CN106905974A - A kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle - Google Patents

A kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle Download PDF

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CN106905974A
CN106905974A CN201710055023.6A CN201710055023A CN106905974A CN 106905974 A CN106905974 A CN 106905974A CN 201710055023 A CN201710055023 A CN 201710055023A CN 106905974 A CN106905974 A CN 106905974A
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quantum dot
core
light emitting
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shell structure
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李剑锋
殷昊
程春晓
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Xiamen sibeike technology limited liability company
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Jinjiang Sibeike New Mstar Technology Ltd
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Abstract

The invention discloses a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle.Core-shell structure nanometer particle, its core metal nanoparticle surface local strong-electromagnetic field can strengthen quantum dot light emitting performance, its inertia shell is it is possible to prevente effectively from fluorescent quenching caused by metal nanoparticle and quantum point contact simultaneously, therefore can significantly improve quantum dot light emitting effect decades of times to thousands of times.Quantum dot film is prepared by disclosed method in the prior art, then disperses core-shell structure nanometer particle in film surface under room temperature condition, realization quickly significantly increases quantum dot light emitting behavior.This experiment Enhancement Method is simple and easy to do, pollution-free, and universality is good, with very strong operability.The principle and method can be applied to the aspects such as light emitting diode, solar cell, nano laser, photovoltaic infrared detector, single electron electric crystal.

Description

A kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle
Technical field
Strengthen luminous method the present invention relates to a kind of, quantum is strengthened with core-shell structure nanometer particle more particularly, to one kind The luminous method of point.
Background technology
Fluorescence is a kind of luminescence generated by light phenomenon, but conventional fluorescent molecule existence and stability is poor, and luminous half-peak breadth is wider, glimmering The low inferior position of light efficiency；And quantum dot has anti-light bleaching power strong, fluorescence efficiency is high, narrow luminous half-peak breadth the features such as, It is widely used in fields such as bioanalysis, photoelectric conversions.But after component film its luminescent behavior have stronger decay by In energy loss potentially between substrate, its application on device is strongly limit.Using coarse gold and silver substrate or gold Surface of Nano silver grain etc. can carry out effective regulation and control from primitive enhancing fluorescent technique to its luminescent behavior, improve it and light Intensity.But there is the loss that the energy transfer between metal and quantum dot is brought.So finding a kind of suitable method simultaneously Being avoided that loss simultaneously and carrying out its luminescent behavior turns into the key of enhancing quantum dot light emitting.
In order to improve the luminescent behavior of quantum dot, people are most begun attempt to using coarse gold early in last century the eighties year The grade on film surface carries out enhancing fluorescence from primitive resonance effects, because electromagnetic field field intensity can simultaneously improve launching efficiency with radiation Rate of decay, therefore surface etc. can significantly improve luminous (Hideo I. et al. from the local Electromagnetic enhancement that primitive is produced Optics express 2010, 18(16), 16546-16560).But surface etc. belongs to across space work from primitive enhancing fluorescence With fluorescence species need to be in apart from nano-particle/substrate appropriately distance.Can there is stronger energy when hypotelorism Transfer causes the decline of fluorescence intensity, and near field enhancing, distant electricity can be belonged to from primitive because waiting when distant Field strength decay is substantially because enhancing ability reduction.Beginning of this century Mikhail Artemyev is utilized and passed through in coarse golden film Regulating and controlling different PMMA thickness degree carries out the power of quantum dot light emitting, and obtains nearly ten times of enhancing（Olga K. et al. Nano Letters, 2002, 2 (12), 1449–1452）；But traditional enhancing mechanism is just with simple gold and silver nanometer Particle or rough base are strengthened, and simple nano-particle enhancing is limited in one's ability, but if it is carried out into coupling with gold and silver substrate Close, field intensity can realize further raising, for nano-particle is simply used merely, local pole in coupling regime Strong electromagnetic field has a significant impact for system luminescent behavior.Therefore regulate and control suitable distance and improve in local field intensity for System luminescence enhancement is very crucial.
To the beginning of this century, applicant's design has synthesized the core-shell structure nanometer particle of gold and silver core silica inertia shell, i.e., One layer of chemical deposition is very thin and pin-free on gold and silver nano-particle, the controllable inertia shell of thickness, borrows kernel gold and silver nanometer The extremely strong electromagnetic field of particle strengthens the Raman vibration signal and fluorescence signal of surface molecular（Moskovits, M.; Jeong, D. H. Chem. Phys. Lett. 2004, 397, 91.；Kamat, P. V.; Shanghavi, B. J. Phys. Chem. B 1997, 101, 7675；）.But current system is mainly used in the system of fluorescence molecule, for quantum dot light emitting The regulation and control of behavior do not obtain considerable enhancing result also at present, only only tens times, therefore searching one kind passes through Control accurate distance, realizes the enhanced method to quantum dot-based bottom fluorescence signal, and then it is luminous to obtain the enhancing of higher degree Ability is highly important.
