CN110195252A - A kind of method of layer of solution growth perovskite monocrystalline - Google Patents
A kind of method of layer of solution growth perovskite monocrystalline Download PDFInfo
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- CN110195252A CN110195252A CN201910614086.XA CN201910614086A CN110195252A CN 110195252 A CN110195252 A CN 110195252A CN 201910614086 A CN201910614086 A CN 201910614086A CN 110195252 A CN110195252 A CN 110195252A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The present invention provides the methods of a kind of layer of solution growth perovskite monocrystalline, belong to perovskite material single crystal technology field.The frost zone that the present invention passes through addition solution A or solution B between solution A and solution B, the mixing rate of solution A layer Yu solution B layer can be slowed down, and the heat of two layers of solution reaction releasing can be frozen layer and be offset, so that the reaction between two layers of solution is gentler, keep crystal nucleation more steady with growth course, gained perovskite single crystal size is big after stationary culture, quality is high, monocrystalline plane of crystal is more smooth.And method provided by the invention is easy to operate, do not need accurate growth apparatus, requires experimental situation low, low in cost, has wider array of universality for the preparation of monocrystalline.Embodiment the result shows that, for the perovskite monocrystalline length obtained using the method for the present invention up to 0.5~2cm, crystal structure degree is good.
Description
Technical field
The present invention relates to perovskite material single crystal technology field, in particular to a kind of layer of solution growth perovskite monocrystalline
Method.
Background technique
Perovskite is a kind of with ABX3The material of class compound structure.In recent years, perovskite material photoelectric conversion,
The fields such as electroluminescent, detector, ferroelectricity also have a wide range of applications in life by the concern of researchers.However it is worth
It must be concerned with, the perovskite material for being studied and applying is largely block materials and thin-film material, internal crystal boundary,
Defect is more, this is unfavorable for the crystal structure of research material, while this also reduces material property, reduced service life.
In order to further increase the performance of perovskite material, monocrystal material is more of interest by people.Monocrystal material is compared
There is no internal flaw for thin-film material or block materials, is the best object for characterizing crystal structure；And monocrystal material
Service life, performance etc. are significantly promoted compared to the material of other forms, such as perovskite single crystal battery, efficiency are more than
18%；Perovskite monocrystalline detector, with extensive detection performance, detectable X-ray, gamma-rays, visible light etc..
Although perovskite monocrystal material has been widely studied and has applied, the growth success rate of monocrystalline is low, and preparation is very
It is difficult.In recent years, the synthetic method of perovskite monocrystalline mainly has slow evaporation method, inversion degree growth method, anti-solvent evaporation auxiliary
Method, top-seeded flux method, bottom seed crystallization method, falling temperature method, Bridgman method and Solvothermal etc..However often at present
The above method requires harshness to experimental situation, needs to carry out strict temperature control, operating procedure is complicated, crystal growth
Success rate is low, and obtained monocrystalline quality is low, size is small.
Summary of the invention
In view of this, it is an object of that present invention to provide the methods of a kind of layer of solution growth perovskite monocrystalline.The present invention mentions
The method of confession is easy to operate, requires low, crystal growth success rate high experimental situation, and gained monocrystalline better crystallinity degree, size be big, matter
Amount is high.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides the methods of a kind of layer of solution growth perovskite monocrystalline, comprising the following steps:
Frost zone, the solution A of solution B, solution A or solution B are sequentially added in crystal growth vessel, after stationary culture
To perovskite monocrystalline；The general structure of the perovskite is AaBbXn, wherein a:b:n=(0.5~3:0.5~3:3~9)；It is described
Solution A is to provide the precursor solution of A ion and/or X ion in perovskite；The solution B is to provide B ion in perovskite
And/or the precursor solution of X ion；At least one in the solution A and solution B includes X ion.
Preferably, the solution A is halides solution, and the general structure of the halides is MXn, wherein M be Cu, Ge,
One of Bi, Sn, Pb, Cs, Rb, Fe, Co, Ni, Cd, Hg, Mn and Ti；X is one or more of F, Cl, Br and I；N=0
~6；
Or the halides be CHNHBr, HN-CH=NHBr, (CH) NBr, CHNHI, HN-CH=NHI, (CH) NI,
One or more of CHNHCl, HN-CH=NHCl and (CH) NCl；
The solvent of the halides solution is hydrobromic acid, hydroiodic acid, hydrochloric acid, gamma-butyrolacton, N, N- dimethyl formyl
It is one or more of in amine, dimethyl sulfoxide and n-methyl-2-pyrrolidone；The molar concentration of the solution A is 0.01~6mol/
L。
Preferably, the general structure of the solute of the solution B is CXn, wherein C is CH6N、C2H8N、C3H10N、C4H12N、
C6H8N、C7H10N、C8H12N、C9H14N、C10H16N and HC (NH2)2One or more of I；X be one of F, Cl, Br and I or
It is several；N=0~6；
The solvent of solution B is hydrobromic acid, hydroiodic acid, hydrochloric acid, gamma-butyrolacton, N,N-dimethylformamide, dimethyl Asia
One or more of sulfone and n-methyl-2-pyrrolidone, the molar concentration of the solution B are 0.01~6mol/L.
