CN105694893A - Langmiur-Blodgett composite lighting film of cadmium telluride quantum dots and layered double hydroxide and manufacturing method thereof - Google Patents
Langmiur-Blodgett composite lighting film of cadmium telluride quantum dots and layered double hydroxide and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a Langmuir-Blodgett (LB) composite lighting film of cadmium telluride quantum dots and layered double hydroxide and a manufacturing method thereof. The LB film is made by peeling layered double hydroxide nanoplates in organic solvent using a LB film drawing machine, and then alternatively assembled with the cadmium telluride quantum dots in the three-dimensional space layer by layer to form cadmium telluride quantum dots and layered double hydroxide supermolecule laminar materials of an ordered structure. According to different number of assembly layers, the thickness of the film can be controlled in the range of 20-9000 nm. By means of charge adjustment and group modification, the cadmium telluride quantum dots are fixed. With the rigid structure of the layered double hydroxide laminate and under the limitation effect of the two-dimensional space, the cadmium telluride quantum dots are fixed and are sequenced in order on the molecular scale, stability of the cadmium telluride quantum dots is optimized, and fluorescence quenching caused by intermolecular gathering is reduced. By the Langmiur-Blodgett film drawing method, lighting efficiency of the film is remarkably increased, and the film is of certain significance for fixing of various lighting molecules.
Description
Technical field
The invention belongs to composite luminescent material preparing technical field, in particular, provide a kind of cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film and preparation method thereof。
Background technology
Quantum dot (quantumdots, QDs) as the semiconductor nano material of a kind of novelty, there is nanometer character of many uniquenesses, there is wide absorption spectra, the emission spectra of narrower size adjustable, it is possible to excite the QDs of many different colours with single wavelength, possesses better light resistance, optical stability, it is possible to remain that through exciting of repeatedly circulating the luminescence of stronger fluorescence is from ultraviolet to infrared。CdTeQDs scope is at 2.5-4.0nm, and transmitting wavelength is 520-650nm, emission lifetime that signal is longer and higher signal intensity, slower photobleaching, and the susceptiveness of reaction strengthens。QDs, as a kind of fluorescent material, due to quantum limitation effect, has the electrical and optical properties of uniqueness, and synthesis in water quantum dot has the advantage that the organic synthesis methods such as synthetic operation is simple, cost is low, toxicity is little are incomparable。
It is a kind of novel multi-functional layered material that LDHs is also called brucite (LayeredDoubleHydroxides is abbreviated as LDHs), the multiple advantages such as it is adjustable that it has laminate metallic element, and interlayer ion is commutative。Research at present points out that hydrotalcite material carries out the monolayer nanometer sheet of the peelable one-tenth high degree of dispersion of mechanical agitation in organic solvent, the nanometer sheet of this stripping can pass through electrostatic, hydrogen bond, the anion of the active force such as hydrophobe and difference in functionality characteristic is assembled into the thin-film material of ordered arrangement layer by layer。
Langmuir-Blodgett film (be called for short LB film) is a kind of ultra-thin organic film, and its thickness in monolayer only has zero point several between several nanometers。LB membrane technology is the masking technique of a kind of accurate control film thickness and molecular structure。This is a kind of monomolecular film deposition technique, it is to be dispersed in by the amphiphile, amphiphilic molecule with hydrophilic head and hydrophobic tail on the water surface (parfacies), in the horizontal direction the water surface is applied pressure, make molecule close-packed arrays on the water surface, form one layer of orderly insoluble monomolecular film of arrangement。LB membrane technology is exactly the monomolecular film in above-mentioned air liquid interface is transferred to the surface of solids and realizes the technology that transfer assembles continuously。LB film has thickness and can accurately control, film-forming process does not need significantly high condition, simple to operation, the features such as film Middle molecule arrangement high-sequential, therefore assembling on a molecular scale can be realized, all have wide practical use in fields such as materialogy, optics, electrochemistry and bionics, become one of focus of people's concern in recent years。
