CN107418558A - A kind of preparation method of environment-friendly type bimetallic perovskite quantum dot - Google Patents
A kind of preparation method of environment-friendly type bimetallic perovskite quantum dot Download PDFInfo
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Abstract
The invention provides a kind of preparation method of environment-friendly type bimetallic perovskite quantum dot.Under conditions of inert gas shielding, first by AgBr and BiBr3With reaction dissolvent octadecylene, surfactant oleic acid, oleyl amine mixing, it is completely dissolved it, then mixed solution is heated to reaction temperature, is subsequently injected into the DMF solution dissolved with bromination butylamine, system starts reaction generation perovskite structure, and with the progress of reaction, gradually form (C4H9NH3)2AgBiBr6Quantum dot, reaction finally is quenched with acetone, that is, obtains final (C4H9NH3)2AgBiBr6Bimetallic perovskite quantum dot.The present invention, by adjusting the acidity of synthetic environment, on the premise of perovskite pattern and crystal structure is not changed, realizes the regulation and control to perovskite optical property using heat injection synthetic method.The perovskite quantum dot monodispersity and stability of synthesis are preferable, and pattern is homogeneous, have far-reaching significance for constructing the adjustable photoelectric device of band gap.
Description
Technical field
The present invention relates to a kind of technology of environment-friendly type bimetallic perovskite quantum dot preparation method, belongs to new material and prepares skill
Art field.
Background technology
With the appearance of new perovskite solar cell, perovskite material is widely paid close attention to by people.But the height of lead
Cost and toxicity are the problem of can not be ignored, and explore the inevitable requirement that synthesis is cheap, environment-friendly calcium titanium ore increasingly becomes research.
People have synthesized (CH at present3NH3)2MCl4(M=Sn, Ge, Cu, Fe, Mn, Cd) type perovskite, but because of band gap and relative matter
The change of amount, so as to also result in certain influence to the photoelectric properties of perovskite.In order to keep the original performance of perovskite, closely
Phase has also been proposed the A of bimetallic perovskite2B′B″X6Conception, wherein B ', B " be respectively monovalent metal and trivalent metal, monovalence
Cu in metal, Ag, Au are most suitable selection, and Sb in trivalent metal, Bi is most suitable selection.By crystal growth method,
Slavney has synthesized the preferable Cs of hot wet stability2AgBiBr6Perovskite monocrystalline (Slavney A H, Hu T, Lindenberg
A M,et al.A bismuth-halide double perovskite with long carrier recombination
lifetime for photovoltaic applications[J].Journal of the American Chemical
Society,2016,138(7):2138-2141).But it is concentrated mainly on purely inorganic monocrystalline for bimetallic research at present
Perovskite field, the research of organic bimetallic perovskite do not occur still.The present invention just there is provided a kind of double gold of environment-friendly type
Belong to the synthesis technique of perovskite, the quantum that stable performance, appearance and size are homogeneous and can be regulated and controled to its optical property can be obtained
Point.
The content of the invention
Technical problem:For problem of the prior art, there is provided a kind of preparation of environment-friendly type bimetallic perovskite quantum dot
Method.The amount of hydrobromic acid is added in the present invention by changing, makes up the bromine vacancy of perovskite in itself, can band gap occur it is certain
Change, so as to cause the change of its optical property.
Technical scheme:In order to solve the above-mentioned technical problem, the invention provides a kind of environment-friendly type bimetallic perovskite quantum
The preparation method of point, comprises the following steps:
Step 1, under the conditions of ice-water bath, hydrobromic acid is added dropwise in butylamine, methanol solution, stirred, removes ice
Water-bath, after room temperature reaction, revolving makes its crystallization, then with ether wash crystallization product, finally dries product vacuum, you can obtain
The bromination butylamine product of white, as the raw material reacted below;
Step 2, by reactant A gBr, BiBr3Mix with octadecylene, first vacuumize the mixed solution, after be passed through inertia
Gas, then vacuumize again, circulate operation;Last heat preservation and dryness under vacuum;
Step 3, inert gas is passed through, mixing surfactant oleic acid, oleyl amine, HBr added after step 2 heat preservation and dryness
In solution, continuing insulation is completely dissolved reactant, and metal salt precursor solution is made;
Step 4, bromination butylamine solid in step 1 is taken to be dissolved in DMF solution, before being rapidly injected metal salt made from step 3
Drive in liquid solution, generate (C4H9NH3)2AgBiBr6;1-1.5h is incubated at 110-120 DEG C, reaction then is quenched with acetone, i.e.,
Obtain (C4H9NH3)2AgBiBr6Perovskite quantum dot.