Preferably, the addition rate of the solution B and solution A independently is 0.01~10mL/min.
Preferably, the crystal growth vessel is elongated tubular container；The internal diameter of the crystal growth vessel be 0.05~
50cm；The inner wall material of the crystal growth vessel is glass or polytetrafluoroethylene (PTFE).
Preferably, the addition height of the solution A and solution B in crystal growth vessel independently is 0.01~10cm.
Preferably, the frost zone shape of the solution A or solution B is cylindric；The frost zone with a thickness of 0.01~
10cm, diameter are identical as the internal diameter of crystal growth vessel.
Preferably, the temperature of the frost zone is -50~20 DEG C.
Preferably, the environment temperature of the stationary culture is -50~150 DEG C, and the time is 1~60 day.
The present invention provides the method for a kind of layer of solution growth perovskite monocrystalline, the present invention passes through in solution A and solution B
Between the frost zone of solution A or solution B is added, the mixing rate of solution A layer Yu solution B layer can be slowed down, and two layers of solution is anti-
The heat that should be released can be frozen layer and be offset so that the reaction between two layers of solution is gentler, make crystal nucleation with
Growth course is more steady, and gained perovskite single crystal size is big after stationary culture, quality is high, monocrystalline plane of crystal is more smooth.
And method provided by the invention is easy to operate, do not need accurate growth apparatus, experimental situation is required it is low, low in cost, it is right
There is wider array of universality in the preparation of monocrystalline.Embodiment the result shows that, the perovskite monocrystalline obtained using the method for the present invention is long
It spends up to 0.5~2cm, crystal structure degree is good, and crystalline quality is high.
Detailed description of the invention
Fig. 1 is perovskite single crystal growth process schematic diagram；
Fig. 2 is the pictorial diagram of 1 gained perovskite monocrystalline of embodiment；
Fig. 3 is the X diffracting spectrum of 1 gained perovskite monocrystalline of embodiment.
Specific embodiment
The present invention provides the methods of a kind of layer of solution growth perovskite monocrystalline, comprising the following steps:
Frost zone, the solution A of solution B, solution A or solution B are sequentially added in crystal growth vessel, after stationary culture
To perovskite monocrystalline；The general structure of the perovskite is AaBbXn, wherein a:b:n=(0.5~3:0.5~3:3~9)；It is described
Solution A is to provide the precursor solution of A ion and/or X ion in perovskite；The solution B is to provide B ion in perovskite
And/or the precursor solution of X ion；At least one in the solution A and solution B includes X ion.
In the present invention, the solution A is preferably halides solution, and the general structure of the halides is MXn, wherein M
Preferably one or more of Cu, Ge, Bi, Sn, Pb, Cs, Rb, Fe, Co, Ni, Cd, Hg, Mn and Ti；X is preferably F, Cl, Br
One or more of with I；N=0~6；Specifically, the halides are preferably bismuth iodide BiI3, bismuth chloride BiCl3, bismuth bromide
BiBr3, it is fluorinated bismuth BiF3, cupric iodide CuI2, copper chloride CuCl2, copper bromide CuBr2, copper fluoride CuF2, stannic iodide SnI2, chlorination
Tin SnCl2, stannic bromide SnBr2, tin fluoride SnF2, lead iodide PbI2, lead chloride PbCl2, lead bromide PbBr2, lead fluoride PbF2, iodine
Change germanium GeI2, germanium chloride GeCl2, bromination germanium GeBr2, it is fluorinated germanium GeF2One or more of；
Or the halides are preferably bromine methylamine CHNHBr, bromine carbonamidine HN-CH=NHBr, bromination tetramethylammonium (CH) NBr, iodine
Methylamine CHNHI, iodine carbonamidine HN-CH=NHI, iodate tetramethylammonium (CH) NI, chloromethane amine CHNHCl, chloromethane amidine HN-CH=NHCl and
One or more of tetramethylamine chloride (CH) NCl；
The solvent of the halides solution is preferably hydrobromic acid, hydroiodic acid, hydrochloric acid, gamma-butyrolacton, N, N- dimethyl methyl
It is one or more of in amide, dimethyl sulfoxide and n-methyl-2-pyrrolidone；The molar concentration of the solution A is preferably 0.01
~6mol/L, more preferably 1~3mol/L.