Quantum dot is due to smaller event less stable, being difficult to long-term storage, in application aspect, how immobilized and device be its difficult point, utilize the principle of charge matching, the hydrotalcite nano piece of positively charged can carry out alternately assembling with the cadmium telluride quantum dot solution that entirety is electronegativity, prepares laminated film, but its complex operation, and luminous efficiency is relatively low, the present invention uses LB membrane technology, is preparing on the basis of brucite LB film, it is achieved the assembling of cadmium telluride quantum dot。Be conducive to improving cadmium telluride quantum dot aligning with dispersed on molecular scale, further increase fluorescence efficiency, simplify experimental implementation, be conducive to carrying out next step application。
Summary of the invention
It is an object of the invention to provide a kind of cadmium telluride quantum dot and brucite Langmuir-Blodgett composite luminescent film and preparation method thereof。Langmuir-Blodgett membrane technology is applied to the assembling of brucite and cadmium telluride quantum dot by the present invention as a kind of new assemble method, improve cadmium telluride quantum dot and align with dispersed on molecular scale, further increase fluorescence efficiency, simplifying experimental implementation, the raising for the immobilized luminous efficiency of cadmium telluride quantum dot provides solution。
The technical scheme is that the hydrotalcite nano piece peeled off in organic solvent is made Langmiur-Blodgett film by use LB film balance, alternately assemble layer by layer at three dimensions with cadmium telluride quantum dot again, form structurally ordered cadmium telluride quantum dot and brucite supermolecule stratified material。According to the difference assembling the number of plies, film thickness uniformly can regulate and control between 20-9000nm。This composite takes full advantage of the rigid structure of brucite and the confinement effect of two-dimensional space and host-guest interaction, it is achieved that the immobilization of quantum dot。
The preparation method of cadmium telluride quantum dot of the present invention and brucite Langmiur-Blodgett composite luminescent film is:
1) hydrotalcite precursor is added peel off in formamide solvent, addition is 0.5-1.5g/L, mixing speed is 3000-5000 rev/min, it is centrifuged after reacting 12-36 hour, discard precipitate, obtain clear colloid solution, be diluted to 0.01-0.5g/L, the NaOH solution using 0.1-0.4mol/L regulates PH to 9-9.5, is designated as solution A；
2) regulate the pH value of hydrophilic cadmium telluride quantum dot solution to 9-9.5 by the NaOH solution of 0.1-0.4mol/L, be designated as colloid solution B；
3) being dissolved in organic solvent by amphipathic molecule, be then added drop-wise in solution A, treat that organic solvent volatilizees, amphipathic molecule is evenly laid out, and control mould is 20-40mNm-1, substrate is carried out hydrophobization process, then uses the lift of LB film balance to prepare brucite LB film；It is positioned in colloid solution B again, soaks 10-20 minute and fully clean, the cadmium telluride quantum dot once circulated and brucite Langmiur-Blodgett composite luminescent film；
4) step 3 is repeated), alternately in solution A, lift operates and dip operation 1-10 time in colloid solution B, obtains multilamellar cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film。
The interlayer anion of described hydrotalcite precursor is NO3 —Or Cl—, on laminate, divalent metal and trivalent metal cation mol ratio are 2.0-4.0；Described divalent metal is Mg2+、Co2+、Ni2+、Ca2+, or Cu2+, trivalent metal cation is Al3+、Cr3+、Co3+Or Fe3+。