Wherein:
In step 1, described stirring, its speed is 900-1000rpm, and the described room temperature reaction time is 1.75-
2.25h。
In step 1, described revolving temperature is 45-60 DEG C.
Described to be washed with ether in step 1, washing times are 2-4 times, and wash time is each 20-30min.
In step 1, described vacuum drying, its temperature is 50-60 DEG C, drying time 18-24h.
In step 2, described BiBr3, AgBr materials amount ratio be 1:(1-1.25), mixing speed 900-1000rpm.
In step 2, described circulate operation, number is 2-4 times, and holding temperature is 110-130 DEG C, soaking time 1-
2h。
In step 3, the oleic acid of the addition, the volume ratio of oleyl amine are 1:(1-1.25), and be after vacuum drying
Anhydrous solvent;The volume ratio of the addition HBr and solution are (0.1-1):15.
In step 4, the DMF solution of the bromination butylamine of described addition and the volume ratio of solution are (1-1.25):30, bromination
The concentration of butylamine DMF solution is 1.9-2.1mol/L.
In step 4, the volume ratio (1-2) of the amount and solution for adding quencher acetone:1.
Beneficial effect:A kind of preparation method advantage of environment-friendly type bimetallic perovskite quantum dot of the present invention is:1) this hair
The perovskite quantum dot monodispersity and stability of bright synthesis are preferable, and pattern is homogeneous;2) the raw material letter needed for perovskite synthesis
Monocyclic guarantor, technology of preparing is stable, and method is simple, easy to operate, and repetitive rate is high;3) hot injection method can make nanocrystalline crystallinity more
It is good, excellent in optical properties.By changing the acidity of synthetic environment, adjustable 404-470nm fluorescence can be sent, this is advantageous to
The regulation of the photoelectric device performance in later stage.
Brief description of the drawings
Fig. 1 is that the TEM of perovskite quantum dot made from embodiment 1,7 schemes;
Fig. 2 is the XRD of perovskite quantum dot made from embodiment 1-2,4-7;
Fig. 3 is the fluorescence emission spectrogram of compound of perovskite quantum dot made from embodiment 1-7.
Embodiment
The present invention is further described with reference to embodiment and accompanying drawing.
A kind of preparation method of environment-friendly type bimetallic perovskite quantum dot of the present invention, is the condition in inert gas shielding
Under, first by AgBr and BiBr3With reaction dissolvent octadecylene, surfactant oleic acid, oleyl amine mixing, it is completely dissolved it, then
Mixed solution is heated to reaction temperature, is subsequently injected into the DMF solution dissolved with bromination butylamine, system starts reaction generation perovskite
Structure, and with the progress of reaction, gradually form (C4H9NH3)2AgBiBr6Quantum dot, reaction finally is quenched with acetone, that is, obtains
Final (C4H9NH3)2AgBiBr6Bimetallic perovskite quantum dot.
Embodiment 1:
Step 1, under the conditions of ice-water bath, 10mL hydrobromic acids are added dropwise to 10mL butylamine, 25mL methanol mixed solutions
In, it is sufficiently stirred.Remove ice-water bath, after reacting at room temperature 2h, 60 DEG C of revolvings make its crystallization, then are washed three times with ether, and every time 30
Minute.Finally by 60 DEG C of vacuum drying of product, you can the bromination butylamine product of white is obtained, as the raw material reacted below;
Step 2, by reactant 0.1mmol AgBr, 0.1mmol BiBr3Mix with octadecylene, first take out the mixed solution
Vacuum, after be passed through inert gas, then vacuumize again, circulate operation;Last heat preservation and dryness under vacuum;
Step 3, inert gas is passed through, surfactant 0.5mL oleic acid, 0.5mL oleyl amines, 0 μ L HBr are added into step 2
In mixed solution, continuing insulation is completely dissolved reactant, and metal salt precursor solution is made;
Step 4, take bromination butylamine solid 0.2mmol in step 1 to be dissolved in 100 μ L DMF solutions, be rapidly injected metal salt
In precursor solution, (C is generated4H9NH3)2AgBiBr6;1h is incubated at 120 DEG C, reaction then is quenched with acetone, that is, obtains
(C4H9NH3)2AgBiBr6Perovskite quantum dot.