The content of the invention
It is an object of the invention to provide a kind of simple to operate, quick, low cost, good fluorescence signal, favorable reproducibility, general The method for strengthening quantum dot fluorescence using core-shell structure nanometer particle.
In order to reach above-mentioned purpose, the technical solution adopted by the present invention is：
First in the chemically inert fine and close shell of surfaces of metal nanoparticles parcel last layer difference shell thickness, then will amount Son point is assembled on glass/Si/Au/ devices, is then disperseed/be assembled in substrate these nano-particles, using core metal The extremely strong electromagnetic field of nano-particle local strengthens the luminescent behavior of quantum dot film.
The present invention is comprised the following steps：
1) metal nanoparticle is prepared for kernel, and controllable thickness inert material is the nuclear shell structure nano grain of the core shell structure of shell Son；
2) synthesis luminescent behavior is clear and definite, quantum yield quantum dot higher；
3) quantum dot is used into chemisorbed/LB films/Electrostatic Absorption/spin coating (Spin-coating)/drop coating (Dip-coating) Etc. mode be assembled in glass, silicon, gold and silver substrate；
4) by the uniform spreading of nanometer/be assembled in testing sample surface；
5) test of surface enhanced quantum dot fluorescence is directly carried out.
The metal nanoparticle is preferably golden nanometer particle, Nano silver grain, copper nano-particle or aluminum nanoparticles etc. The metal nanoparticle of the property that resonated from primitive with notable surface etc..
The metal nanoparticle is preferably spherical, cube or the variously-shaped structures of metal nanoparticles such as bar-shaped, The particle diameter of the metal nanoparticle is preferably 10-300nm.
The shell is preferably silica shells, alumina case, titanium dioxide shell, silicon nitride shell or graphite The chemical inert material shell such as alkene shell.
The thickness of the shell is 1-30 nm controllable precises.
The quantum dot is water-soluble cadmium system quantum dot, oil-soluble cadmium system quantum dot, tradition without cadmium quantum dot, new quantum Point（Graphene quantum dot, Ca-Ti ore type quantum dot etc.）.
The excitation source wavelength of the method detection of the core-shell structure nanometer particle enhancing quantum dot fluorescence is 300-1100 nm。
Principle of the invention is：Local electromagnetic field high is produced to strengthen week by by core metal nanoparticle surface Enclose dipole to light, i.e., one layer of chemically inert cause of controllable thickness is wrapped up on the metal nanoparticle with extremely strong surface electromagnetic field Close shell（The materials such as silica, aluminum oxide, silicon nitride, titanium dioxide）, constitute core-shell structure nanometer particle, shell thickness control Then be placed in for the nano-particle and exist on quantum dot film by system within several nanometers, and Fluorescence Increasing test is carried out after drying, Strengthen the fluorescence signal of bottom quantum dot using the long-range effect of the strong Electromagnetic enhancement of inner layer metal nano-particle.
The present invention is to ensure quantum dot between metal nanoparticle using the upper controllable shell inertia densification shell of cladding Away from controllable, otherwise when spacing is too near, obvious quenching effect is had；Or the two spacing it is too remote when, electromagnetic field Intensity has substantially decay again, in the absence of enhancement effect of fluorescence.Therefore shell thickness must be regulated and controled reaches certain ideal distance, I.e. shell is controllable.
Compared with prior art, the present invention with it is following prominent a little and technique effect：
1) preparation method and raw material of core-shell structure nanometer particle of the invention are simple, and wherein core metal nano-particle is big The size of small and inertia shell thickness and quantum dot is controllable.
2) core-shell structure nanometer particle of the invention, the chemical inertness shell in cladding can be very good to receive core metal Rice corpuscles is hedged off from the outer world out, it is ensured that metal nanoparticle is not directly contacted with illuminator, will not cause obvious fluorescent quenching Phenomenon, and controllable shell can be very good the coupling model constructed between same substrate, so as to further improve luminescent behavior.