In the present invention, the general structure of the solute of the solution B is CXn, wherein C is methyl amine group CH6N, ethylamine
Group C2H8N, propyl amine groups C3H10N, butylamine group C4H12N, phenyl amine groups C6H8N, benzylamino rolls into a ball C7H10N, benzene
Ethyl amine groups C8H12N, phenylpropyl amine groups C9H14N, benzene butylamine group C10H16N and carbonamidine group HC (NH2)2One in I
Kind is several；X is one or more of F, Cl, Br and I；N=0~6；
The solvent of the solution B is hydrobromic acid, hydroiodic acid, hydrochloric acid, gamma-butyrolacton, N,N-dimethylformamide, diformazan
One or more of base sulfoxide and n-methyl-2-pyrrolidone, the molar concentration of the solution B are preferably 0.01~6mol/
L, more preferably 1~3mol/L；The preferably dropwise addition of the adding manner of the solution B and solution A, the solution B and solution A add
Entering rate is independently preferably 0.01~10mL/min, more preferably 0.2~2mL/min.
In the present invention, the crystal growth vessel is preferably elongated tubular container；The internal diameter of the crystal growth vessel
Preferably 0.05~50cm, more preferably 0.5~20cm；The highly preferred of the crystal growth vessel is greater than solution B, solution A
Or total height of the frost zone, solution A of solution B in crystal growth vessel；The choosing of fine quality of the inner wall material of the crystal growth vessel
For glass or polytetrafluoroethylene (PTFE)；The present invention, can be to avoid inner tubal wall by selection glass or the inner tubal wall of polytetrafluoroethylene (PTFE) material
It reacts with solution.In the present invention, the inner tubal wall of the crystal growth vessel needs smooth, under an optical microscope without obvious
Scratch, it is brilliant if inner wall scratch is too many because the scratch of container inner wall, which can provide one for the growth forming core of crystal, depends on place
Body will be skewed towards in small and broken.
In the present invention, highly preferred in crystal growth vessel of the solution A is 0.01~10cm, more preferably
0.1~6cm；Height of the solution B in crystal growth vessel is 0.01~10cm, more preferably 0.1~6cm.The present invention
By controlling the height of solution A and solution B, can effectively control solution A and the mixing diffusion rate of solution B, react exoergic,
Crystal nucleation and growth course.
In the present invention, the frost zone of the solution A or solution B is preferably shaped to cylindric；The thickness of the frost zone
Preferably 0.01~10cm, more preferably 0.1~3cm；The diameter of the frost zone preferably with the internal diameter phase of crystal growth vessel
Together.In the present invention, the temperature of the frost zone is preferably -50~20 DEG C, more preferably -30~10 DEG C.In the present invention, when
When the temperature of the frost zone is greater than 0 DEG C, the present invention preferably makes liquid be converted into solid by way of high pressure compressed.In this hair
In bright, the environment temperature of the stationary culture is preferably -50~150 DEG C, more preferably -20~100 DEG C；The stationary culture
Time is preferably 1~60 day, and more preferably 7~14 days.
Perovskite single crystal growth process schematic diagram of the present invention is as shown in Figure 1, the present invention passes through in solution A and solution B
Between the frost zone of solution A or solution B is added, the mixing rate of solution A layer Yu solution B layer can be slowed down, and two layers of solution is anti-
The heat that should be released can also be frozen layer and be offset, so that the reaction between two layers of solution is gentler, make crystal nucleation
More steady with growth course, gained perovskite single crystal size is big after stationary culture, quality is high, monocrystalline plane of crystal is more flat
It is whole.In addition, the frost zone of thawing is also used as solution A or the reaction of solution B is former while frost zone provides cooling effect
Material.
It is carried out specifically below with reference to method of the embodiment to layer solution growth perovskite monocrystalline provided by the invention
It is bright, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Solution B (the BiI of 3cm is sequentially added in the glass crystal growing container that internal diameter is 10mm3HI solution, 1mol/
L), the frost zone (temperature be -20 DEG C), 3cm of the solution B of 1cm solution A (ethanol solution of PhAI (benzyl ammonium iodide),
1mol/L), wherein solution A, the drop rate of B are 1mL/min, obtain perovskite after stationary culture 10 days under conditions of 25 DEG C
Monocrystalline PhABiI3, the pictorial diagram of gained perovskite monocrystalline is as shown in Figure 2.
As shown in Figure 2, the size of perovskite monocrystalline obtained by the method for the present invention is 1.1cm, and crystallinity is good, crystalline quality
It is high.
