CN108300470A - A kind of preparation method of quasi- low-dimensional bismuthino perovskite nano material - Google Patents
A kind of preparation method of quasi- low-dimensional bismuthino perovskite nano material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of quasi- low-dimensional bismuthino perovskite nano material, and this method comprises the following steps：Using quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder be raw material, amine obtains mixture as remover, and using solvent；Then, the mixture is handled using cell disruptor, then centrifuged, it is MA to take supernatant to obtain chemical formula3Bi2X9Nano material.The present invention is improved by the Parameter Conditions etc. to crucial preparation method integral process flow design, each step, strong energy is given especially with cell disruptor to split quasi- low-dimensional bismuthino perovskite material plus the release effect of amine, type and proportioning, the specific power of the crushing process and time etc. of raw material, the synthetic method complexity that can effectively solve the problem that bismuthino perovskite nano material compared with prior art, the problem that the concentration of obtained nano material colloidal solution is relatively low, yield is relatively low are reacted by control.
Description
Technical field
The invention belongs to field of photoelectric material preparation, more particularly, to a kind of quasi- low-dimensional bismuthino perovskite nano material
Preparation method.
Background technology
Perovskite nano material is being sent out because of the advantages that its high quantum yield, cheap cost, simple preparation method
Light display field has broad application prospects.
Perovskite nano material can to adjust its luminescent properties, (mainly shine wave using halogens and dimensional effect
It is long), therefore its luminescent spectrum can cover entire visible region (400-800nm), have great potentiality using upper in LED.But
At present to the research of perovskite nano material mainly for Pb bases, and Pb etc. is replaced because of fault in material concentration with novel non-toxic element
Excessively high or stability is worse and there are huge difficulty, only the Bi based perovskites quantum dot of ligand auxiliary reprecipitation and heat injection
The nontoxic perovskite of Sn bases of method preparation is nanocrystalline to have obtained a degree of trial, but because of its preparation process complexity, still needs into one
Step is improved.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the purpose of the present invention is to provide a kind of quasi- low-dimensional bismuthino calcium
The preparation method of titanium ore nano material, wherein passing through the ginseng to crucial preparation method integral process flow design, each step
Said conditions etc. are improved, especially with cell disruptor give strong energy plus amine release effect by quasi- low-dimensional bismuthino calcium titanium
Pit wood material is split, and reacts the type and proportionings of raw material, the specific power of crushing process and time etc. by control, and existing
The nano material colloidal solution that technology is compared and can effectively solve the problem that the synthetic method of bismuthino perovskite nano material is complicated, obtains
The problem that concentration is relatively low, yield is relatively low, this method, which can be realized from the powder or block materials of higher-dimension (such as 3 dimension), switchs to low-dimensional
Bismuthino perovskite nano material synthesis such as the nano material of (such as 0/1/2 dimension) " from high to low, from having nothing ", synthetic method
Simply, and the bismuthino perovskite nano ZnO that is prepared of this method is stablized, and has excellent performance.
To achieve the above object, it is proposed, according to the invention, provide a kind of preparation side of quasi- low-dimensional bismuthino perovskite nano material
Method, which is characterized in that include the following steps：Using quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder be raw material, amine conduct
Remover, and solvent is used, it obtains including the quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder, the amine and
The mixture of the solvent, wherein X are at least one of Cl, Br, I, the solvent can dissolve the remover and for
The solubility of the remover is more than to the quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Solubility；Then, cell powder is utilized
Broken machine handles the mixture, then centrifuges, and it is MA to take supernatant to obtain chemical formula3Bi2X9Quasi- low-dimensional bismuthino perovskite receive
Rice material.
As present invention further optimization, the quasi- low-dimensional bismuthino perovskite material MA as the raw material3Bi2X9
Powder substance amount ranging from 0.02~0.1mmol.
As present invention further optimization, the amine as the remover is in butylamine, n-octyl amine and oleyl amine
At least one；
The solvent is any one of normal octane, n-hexane, toluene and methanol/normal octane in the mixed solvent.
As present invention further optimization, in the mixture, the quasi- low-dimensional bismuthino perovskite material MA3Bi2X9's
The ratio of the amount of the substance of both powder, the amine is 1：15~62.5；
The quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder substance amount and the solvent volume ratio between two
For 0.04mmol:6ml~15ml.
Also include the oleic acid as ligand, the quasi- low-dimensional as present invention further optimization, in the mixture
Bismuthino perovskite material MA3Bi2X9Powder and both the oleic acid substance amount ratio be 1:37.5~75.
As present invention further optimization, the cell disruptor handles the mixture, is in 200W~400W
It is handled 30~60 minutes under power, the operative duty cycles of cell disruptor are 1/3~1/2, and the continuous ultrasound time is 1 second.
