
People successfully prepare based on Sn2+Solar cell device.Shao et al. studied based on FASnI3Perovskite electricity
Pond device photoelectric transformation efficiency can achieve 9%.Meanwhile being based on Sn2+Full-inorganic perovskite CsSnI3Also it successfully answers
For in photovoltaic device and having obtained 4.8% incident photon-to-electron conversion efficiency.Although being based on Sn compared with lead-based perovskite2+Calcium titanium
Mine avoids influence of the toxicity to people on to greatest extent, but its characteristic is more unstable, in air, Sn2+Have by
It is oxidized into Sn4+Trend, this greatly limits Sn2+The application of perovskite in actual production.Therefore, for nontoxic steady
The production preparation and application study of fixed novel perovskite material become the new trend developed at present.
In newest research, one kind being based on Sn4+Novel perovskite material C s2SnAxB6-x(wherein A, B be halogen, 0
≤ x≤6) concern of people has been obtained, it is many excellent that this novel perovskite has non-toxic stable, narrow band gap, absorption coefficient height etc.
Point.In existing result of study, Cs2SnAxB6-xSuccessfully it is applied to plane joint solar cell as light absorbing material
In mesoporous type perovskite battery, and obtain respectively nearly 1% incident photon-to-electron conversion efficiency.Meanwhile studies have shown that Cs2SnAxB6-x
It is also equipped with good hole transport performance, hole mobile material is can be used as and is applied in solid-state dye sensitized battery, to keep away
Exempt from electrolyte in liquid dye sensitized cells and encapsulates problem caused by existing to the corrosion of battery and because of liquid electrolyte.Except this it
Outside, researcher is also to Cs2SnAxB6-xHomologue carried out exploratory development, main includes replacing Sn to synthesize phase with Ag, Te etc.
The perovskite material of pass has simultaneously carried out exploratory development to its photoelectric properties.This series of results shows this novel perovskite material
Prepared by the production of material and application study has extremely important meaning to the development of non-toxic stable solar battery of new generation.
In Cs2SnAxB6-xProduction prepare aspect, the preparation method reported at present mainly includes solid reaction method and molten
Liquid reaction method.Solid reaction method not only needs up to 400 DEG C of high temperature, but also needs special equipment to guarantee high vacuum environment
Or inert gas atmosphere, it is unfavorable for large-scale production.In terms of solution reaction method, Sn is usually used4+Or Sn2+Solution
As the source Sn (Sn2+Solution is first oxidized to Sn4+Solution), be halogen with CsA(A) solution reaction generation target product.On although
Operating method and uncomplicated is stated, but in experiment is attempted, researcher has been also found that shortcoming present in the above method.
For example it needs that initial reactant is added at a high temperature of 120 DEG C in these preparation methods, or need first to prepare precursor solution
To carry out next step reaction, these all bring biggish limitation to preparation process, therefore above-mentioned solid reaction method or solution are anti-
Ying Fajun is unfavorable for this non-toxic stable perovskite Cs2SnAxB6-xLarge-scale production and preparation, to influence it in solar-electricity
Further applying in pond.
In conclusion how to propose a kind of new non-toxic stable perovskite Cs on the basis of existing technology2SnAxB6-x's
Preparation method simplifies reaction method as much as possible, overcomes the various restrictive conditions in preparation process, also just becomes technology in the industry
The new research direction of personnel.
Summary of the invention
In view of the prior art there are drawbacks described above, the invention proposes a kind of preparation method of non-toxic stable perovskite,
Preparation route is as follows,
,
Wherein, A, B are any halogen atom, and m, n, l, x, y, z are constant more than or equal to 0, and m and n are not simultaneously 0, l and
X is not 0 simultaneously；
X is the arbitrary constant in section [0,6]；
When x is 0, reaction equation is,
, or
,
Preparation method includes the following steps,
S1, reaction raw materials are weighed, and reaction raw materials is put into heating reaction in organic solvent and are stirred 2 ~ 12 hours；
S2, cleaning solvent is added into the reaction product of S1 and stands 3 ~ 5 minutes；
S3, the reaction product of S2 is filtered, removes its solvent portions and obtains sediment, then using cleaning solvent to precipitating
Object carries out 3 ~ 5 cleanings；
S4, will be completed in S3 cleaning after sediment place with baking oven in dry 5 ~ 8 hours, obtain final product.
Preferably, in S1, after weighing reaction raw materials, first reaction raw materials are dissolved separately in organic solvent, then again
It is mixed and heated reaction.
Preferably, in S1, after weighing reaction raw materials, any two or more in reaction raw materials are mixed, with
After will be dissolved in organic solvent and heat reaction.
Preferably, organic solvent described in S1 is 1,4-butyrolactone.
Preferably, reaction raw materials are put into heat in organic solvent described in S1 and is reacted, reaction temperature is 25 ~ 220 DEG C.
Preferably, reaction raw materials are put into heat in organic solvent described in S1 and is reacted, reaction temperature is 70 DEG C.