Described hydrotalcite precursor adopts coprecipitation, urea method, ion exchange or water heat transfer。
The preparation method of described hydrophilic cadmium telluride quantum dot solution is: under nitrogen protection with stirring condition; mercaptopropionic acid is added in the cadmium acetate solution that concentration is 0.002-0.004mol/L; regulating pH value by the NaOH solution of 0.1-0.4mol/L is 10.5-11; add potassium tellurate solution and sodium borohydride that concentration is 0.0004-0.0008mol/L; 100-120 DEG C is heated to reflux 0.5-10h, wherein cadmium acetate, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:5-20。
Described substrate is piezoid, silicon chip or sheet glass。
The method that described hydrophobization processes is: substrate chromic acid solution is soaked 6-8h, then after fully cleaning with deionized water, then 10-12h in the NaOH solution of 3-5wt% it is soaked in, washing, finally it is soaked in 20-30min in the chloroformic solution of the trim,ethylchlorosilane that volumetric concentration is 10-15%, takes out dry。
Cadmium acetate in the preparation method of described hydrophilic cadmium telluride quantum dot, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:5-9,100-120 DEG C is heated to reflux 1-10h, may finally obtain cadmium telluride quantum dot and the brucite Langmiur-Blodgett composite luminescent film of green light。
Cadmium acetate in the preparation method of described hydrophilic cadmium telluride quantum dot, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:10-14,100-120 DEG C is heated to reflux 3-10h, may finally obtain cadmium telluride quantum dot and the brucite Langmiur-Blodgett composite luminescent film of Yellow light-emitting low temperature。
Cadmium acetate in the preparation method of described hydrophilic cadmium telluride quantum dot, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:15-20,100-120 DEG C is heated to reflux 9-10h, may finally obtain the cadmium telluride quantum dot and the brucite Langmiur-Blodgett composite luminescent film that glow。
It is an advantage of the current invention that: the present invention utilizes electric charge to regulate and base group modification, it is achieved the immobilization of cadmium telluride quantum dot；Utilize the rigid structure of brucite laminate and the confinement effect of two-dimensional space, achieve the immobilization of photolytic activity cadmium telluride quantum dot and the ordered arrangement on molecular scale, improve the stability of cadmium telluride quantum dot, reduce the fluorescent quenching produced because of intermolecular aggregation；Achieve being obviously improved of thin-film light emitting efficiency by Langmiur-Blodgett film czochralski method, for multiple light emitting molecule immobilization, there is certain meaning。The membrane-film preparation process of two ways is easily operated, and the luminous intensity of thin film and film thickness all can assemble number of times by change and realize controllable precise。The transmitting optical range of thin film can realize the modulation from 520nm to 630nm, including green glow, gold-tinted, HONGGUANG。
Accompanying drawing explanation
The cadmium telluride quantum dot solution of Fig. 1 embodiment 1 synthesis and the fluorescent emission figure of cadmium telluride quantum dot and brucite Langmuir-Blodgett composite luminescent film。The cadmium telluride quantum dot of illustration to be glow color be gold-tinted and HONGGUANG and brucite Langmuir-Blodgett composite luminescent film in figure, at the camera picture of 365nm ultra violet lamp。
The cadmium telluride quantum dot that the assembling number of plies is 1 to 7 layers that Fig. 2 embodiment 2 obtains and brucite Langmuir-Blodgett composite luminescent film, for to carry out first order fluorescence spectrum test every 2 layers in figure, and the fluorescent emission figure of the cadmium telluride quantum dot prepared by laminated assembling technology and brucite layer assembly light-emitting film, the layer assembly thin film number of plies is 10 layers。In figure, illustration is cadmium telluride quantum dot and brucite layer assembly light-emitting film (10 layers) and cadmium telluride quantum dot and brucite Langmuir-Blodgett composite luminescent film (3 layers), at the camera picture of 365nm ultra violet lamp。