Contemplated above technical scheme through the invention (is especially matched by using comminuting method compared with prior art
Body assisted comminution method) novel synthesis of this " from high to low, from having nothing " synthesizes environmentally protective, high-fluorescence quantum yield
MA3Bi2X9Perovskite nano material, the synthetic method that on the one hand can solve bismuthino perovskite nano material in the prior art are multiple
Miscellaneous problem, on the other hand can also overcome that the concentration of nano material colloidal solution obtained by the prior art is relatively low, yield is more low
Defect, the present invention is of great significance to novel semi-conductor nano ZnO and luminescence research.
The process that the forming core that existing perovskite nano material synthetic method is " from scratch " is grown up again, and main needle
To Pb based perovskite materials.And relative to Pb based perovskites, Bi based perovskites are not only environmentally friendly, and subject to low-dimensional
Material, i.e., octahedra frame is low dimensional structures, and MA+(the low-dimensional material of quasi- low-dimensional materials and standard is inserted in octahedra frame
Material is compared, it is identical in that all containing low latitude structure division in crystal structure, difference is：1. the low latitude in accurate low latitude material
Structure is composed of anion octahedron；The low latitude structure of the low latitude material of standard is directly composed of atom；2. accurate
In low latitude material, low latitude structure charge is uneven, needs cation to provide electrostatic force and keeps charge balance, therefore MA+ cations
It is to be located near low latitude structure；In the low latitude material of standard, low latitude structure has been electroneutral, combines shape by Van der Waals force
At macroscopic material).
Quasi- low-dimensional bismuthino perovskite material MA used in the present invention3Bi2X9Powder raw material, existing skill may be used
Preparation method in art is made, such as the anti-solvent precipitation method, solvent evaporation method etc.；It is by a large amount of accurate low for the powder raw material
Dimension structure is linked together by ionic bond, is not typically available single quasi- low-dimensional bismuthino perovskite nano material；And this hair
It is bright and to be ultrasonically treated using solvent using amine as remover, single, mutually separated nanometer material can be obtained
Material, these quasi- low-dimensional bismuthino perovskite nanomaterial products are in single separation shape, the standard being available under the microscope
Low-dimensional bismuthino perovskite nano material.The present invention further preferably using oleic acid as ligand, makes the nanometer of oleic acid attachment after isolation
Material surface plays a protective role, to which the nano material that can be stabilized be made.
The present invention is particularly by quasi- low-dimensional bismuthino perovskite material MA used in control3Bi2X9Powder amount, stripping
The ratio of agent and powder, the specific power of crushing process and time, by quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder
The amount control of substance is no more than 0.1mmol, it can be ensured that powder uniformly removed (this be primarily due to amount of powder used with
The volume of solvent is directly proportional, and ultrasonic wave used in crushing process is generated by vibrating head, energy with distance increase and
Weaken, liquor capacity too conference causes a large amount of powder not remove uniformly)；It is accurate in mixture by taking solvent is normal octane as an example
Low-dimensional bismuthino perovskite material MA3Bi2X9Powder, amine, normal octane three substance amount ratio be 1：15~62.5：1000
~2250, and be 200W~400W by the power control used in crushing process, it is 30~60 minutes that will control processing time, profit
Strong energy is given with cell disruptor to split quasi- low-dimensional bismuthino perovskite material plus the release effect of amine, to realize
Has the preparation of good stability and the quasi- low-dimensional bismuthino perovskite nano material of other performances.
Description of the drawings
Fig. 1 is the MA realized according to the present invention3Bi2X9Cell configuration figure, correspond to Cl (1D), Br respectively from left to right
(2D) and I (0D), wherein I (0D), Br (2D), Cl (1D) correspond to 0 dimension-MA of standard respectively3Bi2I9, 2 dimension-MA of standard3Bi2Br9And it is accurate
1 dimension-MA3Bi2Cl9Structure；
Fig. 2 is the MA realized according to the present invention3Bi2Br9The absorption collection of illustrative plates of nano material；
Fig. 3 is the MA realized according to the present invention3Bi2Br9The fluorescence pattern of nano material；
Fig. 4 is the MA realized according to the present invention3Bi2Cl9The electron microscope picture of nano material.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The preparation method of quasi- low-dimensional bismuthino perovskite nano material, includes the following steps in the present invention：Using quasi- low-dimensional bismuth
Based perovskite material MA3Bi2X9The powder of (X=Cl, Br, I) is raw material, and amine is added as remover, uses normal octane for solvent
(other solvents can also be used, as long as can meet simultaneously：Perovskite material described in insoluble or slightly soluble, it would be desirable to be able to dissolving stripping
From agent；Such as n-hexane, toluene, methanol/normal octane mixed solvent may be used etc.)；Strong energy is given using cell disruptor
In addition the release effect of amine splits quasi- low-dimensional bismuthino perovskite material, the new nanometer of " from high to low, from having nothing " is realized
Materials synthesis；It is MA to take supernatant to obtain chemical formula after centrifugation3Bi2X9Nano material.