Step 5,5min is centrifuged through 7000rpm, removes supernatant.Precipitation is taken to be dissolved in toluene i.e. available
(C4H9NH3)2AgBiBr6Quantum dot dispersion liquid.
Example 2:
Using the same process of embodiment 1, difference is, the amount of HBr in the step 3) of embodiment 1 is changed into 20 μ L, other
Condition is consistent, and obtains the product under 20 μ L acidity conditions.
Example 3:
Using the same process of embodiment 1, difference is, the amount of HBr in the step 3) of embodiment 1 is changed into 40 μ L, other
Condition is consistent, and obtains the product under 40 μ L acidity conditions.
Example 4:
Using the same process of embodiment 1, difference is, the amount of HBr in the step 3) of embodiment 1 is changed into 60 μ L, other
Condition is consistent, and obtains the product under 60 μ L acidity conditions.
Example 5:
Using the same process of embodiment 1, difference is, the amount of HBr in the step 3) of embodiment 1 is changed into 80 μ L, other
Condition is consistent, and obtains the product under 80 μ L acidity conditions.
Example 6:
Using the same process of embodiment 1, difference is, the amount of HBr in the step 3) of embodiment 1 is changed into 100 μ L, other
Condition is consistent, and obtains the product under 100 μ L acidity conditions.
Example 7:
Using the same process of embodiment 1, difference is, the amount of HBr in the step 3) of embodiment 1 is changed into 200 μ L, other
Condition is consistent, and obtains the product under 200 μ L acidity conditions.
Acidity by adjusting reaction condition can obtain the high perovskite quantum of homogeneous pattern, good dispersion, stability
Point, with the enhancing of acidity, it can be seen that its pattern, size and lattice structure from Fig. 1,2 and be basically unchanged, keep original calcium titanium
The crystal structure of ore deposit.Fluorescent emission collection of illustrative plates in comparison diagram 3, finds the increase with acidity, and fluorescent emission collection of illustrative plates occurs certain
Red shift, its fluorescent emission peak position increase to 470nm from 404nm.
Claims (10)
1. a kind of preparation method of environment-friendly type bimetallic perovskite quantum dot, it is characterised in that the preparation method includes following step
Suddenly:
Step 1, under the conditions of ice-water bath, hydrobromic acid is added dropwise in butylamine, methanol solution, stirred, removes ice-water bath,
After room temperature reaction, revolving makes its crystallization, then with ether wash crystallization product, finally dries product vacuum, you can obtain white
Bromination butylamine product, as the raw material reacted below;
Step 2, by reactant A gBr, BiBr3Mix with octadecylene, first vacuumize the mixed solution, after be passed through inert gas,
Then vacuumize again, circulate operation;Last heat preservation and dryness under vacuum;
Step 3, inert gas is passed through, mixed solution surfactant oleic acid, oleyl amine, HBr added after step 2 heat preservation and dryness
In, continuing insulation is completely dissolved reactant, and metal salt precursor solution is made;
Step 4, take bromination butylamine solid in step 1 to be dissolved in DMF solution, be rapidly injected metal salt presoma made from step 3
In solution, (C is generated4H9NH3)2AgBiBr6;1-1.5h is incubated at 110-120 DEG C, reaction then is quenched with acetone, that is, obtains
(C4H9NH3)2AgBiBr6Perovskite quantum dot.
A kind of 2. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 1, described stirring, its speed is 900-1000rpm, and the described room temperature reaction time is 1.75-2.25h.
A kind of 3. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 1, described revolving temperature is 45-60 DEG C.