Detailed description of the invention
[embodiment 1]
1. ion exchange prepares nitrate anion hydrotalcite precursor:
A. by the solid Mg (NO of 0.09mol3)2·6H2Solid Al (the NO of O and 0.045mol3)3·9H2The solid urea of O and 0.54mol is dissolved in 300mL except CO2Deionized water in, shift after stirring in the politef pressure reacting container of 5 90 milliliters, crystallization 12 hours under 130 DEG C of conditions, be about under 7,60 DEG C of conditions dry 12h with deionized water centrifuge washing to pH, obtain carbonate brucite；
B. above-mentioned carbonate brucite 0.625g and solid NaNO is taken3118g is dissolved in 500mL except CO2Deionized water in, after dispersed, add after 0.25mL concentrated nitric acid, stir when nitrogen atmosphere, after room temperature carries out ion-exchange reactions 24 hours, with except CO2Deionized water centrifuge washing be about 7,70 DEG C of dry 12h to pH, obtain magnalium type nitrate anion intercalated houghite precursor；
2. take 0.15g above-mentioned magnalium type nitrate anion intercalated houghite precursor to stir 12 hours in 100 milliliters of formamide solvent, mixing speed is 5000 revs/min, by the brucite solution centrifugal after stripping, discard precipitate, obtain clear colloid solution, it is diluted to 0.1g/L, uses the NaOH solution of 0.1mol/L to regulate PH to 9, be designated as solution A；
3. aqueous phase synthesis method prepares cadmium telluride quantum dot:
A. taking cadmium acetate 0.0533g and be dissolved in 50ml deionized water, stir under nitrogen atmosphere, the NaOH solution adding mercaptopropionic acid 17.4 μ l, 0.1mol/L regulates PH to 10.5；Take potassium tellurate 0.01012g to be dissolved in 50ml deionized water, be subsequently adding above in solution, be eventually adding sodium borohydride 0.1518g；100 DEG C of oil bath heating, condensing reflux；
B. time segment sampling, observes at 5h and 10h sampling and testing respectively；The NaOH solution of the hydrophilic cadmium telluride quantum dot solution 0.1mol/L obtained regulates pH value to 9, is designated as colloid solution B；
4. prepare cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film:
A. hydrophobization processes: piezoid chromic acid solution soaks 8h, and after fully cleaning with deionized water, is soaked in 12h in 4wt%NaOH solution, and washing, being finally soaked in volumetric concentration is 20min in 10% trim,ethylchlorosilane chloroformic solution, takes out dry；
B. in solution A, drip the arachidic acid chloroformic solution 25 μ l that concentration is 0.001mol/L, treat that chloroform volatilizees, make arachidic acid evenly laid out；Using Y type LB film czochralski method, control mould is 20mNm-1, pull rate 4.5mm/min, film barrier speed 12.9mm/min, the piezoid after being processed by hydrophobization immerses solution A, then uses the lift of LB film balance to prepare brucite LB film；It is positioned in colloid solution B again, soaks 10 minutes and fully clean, the cadmium telluride quantum dot once circulated and brucite Langmiur-Blodgett composite luminescent film；
C. repeating step b, alternately in solution A, lift operates and dip operation 1 time in colloid solution B, obtains multilamellar cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film。
The light-emitting film that the solution obtained of b in step 3 and step 4 are finally given carries out Fluorescent Characterization: as shown in Figure 1, the fluorescence emission peak comparing cadmium telluride quantum dot colloid solution lays respectively at 570 and 613nm place, cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film blue shift to 566 and 608nm place。
[embodiment 2]
1. ion exchange prepares nitrate anion hydrotalcite precursor:
A. by the solid Mg (NO of 0.06mol3)2·6H2Solid Al (the NO of O and 0.03mol3)3·9H2The solid urea of O and 0.27mol is dissolved in 300mL except CO2Deionized water in, shift after stirring in the politef pressure reacting container of 5 90 milliliters, crystallization 30 hours under 100 DEG C of conditions, be about 7,30 DEG C of dry 24h with deionized water centrifuge washing to pH, obtain carbonate brucite；