3）Only need to be placed in core-shell structure nanometer particle on quantum dot film/array/device by the present invention, can just improve quantum Optics behavior itself is put, and the enhancing of extremely strong multiple can be realized, and realize luminescent lifetime by nanosecond scale to psec chi The regulation and control of degree, explain for enhancing fluorescence system mechanism and provide strong experimental basis.
4) widened from primitive resonant check fluorescent technique range of application the invention enables surface etc., be high-efficiency quantum dot hair The raising of light/photoelectric device performance lays the foundation and introduces new pattern.
Brief description of the drawings
Fig. 1 is the experiment flow schematic diagram for preparing core-shell structure nanometer particle；
Fig. 2A-Fig. 2 E are the scanning electron microscope diagram (SEM) and transmission electron microscope figure of core-shell structure nanometer particle (TEM)；
Fig. 3 A- Fig. 3 C are classical cadmium system Quantum dots CdS e and new quantum dot CsPbBr3Transmission electron microscope figure (TEM) and The transmission electron microscope figure of carbon film over-assemble CdSe types quantum dot/nano-particle；
Fig. 4 A- Fig. 4 B are to strengthen quantum dot fluorescence lab diagram on golden film/glass.
Specific embodiment
Following examples will the invention will be further described with reference to accompanying drawing.
Embodiment 1
A kind of preparation of core-shell structure nanometer particle：
Fig. 1 provides the experiment flow schematic diagram of core-shell structure nanometer particle.
By taking silica film contracted payment core-shell structure nanometer particle as an example.Its specific preparation method is：
The aqueous solution of chloraurate that 200 mL mass fractions are 0.01% is taken, boiling is heated under stirring condition, be subsequently adding 1.6 mL The sodium citrate aqueous solution of mass fraction 1%, and the min of micro-boiling 50 is kept, solution makes it react completely by gradually becoming brownish red After naturally cool to room temperature, obtain final product the golden nanometer particle colloidal sol that diameter is about 45 ± 10 nm.The golden nanometer particle for taking 10 mL is molten Glue dilutes ten times as seed, and the mM silver nitrates of 4 mL 20 are gradually added dropwise and enter containing a certain amount of sodium citrate and ascorbic acid Seed liquor in, obtain final product the silver-colored gold-covered nano particle of the nm of particle diameter 150 ± 10.Above-mentioned silver-colored gold-covered nano particle is taken as seed, plus Enter the amino silane aqueous solution that 1-5 mL concentration is 0.1-10 mM, 15 min are stirred at room temperature, being subsequently adding 4 mL concentration is 10 mM sodium borohydride aqueous solutions and 1-20 mL sodium silicate aqueous solutions, adjust pH value about 9.5-10.5 afterwards.90 DEG C of water-baths are anti- Different time is answered, the silica contracted payment shell structurre nanoparticle sol of different shell thicknesses, wherein silica shell is obtained final product Thickness degree is about 2-30 nm.
Fig. 2A is the scanning electron microscope diagram (SEM) of silica contracted payment core-shell structure nanometer particle, and Fig. 2 B, 2C are oxidations Silicon contracted payment core-shell structure nanometer particle transmission electron microscope（TEM）, Fig. 2 D are that titanium oxide contracted payment core-shell structure nanometer particle is saturating Electron microscope (TEM) is penetrated, Fig. 2 E are titanium oxide contracted payment core-shell structure nanometer particle high resolution transmission electron microscopies.From height The fine and close titanium oxide shell layer of galactic nucleus Surface coating last layer can be best seen in resolved transmittance Electronic Speculum.In fig. 2, Scale is 4 μm, and scale is 50 nm in fig. 2b, and scale is 100 nm in Fig. 2 C, and scale is 20 nm, Fig. 2 E acceptances of the bid in Fig. 2 D Chi is 2 nm.
Embodiment 2
Detection core-shell structure nanometer particle strengthens sheet glass assembling quantum dot the test of fluorescence.
Oil phase CdSe nano-particles and novel inorganic perovskite CsPbBr have been synthesized using high warm injecting method3Quantum Point, Fig. 3 A are the fluorescence photo and transmission electron microscope figure of oil phase CdSe quantum dot, and Fig. 3 B are inorganic CsPbBr3Quantum The fluorescence photo and transmission electron microscope figure of point.CdSe quantum dot particle size -3.7 nm, CsPbBr in figure3Particle diameter is big Small -8 nm.