Preferably, cleaning solvent described in S2 and S3 is alcohol organic solvent.
Preferably, cleaning solvent described in S2 and S3 is ethyl alcohol.
Compared with prior art, advantages of the present invention is mainly reflected in the following aspects:
Cs provided by the present invention2SnAxB6-xThe novel solutions preparation method of (A, B are halogen) avoids existing solution preparation
In add reactant at high temperature and prepare the operating procedure of precursor solution, not only simplify reaction process, while also avoiding
Special device requirement and reaction atmosphere requirement in solid reaction method, preparation method integrated operation is simple, can directly apply
During large-scale production and preparation, there is huge potential using value.
In addition, the present invention also provides reference for other relevant issues in same domain, can be opened up on this basis
Extension is stretched, and is applied in the technical solution of other preparation methods same domain Nei, has very wide application prospect.
Just attached drawing in conjunction with the embodiments below, the embodiment of the present invention is described in further detail, so that of the invention
Technical solution is more readily understood, grasps.
Detailed description of the invention
It using 1,4-butyrolactone (GBL) and n,N-Dimethylformamide be respectively to react that Fig. 1, which is in the embodiment of the present invention 1,
Cs prepared by solvent2SnI6XRD characterization figure；
Fig. 2 is in the embodiment of the present invention 1 using the EDS phenogram that GBL is Cs2SnI6 prepared by solvent；
Fig. 3 is the XRD characterization figure of the Cs2SnBr6 prepared in the embodiment of the present invention 2；
Fig. 4 is the XRD characterization figure of the Cs2SnBr3I3 prepared in the embodiment of the present invention 3.
Specific embodiment
Present invention discloses a kind of preparation method of non-toxic stable perovskite,
Preparation route is as follows,
Wherein, A, B are any halogen atom, and m, n, l, x, y, z are the arbitrary constant more than or equal to 0, and M and N are not simultaneously
0, L and X is not 0 simultaneously；X is the arbitrary constant between 0 ~ 6, herein includes 0 and 6 two constant.Particularly, when x is 0, instead
Answer formula are as follows:
,
Or
,
Preparation method includes the following steps,
S1, reaction raw materials are weighed, and reaction raw materials is put into heating reaction in organic solvent and are stirred 2 ~ 12 hours.It is described organic
Solvent is 1,4-butyrolactone (GBL), and very pure target product can be obtained using this organic solvent.Reaction temperature be 25 ~
220 DEG C, in the present embodiment, preferred reaction temperature is 70 DEG C.
S2, cleaning solvent is added into the reaction product of S1 and stands 3 ~ 5 minutes.
S3, the reaction product of S2 is filtered, removes its solvent portions and obtains sediment, then use cleaning solvent pair
Sediment carries out 3 ~ 5 cleanings.The cleaning solvent is alcohol organic solvent, in the present embodiment, preferably ethyl alcohol.
S4, will be completed in S3 cleaning after sediment place with baking oven in dry 5 ~ 8 hours, obtain final product.
It, can be there are two types of mode of operation, first, can first distinguish reaction raw materials molten after weighing reaction raw materials in S1
Solution is then mixed and heated reaction in organic solvent again.Second, can by reaction raw materials it is any two or more
It is mixed, will be then dissolved in organic solvent and heats reaction.
Above-mentioned technical proposal is specifically described below in conjunction with specific embodiment.
Embodiment 1:Cs2SnI6Synthesis
The CsI of 1.036g, the SnI of 0.744g are weighed respectively2, the I of 0.508g2, take 5 ml organic solvent 1,4-butyrolactone (GBL)
Or n,N-Dimethylformamide (DMF), it sequentially adds in the 10 ml reaction flasks containing magneton and forms mixed solution.It will mixing
Solution is placed on magnetic force hot plate and is stirred to react at 70 DEG C, stops reaction after 10 hours, and it is quiet that dehydrated alcohol is added into reaction flask
It sets 3-5 minutes, then removes to obtain black precipitate by reaction flask middle and upper part solvent portions, next reuse dehydrated alcohol pair
Precipitating cleaning 3-5 times, is placed in 70 DEG C of drying in baking oven for precipitating after the completion of cleaning and obtains final product in 5-8 hours.Attached drawing 1
Phenogram is tested for the XRD of products therefrom when to use GBL and DMF be reaction dissolvent, dotted line is simulation Cs in figure2SnI6Data.
When the use of GBL being reaction dissolvent, product X RD diffraction maximum and simulation Cs2SnI6Data peak is completely coincident, and impurity peaks are not deposited
?；When the use of DMF being reaction dissolvent, there is the diffraction maximum of CsI in the XRD test phenogram of products therefrom, i.e., in product
There is CsI impurity.The EDS of products therefrom tests phenogram when attached drawing 2 is is reaction dissolvent using GBL, wherein product atom
Number ratio Cs:Sn:I=20.98:12.75:66.27, substantially conforms to Cs2SnI6In atom number ratio, it was demonstrated that product has very high
Purity.