B. above-mentioned carbonate brucite 0.5g and solid NaNO is taken360g is dissolved in 500mL except CO2Deionized water in, after dispersed, add after 0.16mL concentrated nitric acid, stir when nitrogen atmosphere, room temperature carries out ion-exchange reactions after 12 hours with except CO2Deionized water centrifuge washing be about 7,50 DEG C of dry 24h to pH, obtain magnalium type nitrate anion intercalated houghite precursor；
2. take 0.1g above-mentioned magnalium type nitrate anion intercalated houghite precursor to stir 36 hours in 100 milliliters of formamide solvent, mixing speed is 3000 revs/min, by the brucite solution centrifugal after stripping, discard precipitate, obtain clear colloid solution, it is diluted to 0.1g/L, uses the NaOH solution of 0.1mol/L to regulate PH to 9.5, be designated as solution A；
3. aqueous phase synthesis method prepares cadmium telluride quantum dot:
A. taking cadmium acetate 0.0533g and be dissolved in 50ml deionized water, stir under nitrogen atmosphere, the NaOH solution adding mercaptopropionic acid 17.4 μ l, 0.1mol/L regulates PH to 11；Take potassium tellurate 0.01012g to be dissolved in 50ml deionized water, be subsequently adding above in solution, be eventually adding sodium borohydride 0.0759g；100 DEG C of oil bath heating, condensing reflux 7h；
The NaOH solution of the hydrophilic cadmium telluride quantum dot solution 0.1mol/L b. obtained regulates pH value to 9, is designated as colloid solution B；
4. prepare cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film:
A. hydrophobization processes: piezoid chromic acid solution soaks 8h, and after fully cleaning with deionized water, is soaked in 12h in 4wt%NaOH solution, and washing, being finally soaked in volumetric concentration is 20min in 10% trim,ethylchlorosilane chloroformic solution, takes out dry；
B. in solution A, drip the arachidic acid chloroformic solution 25 μ l that concentration is 0.001mol/L, treat that chloroform volatilizees, make arachidic acid evenly laid out；Using Y type LB film czochralski method, control mould is 20mNm-1, pull rate 4.5mm/min, film barrier speed 12.9mm/min, the piezoid after being processed by hydrophobization immerses solution A, then uses the lift of LB film balance to prepare brucite LB film；It is positioned in colloid solution B again, soaks 10 minutes and fully clean, the cadmium telluride quantum dot once circulated and brucite Langmiur-Blodgett composite luminescent film；
C. repeating step b, alternately in solution A, lift operates and dip operation 1 time, 3 times, 5 times, 7 times in colloid solution B, obtains multilamellar cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film。
The thin film finally given is characterized: as shown in Figure 2, cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film are along with the increase assembling the number of plies, the maximum absorption band of its fluorescence emission spectrum presents continuous growth trend, as shown in Figure 2, the transmitting wavelength of this component film is 570 nanometers, for yellow orange light-emitting zone。Illustration in Fig. 2 is it can be seen that the thin film assembled is yellow orange light emission。
[comparative example 1]
Cadmium telluride quantum dot prepared by laminated assembling technology and brucite layer assembly light-emitting film:
1. piezoid is made hydrophilicity-imparting treatment: piezoid is soaked in concentrated sulphuric acid in advance: half an hour in the mixed solution of hydrogen peroxide=7:3 (volume ratio), then take out and dry with after deionized water ultrasonic cleaning；The piezoid handled well is joined PDDA solution soaks (PDDA:H half an hour2O=1:20, volume ratio), then dry with after deionized water cleaning；
3. being immersed in by the piezoid after hydrophilicity-imparting treatment in colloid solution B prepared by embodiment 2 10 minutes, take out deionized water rinsing, nitrogen dries up；Being immersed in by piezoid in the clear colloid solution (not regulating pH value) that embodiment 2 step 2 obtains again 10 minutes, take out deionized water rinsing, nitrogen dries up；Repeat aforesaid operations, alternately the houghite colloidal solution after colloid solution B and stripping is soaked, obtain 10 layers of cadmium telluride quantum dot and brucite layer assembly light-emitting film。Its fluorescent emission figure is as shown in Figure 2。