Using chemiadsorption/LB films/spin-coating（spin-coating）/ dipping film（dip-coating）Side Formula is assembled to quantum dot.Specific implementation is as follows, substrate of glass is carried out into surface amination using amino silane, by amination During substrate afterwards is immersed in containing quantum dot solution, thus inhaled to there is ligand exchange, quantum dot between quantum dot due to amino It is attached to substrate surface.Also can using interface formed LB films or using spin-coating by the way of assembled, it is notable that Using chemisorbed mode assembling quantum dot due to changing its surface ligand structure, new defect state is introduced, quantum dot can be caused Luminescent behavior changes, and is embodied in fluorescence spectra red shift and the reduction of quantum efficiency.
The core-shell structure nanometer particle of the different shell thicknesses that will be prepared is dispersed on quantum dot film, and to it Fluorescence behaviour is characterized.Fig. 4 A are to be assembled in golden film surface C dSe（TDPA ligand protections）Quantum dot core-shell structure nanometer particle Enhancing fluorescence results, Fig. 4 B are to be assembled in glass surface CsPbBr3(oleic acid ligand protection) quantum dot core-shell structure nanometer particle Enhancing fluorescence results.Shell thickness is respectively 6 nm, 10 nm, 2 nm, 16 nm, 20 nm and without nano-particle from top to bottom Blank group.Wherein shell is that the core-shell structure nanometer particle of 6 nm thickness realizes optimal enhancing ability, and intensification factor is for CdSe System has 50 times of raisings, for CsPbBr3System also has nearly 20 times of raising.Have this test result indicate that, by using core The electromagnetic field of shell structural nano particle localization, can significantly improve luminous；And different shell thicknesses can also significantly affect luminous Intensity, is also required to consider the influence of quenching during fluorescence is strengthened.Fig. 3 C are shown as core-shell structure nanometer particle and quantum Point package assembly, can reflect the structural representation of both entirety from figure.
Embodiment 3
Detection core-shell structure nanometer particle strengthens gold plaque assembling quantum dot the test of fluorescence.
Golden film we using the layer gold/magnetron sputtering layer gold/in the nm of wafer silicon face hot evaporation thickness about 200 and single Brilliant Au (111) is constructed, and wafer silicon cleaning process uses Piranhas Solution (H successively2SO4:H2O2-1:2), first Benzene/isopropanol (1:1), acetone/isopropanol (1:1), ethanol, ultra-pure water is cleaned by ultrasonic.In order to avoid quantum dot and golden film There is energy transfer and cause and itself be quenched in direct directly contact, our golden film surfaces deposit one layer and receive using technique for atomic layer deposition Rice thickness oxidation aluminium dielectric layer, it is possible to prevente effectively from the Quenching that directly contact causes, while the alumina layer of nano thickness Interference will not be produced to system coupling phenomenon again.
Chemiadsorption：Salic layer golden film is immersed in 10 mM amino silane ethanol solutions, shaken overnight, then With the amino silane of washes of absolute alcohol excess surface, and dried up with high pure nitrogen, i.e., realize amination in alumina surface；Will Substrate after amination is immersed in 12 hours in certain density quantum dot solution, will quantum dot be assembled on substrate.
LB embrane methods：Hexane solution containing 20 nmol quantum dots is slowly added dropwise in acetonitrile, waits hexane to wave naturally Hair, i.e., go out to be formed one layer of quantum dot film at interface, and drop coating (dip-coating) is carried out to quantum dot film using hydrophobic substrate is processed (LB films instrument), that is, complete quantum dot assembling.
Spin-coating method：A certain amount of quantum dot is dispersed in chloroform, 0.1 g PMMA are added, PMMA trichlorines are formed Dichloromethane, Spin-coating operations are carried out to it, and specific rotating speed is Step 1：500 rpm 30 s；Step 2： 6600 rpm 120 s.Film thickness is micron level.Afterwards quantum dot film is formed using acetone solution PMMA.
The quantum dot film spreading core-shell structure nanometer particle that will be assembled, carries out Fluorescence Increasing test.Such as Fig. 4, from upper And hypostratum thickness be respectively 6 nm, 10 nm, 15 nm, 2 nm, without shell Nano silver grain and without nano-particle blank group. Compared to uncoupled mode, intensification factor exists and is obviously improved under CGCM, glimmering under Fourier Series expansion technique by taking 6 nm systems as an example Luminous intensity improves nearly thousand times.
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art Scholar will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all according to the present invention The equivalent change or modification that Spirit Essence is done, should all be included within the scope of the present invention.