Embodiment 2:Cs2SnBr6Synthesis
The CsBr of 0.85g, the SnBr of 1.11g are weighed respectively2, 5ml organic solvent 1,4-butyrolactone is measured, is sequentially added containing magnetic
Mixed solution is formed in 10 ml reaction flasks of son.Mixed solution is placed on magnetic force hot plate at 70 DEG C and is stirred to react, 10 is small
When after stop reaction, into reaction flask be added dehydrated alcohol stand 3-5 minute, then by reaction flask middle and upper part solvent portions removing
Sediment is obtained, dehydrated alcohol is next reused to precipitating cleaning 3-5 times, precipitating is placed in 70 in baking oven after the completion of cleaning
DEG C drying obtains final product in 5-8 hours.Attached drawing 3 is that the XRD of product tests phenogram, and dotted line is simulation Cs in figure2SnBr6
Data, product X RD diffraction maximum and simulation Cs2SnBr6Data peak is overlapped.The above results show as use CsBr and SnBr2It is anti-
Raw material is answered, when GBL is reaction dissolvent, available target product Cs2SnBr6。
Embodiment 3:Cs2SnBr3I3Synthesis
The CsI of 0.1170 g, the SnI of 0.1007 g are weighed respectively2, the SnBr of 0.0376 g2, 0.5 ml organic solvent 1 is measured,
4- butyrolactone sequentially adds in the 5 ml reaction flasks containing magneton and forms mixed solution.Mixed solution is placed on magnetic force hot plate
It is stirred to react at 70 DEG C, stops reaction after 10 hours, dehydrated alcohol is added into reaction flask and stands 3-5 minutes, it then will be anti-
It answers a bottle middle and upper part solvent portions to remove to obtain sediment, next reuses dehydrated alcohol to precipitating cleaning 3-5 times, cleaning is completed
Precipitating is placed in 70 DEG C of drying in baking oven afterwards and obtains final product within 5-8 hours.Attached drawing 4 is that the XRD of product tests phenogram,
Dotted line is simulation Cs in figure2SnBr3I3Data, product X RD diffraction maximum and simulation Cs2SnBr3I3Data peak is overlapped.The above results
Show when according to a certain percentage use CsI, SnI2And SnBr2For reaction raw materials, when GBL is reaction dissolvent, available target
Product Cs2SnBr3I3。
Cs provided by the present invention2SnAxB6-xThe novel solutions preparation method of (A, B are halogen, 0≤x≤6) avoids existing
Have and add reactant at high temperature in solution preparation and prepare the operating procedure of precursor solution, not only simplifies reaction work
Skill, while the special device requirement in solid reaction method and reaction atmosphere requirement are also avoided, preparation method integrated operation letter
It is single, during may be directly applied to large-scale production and preparation, there is huge potential using value.
In addition, the present invention also provides reference for other relevant issues in same domain, can be opened up on this basis
Extension is stretched, and is applied in the technical solution of other preparation methods same domain Nei, has very wide application prospect.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit and essential characteristics of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention, and any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of preparation method of non-toxic stable perovskite, it is characterised in that:
Preparation route is as follows,
,
Wherein, A, B are any halogen atom, and m, n, l, x, y, z are the constant more than or equal to 0, and m and n are not 0, l and x simultaneously
It is not simultaneously 0；
X is the arbitrary constant in section [0,6]；
When x is 0, reaction equation is,
, or
,
Preparation method includes the following steps,
S1, reaction raw materials are weighed, and reaction raw materials is put into heating reaction in organic solvent and are stirred 2 ~ 12 hours；
S2, cleaning solvent is added into the reaction product of S1 and stands 3 ~ 5 minutes；
S3, the reaction product of S2 is filtered, removes its solvent portions and obtains sediment, then using cleaning solvent to precipitating
Object carries out 3 ~ 5 cleanings；
S4, will be completed in S3 cleaning after sediment place with baking oven in dry 5 ~ 8 hours, obtain final product.
2. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: in S1, weigh
After reaction raw materials, first reaction raw materials are dissolved separately in organic solvent, are then mixed and heated reaction again.
3. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: in S1, weigh
After reaction raw materials, any two or more in reaction raw materials are mixed, will then be dissolved in organic solvent and heat
Reaction.
4. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: organic described in S1
Solvent is 1,4-butyrolactone.
5. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: will be anti-described in S1
It answers and heats reaction in raw material investment organic solvent, reaction temperature is 25 ~ 220 DEG C.
6. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: will be anti-described in S1
It answers and heats reaction in raw material investment organic solvent, reaction temperature is 70 DEG C.
7. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: described in S2 and S3
Cleaning solvent be alcohol organic solvent.
8. a kind of preparation method of non-toxic stable perovskite according to claim 1, it is characterised in that: described in S2 and S3
Cleaning solvent be ethyl alcohol.
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