Claims (8)
1. the preparation method of a cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film, it is characterised in that its concrete operation step is:
1) hydrotalcite precursor is added peel off in formamide solvent, addition is 0.5-1.5g/L, mixing speed is 3000-5000 rev/min, it is centrifuged after reacting 12-36 hour, discard precipitate, obtain clear colloid solution, be diluted to 0.01-0.5g/L, the NaOH solution using 0.1-0.4mol/L regulates PH to 9-9.5, is designated as solution A；
2) regulate the pH value of hydrophilic cadmium telluride quantum dot solution to 9-9.5 by the NaOH solution of 0.1-0.4mol/L, be designated as colloid solution B；
3) being dissolved in organic solvent by amphipathic molecule, be then added drop-wise in solution A, treat that organic solvent volatilizees, amphipathic molecule is evenly laid out, and control mould is 20-40mNm-1, substrate is carried out hydrophobization process, then uses the lift of LB film balance to prepare brucite LB film；It is positioned in colloid solution B again, soaks 10-20 minute and fully clean, the cadmium telluride quantum dot once circulated and brucite Langmiur-Blodgett composite luminescent film；
4) step 3 is repeated), alternately in solution A, lift operates and dip operation 1-10 time in colloid solution B, obtains multilamellar cadmium telluride quantum dot and brucite Langmiur-Blodgett composite luminescent film。
2. preparation method according to claim 1, it is characterised in that the interlayer anion of described hydrotalcite precursor is NO3 —Or Cl—, on laminate, divalent metal and trivalent metal cation mol ratio are 2.0-4.0；Described divalent metal is Mg2+、Co2+、Ni2+、Ca2+, or Cu2+, trivalent metal cation is Al3+、Cr3+、Co3+Or Fe3+；Described hydrotalcite precursor adopts coprecipitation, urea method, ion exchange or water heat transfer。
3. preparation method according to claim 1; it is characterized in that; the preparation method of described hydrophilic cadmium telluride quantum dot solution is: under nitrogen protection with stirring condition; mercaptopropionic acid is added in the cadmium acetate solution that concentration is 0.002-0.004mol/L; regulating pH value by the NaOH solution of 0.1-0.4mol/L is 10.5-11; add potassium tellurate solution and sodium borohydride that concentration is 0.0004-0.0008mol/L; 100-120 DEG C is heated to reflux 0.5-10h, wherein cadmium acetate, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:5-20。
4. preparation method according to claim 1, it is characterised in that described substrate is piezoid, silicon chip or sheet glass。
5. preparation method according to claim 1, it is characterized in that, the method that described hydrophobization processes is: substrate chromic acid solution is soaked 6-8h, then after fully cleaning with deionized water, then 10-12h in the NaOH solution of 3-5wt% it is soaked in, washing, is finally soaked in 20-30min in the chloroformic solution of the trim,ethylchlorosilane that volumetric concentration is 10-15%, takes out dry。
6. preparation method according to claim 3, it is characterized in that, cadmium acetate in the preparation method of described hydrophilic cadmium telluride quantum dot, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:5-9,100-120 DEG C is heated to reflux 1-10h, may finally obtain cadmium telluride quantum dot and the brucite Langmiur-Blodgett composite luminescent film of green light。
7. preparation method according to claim 3, it is characterized in that, cadmium acetate in the preparation method of described hydrophilic cadmium telluride quantum dot, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:10-14,100-120 DEG C is heated to reflux 3-10h, may finally obtain cadmium telluride quantum dot and the brucite Langmiur-Blodgett composite luminescent film of Yellow light-emitting low temperature。
8. preparation method according to claim 3, it is characterized in that, cadmium acetate in the preparation method of described hydrophilic cadmium telluride quantum dot, mercaptopropionic acid, potassium tellurate, sodium borohydride molar ratio range be 1:1:0.2:15-20,100-120 DEG C is heated to reflux 9-10h, may finally obtain the cadmium telluride quantum dot and the brucite Langmiur-Blodgett composite luminescent film that glow。
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