The present invention can also utilize ligand assisted comminution method (correspondingly, needing to add ligand material raw material), such as Fig. 1 institutes
Show, producing principle is：1) quasi- low-dimensional bismuthino perovskite material MA is used3Bi2X9The powder of (X=Cl, Br, I) is raw material,
The crushing that amine assists quasi- low-dimensional bismuthino perovskite material as remover is added, use cannot dissolve quasi- low-dimensional bismuthino perovskite material
The normal octane of material is solvent；2) giving strong energy using cell disruptor cooperates with the release effect of amine by quasi- low-dimensional bismuthino perovskite
Material is split, and realizes the new nano material synthesis of " from high to low, from having nothing "；3) supernatant is taken to obtain chemical formula after centrifuging
For MA3Bi2X9Nano material.
The preparation method of quasi- low-dimensional bismuthino perovskite nano material according to the present invention, preparation process and key exist
In：1) powder is utilized cell disruptor by mole value of quasi- low-dimensional bismuthino perovskite material powder between 0.02~0.1mmol
It crushes；2) amine is as remover, in the selection of amine includes the difference C chain lengths such as butylamine, n-octyl amine and oleyl amine in the present invention
Amine type, the molar ratio of raw material powder, amine and solvent normal octane three is 1：15~62.5：Between 1000~2250；3) oily
The sour quantum dot generated as ligand protection simultaneously makes it be dispersed in normal octane.
In the present invention, a variety of materials of selection are selected from the higher element of abundance in the earth's crust, resourceful and because not containing
Malicious ingredient and it is environmentally friendly, and perovskite structure and its adjustable light emitting region become the low cost with development potentiality
Free of contamination Illuminant nanometer material.
It is specific embodiment below：
Embodiment one
Quasi- low-dimensional bismuthino perovskite nano material, specific preparation process are as follows in the present embodiment：
Step 1：Clean a vial；Such as deionized water can be used, acetone, isopropanol, deionized water cleans in vain successively
Vial each ten minutes, then dried up with nitrogen gun；
Step 2：By 0.02mmol MA3Bi2Br9It is added in vial, first 5mL normal octanes and 0.5mL oil is added in backward bottle
Then acid adds the n-octyl amine of 100uL as remover respectively as solvent and ligand；
Wherein, raw material MA3Bi2Br9Subject to 2 dimension bismuthino perovskite powders；
Step 3：It will be put into vial in cell disruptor and power be transferred to 45 (i.e. power is 300W) starts crushing 30
Minute；
Step 4：The suspension in vial is taken out, supernatant is taken after its 8000rpm is centrifuged, obtains flaxen Bi bases
Perovskite nanometer sheet colloidal solution.
Embodiment two
Quasi- low-dimensional bismuthino perovskite nano material, specific preparation process are as follows in the present embodiment：
Step 1：Clean a vial；With deionized water, acetone, isopropanol, deionized water cleans white glass bottle successively
Each ten minutes, then dried up with nitrogen gun；
Step 2：By 0.02mmol MA3Bi2I9It is added in vial, first 5mL normal octanes and 0.5mL oleic acid is added in backward bottle
Respectively as solvent and ligand, the n-octyl amine of 200uL is then added as remover；
Wherein, raw material MA3Bi2I9Subject to 0 dimension bismuthino perovskite powders；
Step 3：To be put into vial in cell disruptor by power be transferred to 45 start crush 30 minutes；
Step 4：The suspension in vial is taken out, supernatant is taken after its 8000rpm is centrifuged, obtains pink Bi bases
Perovskite quantum dot colloidal solution.
Embodiment three
Quasi- low-dimensional bismuthino perovskite nano material, specific preparation process are as follows in the present embodiment：
Step 1：Clean a vial；With deionized water, acetone, isopropanol, deionized water cleans white glass bottle successively
Each ten minutes, then dried up with nitrogen gun；
Step 2：By 0.02mmol MA3Bi2Cl9It is added in vial, first 5mL normal octanes and 0.5mL oil is added in backward bottle
Then acid adds the n-octyl amine of 100uL as remover respectively as solvent and ligand；
Wherein, raw material MA3Bi2Cl9Subject to 1 dimension bismuthino perovskite powders；
Step 3：To be put into vial in cell disruptor by power be transferred to 45 start crush 30 minutes；
Step 4：The suspension in vial is taken out, supernatant is taken after its 8000rpm is centrifuged, obtains the Bi base calcium of white
Titanium ore nano wire colloidal solution.