A kind of 4. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
Described to be washed with ether in 1, washing times are 2-4 times, and wash time is each 20-30min.
A kind of 5. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 1, described vacuum drying, its temperature is 50-60 DEG C, drying time 18-24h.
A kind of 6. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 2, described BiBr3, AgBr materials amount ratio be 1:(1-1.25), mixing speed 900-1000rpm.
A kind of 7. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 2, described circulate operation, number is 2-4 times, and holding temperature is 110-130 DEG C, soaking time 1-2h.
A kind of 8. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 3, the oleic acid of the addition, the volume ratio of oleyl amine are 1:(1-1.25), and be the anhydrous solvent after vacuum drying;Institute
The volume ratio for stating addition HBr and solution is (0.1-1):15.
A kind of 9. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In 4, the DMF solution of the bromination butylamine of described addition and the volume ratio of solution are (1-1.25):30, bromination butylamine DMF solution
Concentration be 1.9-2.1mol/L.
A kind of 10. preparation method of environment-friendly type bimetallic perovskite quantum dot as claimed in claim 1, it is characterised in that step
In rapid 4, the volume ratio (1-2) of the amount and solution for adding quencher acetone:1.
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Cited By (7)
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CN108258119A (en) * | 2018-01-10 | 2018-07-06 | 中国科学院半导体研究所 | Inorganic halide bismuth perovskite battery and preparation method thereof |
CN109912459A (en) * | 2019-03-08 | 2019-06-21 | 武汉工程大学 | A kind of bimetallic perovskite nano material and preparation method thereof |
CN110408993A (en) * | 2019-06-29 | 2019-11-05 | 宁波大学 | A kind of Cs for X-ray detection2AgBiBr6The preparation method of double-perovskite crystal |
CN113233499A (en) * | 2021-06-09 | 2021-08-10 | 曲阜师范大学 | Preparation method for regulating morphology and fluorescence wavelength of inorganic perovskite nanocrystalline by using pH value of aqueous solution |
CN114315646A (en) * | 2021-12-06 | 2022-04-12 | 上海大学 | Preparation method of small-size blue-light perovskite nanocrystalline |
CN115318313A (en) * | 2022-07-25 | 2022-11-11 | 湖南平安环保股份有限公司 | Silver phosphate/double perovskite nanoflower structure composite photocatalytic material and preparation method and application thereof |
CN115646518A (en) * | 2022-07-25 | 2023-01-31 | 湖南平安环保股份有限公司 | Method for degrading antibiotic and preparing hydrogen by using nano-flower structure S-type heterojunction silver phosphate/double perovskite composite photocatalytic material |
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CN108258119A (en) * | 2018-01-10 | 2018-07-06 | 中国科学院半导体研究所 | Inorganic halide bismuth perovskite battery and preparation method thereof |
CN109912459A (en) * | 2019-03-08 | 2019-06-21 | 武汉工程大学 | A kind of bimetallic perovskite nano material and preparation method thereof |
CN109912459B (en) * | 2019-03-08 | 2021-10-12 | 武汉工程大学 | Bimetal perovskite nano material and preparation method thereof |
CN110408993A (en) * | 2019-06-29 | 2019-11-05 | 宁波大学 | A kind of Cs for X-ray detection2AgBiBr6The preparation method of double-perovskite crystal |
CN113233499A (en) * | 2021-06-09 | 2021-08-10 | 曲阜师范大学 | Preparation method for regulating morphology and fluorescence wavelength of inorganic perovskite nanocrystalline by using pH value of aqueous solution |
CN113233499B (en) * | 2021-06-09 | 2022-12-02 | 曲阜师范大学 | Preparation method for regulating morphology and fluorescence wavelength of inorganic perovskite nanocrystal by using pH value of aqueous solution |
CN114315646A (en) * | 2021-12-06 | 2022-04-12 | 上海大学 | Preparation method of small-size blue-light perovskite nanocrystalline |
CN115318313A (en) * | 2022-07-25 | 2022-11-11 | 湖南平安环保股份有限公司 | Silver phosphate/double perovskite nanoflower structure composite photocatalytic material and preparation method and application thereof |
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