X-ray diffraction is carried out to gained perovskite monocrystalline, acquired results are as shown in Figure 3.From the figure 3, it may be seen that XRD diffracting spectrum
In only there are three apparent characteristic peak, and certain rule is distributed in three peaks, it is clear that is that a crystal difference crystal face is corresponding
Diffraction maximum, illustrate that test material is mono-crystalline structures.
Embodiment 2
Solution B (the C of 2cm is sequentially added in the polytetrafluoroethylene (PTFE) crystal growth vessel that internal diameter is 10cm4H12BrN (tetramethyl
Base ammonium bromide) DMF solution, 1mol/L), the frost zone (temperature is 10 DEG C) of the solution B of 0.5cm, 4cm solution A (CuBr2
The hydrobromic acid solution of (copper bromide), 1mol/L), wherein solution A, the drop rate of B are 0.2mL/min, under conditions of -20 DEG C
Stationary culture obtains perovskite monocrystalline [C after 30 days4H12N]2CuBr4。
Embodiment 3
Solution B (the C of 2cm is sequentially added in the polytetrafluoroethylene (PTFE) crystal growth vessel that internal diameter is 20cm4H12IN (tetramethyl
Base ammonium iodide) DMF solution, 1mol/L), the frost zone (temperature is 0 DEG C) of the solution B of 0.1cm, 1cm solution A (CuI2(iodine
Changeization copper) DMF solution, 1mol/L), wherein solution A, the drop rate of B be 2mL/min, under conditions of 100 DEG C stand training
Perovskite monocrystalline [C is obtained after supporting 20 days4H12N]2CuI4。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. the method for a kind of layer of solution growth perovskite monocrystalline, which comprises the following steps:
Frost zone, the solution A of solution B, solution A or solution B are sequentially added in crystal growth vessel, obtain calcium after stationary culture
Titanium ore monocrystalline；The general structure of the perovskite is AaBbXn, wherein a:b:n=(0.5~3:0.5~3:3~9)；The solution
A is to provide the precursor solution of A ion and/or X ion in perovskite；The solution B is to provide B ion and/or X in perovskite
The precursor solution of ion；At least one in the solution A and solution B includes X ion.
2. the method according to claim 1, wherein the solution A is halides solution, the knot of the halides
Structure general formula is MXn, wherein M is one or more of Cu, Ge, Bi, Sn, Pb, Cs, Rb, Fe, Co, Ni, Cd, Hg, Mn and Ti；X
For one or more of F, Cl, Br and I；N=0~6；
Or the halides be CHNHBr, HN-CH=NHBr, (CH) NBr, CHNHI, HN-CH=NHI, (CH) NI, CHNHCl,
One or more of HN-CH=NHCl and (CH) NCl；
The solvent of the halides solution is hydrobromic acid, hydroiodic acid, hydrochloric acid, gamma-butyrolacton, N,N-dimethylformamide, two
It is one or more of in methyl sulfoxide and n-methyl-2-pyrrolidone；The molar concentration of the solution A is 0.01~6mol/L.
3. the method according to claim 1, wherein the general structure of the solute of the solution B is CXn, wherein C
For CH6N、C2H8N、C3H10N、C4H12N、C6H8N、C7H10N、C8H12N、C9H14N、C10H16N and HC (NH2)2One of I or several
Kind；X is one or more of F, Cl, Br and I；N=0~6；
The solvent of solution B be hydrobromic acid, hydroiodic acid, hydrochloric acid, gamma-butyrolacton, N,N-dimethylformamide, dimethyl sulfoxide and
One or more of n-methyl-2-pyrrolidone, the molar concentration of the solution B are 0.01~6mol/L.
4. the method according to claim 1, wherein the addition rate of the solution B and solution A independently is
0.01~10mL/min.
5. the method according to claim 1, wherein the crystal growth vessel is elongated tubular container；It is described
The internal diameter of crystal growth vessel is 0.05~50cm；The inner wall material of the crystal growth vessel is glass or polytetrafluoroethylene (PTFE).
6. the method according to claim 1, wherein the solution A and solution B adding in crystal growth vessel
Enter height and independently is 0.01~10cm.
7. the method according to claim 1, wherein the frost zone shape of the solution A or solution B is cylinder
Shape；The frost zone with a thickness of 0.01~10cm, diameter is identical as the internal diameter of crystal growth vessel.
8. method according to claim 1 or claim 7, which is characterized in that the temperature of the frost zone is -50~20 DEG C.
9. the method according to claim 1, wherein the environment temperature of the stationary culture be -50~150 DEG C,
Time is 1~60 day.
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| CN114150363A (en) * | 2021-12-13 | 2022-03-08 | 吉林大学 | Growth method of tin-based perovskite single crystal |
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