For using the embodiment one that standard 2 ties up bismuthino perovskite powders, in starting powder raw material, a large amount of multi-layer nano pieces
It can combine closely because of the effect of the atom/molecules intermolecular forces such as ionic bond between layer, be stacked, be unable to get microcosmic ruler
Quasi- low-dimensional bismuthino perovskite nano material on degree, and by the preparation method in embodiment one, it can obtain being in be separated from each other
Shape, quasi- low-dimensional bismuthino perovskite nano material on micro-scale；Handle obtained quasi- low-dimensional bismuthino perovskite nano material
Its surface can be combined with oleic acid, form the nano material nanometer sheet being stabilized；If also, by the processing obtain containing receiving
The supernatant (supernatant can not only be used for intermediate product, also can be used as final product) of rice piece is dry, nanometer sheet material therein
The state being separated from each other will still be kept.
The quasi- low-dimensional bismuthino perovskite material MA of raw material of the present invention3Bi2X9Powder, both can be used it is commercially available,
Certainly, preparation method in the prior art (such as the anti-solvent precipitation method, solvent evaporation method) is can also refer to voluntarily to be prepared.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of quasi- low-dimensional bismuthino perovskite nano material, which is characterized in that include the following steps：Using accurate low
Tie up bismuthino perovskite material MA3Bi2X9Powder be raw material, amine obtains including the standard as remover, and using solvent
Low-dimensional bismuthino perovskite material MA3Bi2X9Powder, the amine and the solvent mixture, wherein X be Cl, Br, I in
At least one, the solvent can dissolve the remover and the solubility of the remover are more than to the quasi- low-dimensional bismuth
Based perovskite material MA3Bi2X9Solubility；Then, the mixture is handled using cell disruptor, then centrifuged, take supernatant
It is MA to obtain chemical formula3Bi2X9Quasi- low-dimensional bismuthino perovskite nano material.
2. the preparation method of quasi- low-dimensional bismuthino perovskite nano material as described in claim 1, which is characterized in that as the original
The quasi- low-dimensional bismuthino perovskite material MA of material3Bi2X9Powder substance amount ranging from 0.02~0.1mmol.
3. the preparation method of quasi- low-dimensional bismuthino perovskite nano material as described in claim 1, which is characterized in that as the stripping
The amine from agent is at least one of butylamine, n-octyl amine and oleyl amine；
The solvent is any one of normal octane, n-hexane, toluene and methanol/normal octane in the mixed solvent.
4. the preparation method of quasi- low-dimensional bismuthino perovskite nano material as described in claim 1, which is characterized in that the mixture
In, the quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder, both the amine the ratio of amount of substance be 1：15~
62.5；
The quasi- low-dimensional bismuthino perovskite material MA3Bi2X9The amount of substance of powder be with the solvent volume ratio between two
0.04mmol:6ml~15ml.
5. the preparation method of quasi- low-dimensional bismuthino perovskite nano material as described in claim 1-4 any one, which is characterized in that
Also include the oleic acid as ligand in the mixture, the quasi- low-dimensional bismuthino perovskite material MA3Bi2X9Powder and institute
The ratio for stating the amount of the substance of both oleic acid is 1:37.5~75.
6. the preparation method of quasi- low-dimensional bismuthino perovskite nano material as described in claim 1-5 any one, which is characterized in that
The cell disruptor handles the mixture, is handled 30~60 minutes under the power of 200W~400W, cell disruptor
Operative duty cycles be 1/3~1/2, the continuous ultrasound time be 1 second.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330335A (en) * | 2019-07-19 | 2019-10-15 | 中国工程物理研究院化工材料研究所 | Bismuthino halide ceramic material, preparation method and X-ray detector |
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| CN106390985A (en) * | 2016-08-31 | 2017-02-15 | 中国科学院新疆理化技术研究所 | Preparation method of ultrathin H1.78Sr0.78Bi0.22Nb2O7 nano-sheet |
| CN106433619A (en) * | 2016-09-27 | 2017-02-22 | 华中科技大学 | Preparation method of Bi-based perovskite quantum dot material |
| CN106631816A (en) * | 2016-12-23 | 2017-05-10 | 浙江大学 | Preparation method of atomic-scale thickness two-dimensional perovskite nanosheet by liquid phase stripping |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106390985A (en) * | 2016-08-31 | 2017-02-15 | 中国科学院新疆理化技术研究所 | Preparation method of ultrathin H1.78Sr0.78Bi0.22Nb2O7 nano-sheet |
| CN106433619A (en) * | 2016-09-27 | 2017-02-22 | 华中科技大学 | Preparation method of Bi-based perovskite quantum dot material |
| CN106631816A (en) * | 2016-12-23 | 2017-05-10 | 浙江大学 | Preparation method of atomic-scale thickness two-dimensional perovskite nanosheet by liquid phase stripping |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330335A (en) * | 2019-07-19 | 2019-10-15 | 中国工程物理研究院化工材料研究所 | Bismuthino halide ceramic material, preparation method and X-ray detector |
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