Claims (8)

1. a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle, its feature comprises the following steps：
(1) metal nanoparticle is prepared for kernel, and controllable thickness inert material is the nuclear shell structure nano of the core shell structure of shell Particle；
(2) by quantum dot adsorbing self assembly/LB films self assembly/Electrostatic Absorption/spin coating Spin-coating/ drop coatings Dip- Coating modes are assembled in substrate；
(3) the uniform spreading/assembling of nano-particle is dispersed on quantum dot substrate；
(4) test of surface enhanced quantum dot fluorescence is directly carried out.
2. a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle as claimed in claim 1, it is characterised in that The metal nanoparticle is golden nanometer particle, Nano silver grain, copper nano-particle and aluminum nanoparticles.
3. a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle as claimed in claim 1, it is characterised in that The metal nanoparticle is spherical gold nanoparticles, cube metal nanoparticle or bar-shaped metal nanoparticle.
4. as described in claim 1,2 or 3 it is a kind of with core-shell structure nanometer particle strengthen quantum dot light emitting method, its feature The particle diameter for being the metal nanoparticle is 20-300 nm.
5. a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle as claimed in claim 1, it is characterised in that Shell used is silica shell, aluminum oxide shell, titanium dioxide shell, silicon nitride shell or Graphene shell.
6. a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle as described in claim 1 or 5, its feature exists In the shell thickness be 1-30 nm.
7. a kind of method for strengthening quantum dot light emitting with core-shell structure nanometer particle as claimed in claim 1, it is characterised in that The excitation source wavelength of the method detection of the core-shell structure nanometer particle enhancing quantum dot light emitting is 300-1100 nm.
8. the method for strengthening quantum dot light emitting with core-shell structure nanometer particle as claimed in claim 1, it is characterised in that described Quantum dot be water phase or the sub- point of oil phase cadmium content, without cadmium quantum dot, inorganic Ca-Ti ore type quantum dot or graphene quantum dot.
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CN107611021A (en) * 2017-08-10 2018-01-19 南方科技大学 Prepare the method and its application of the quantum dot light emitting layer of patterns of high precision
CN107681277A (en) * 2017-09-22 2018-02-09 北京师范大学 A kind of luminous method with information storage of surface enhanced based on metal nanoparticle self-assembled structures
CN107759941A (en) * 2017-10-19 2018-03-06 宁波大学 A kind of preparation method of quasi-waveguide structure dyestuff/thin polymer film doped with silver-colored cube silica core shell material
CN108130085A (en) * 2018-01-23 2018-06-08 福州大学 A kind of preparation method of noble metal/silica dioxide composite particles and semiconductor-quantum-point lamination quantum dot light emitting film
CN108192594A (en) * 2018-01-24 2018-06-22 内蒙古民族大学 A kind of method for improving InAs single quantum dot fluorescence extraction efficiencies
CN108192619A (en) * 2018-01-23 2018-06-22 福州大学 A kind of gold/silica core-shell micro-structure and the preparation method of semiconductor-quantum-point composite quantum dot light-emitting film
CN108258059A (en) * 2018-01-23 2018-07-06 福州大学 A kind of preparation method based on gold/silica shell core micro-structure Yu semiconductor-quantum-point laminated film transistor
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CN112645593A (en) * 2021-01-15 2021-04-13 北京师范大学 Material for enhancing rare earth ion glass luminescence by using metal core-shell particles and method thereof
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CN114752371A (en) * 2022-03-18 2022-07-15 嘉庚创新实验室 Plasmon structure for regulating and controlling molecular luminescence and preparation method thereof
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CN107611021A (en) * 2017-08-10 2018-01-19 南方科技大学 Prepare the method and its application of the quantum dot light emitting layer of patterns of high precision
CN107681277A (en) * 2017-09-22 2018-02-09 北京师范大学 A kind of luminous method with information storage of surface enhanced based on metal nanoparticle self-assembled structures
CN107759941A (en) * 2017-10-19 2018-03-06 宁波大学 A kind of preparation method of quasi-waveguide structure dyestuff/thin polymer film doped with silver-colored cube silica core shell material
CN108258059A (en) * 2018-01-23 2018-07-06 福州大学 A kind of preparation method based on gold/silica shell core micro-structure Yu semiconductor-quantum-point laminated film transistor
CN108192619A (en) * 2018-01-23 2018-06-22 福州大学 A kind of gold/silica core-shell micro-structure and the preparation method of semiconductor-quantum-point composite quantum dot light-emitting film
CN108130085A (en) * 2018-01-23 2018-06-08 福州大学 A kind of preparation method of noble metal/silica dioxide composite particles and semiconductor-quantum-point lamination quantum dot light emitting film
CN108192594A (en) * 2018-01-24 2018-06-22 内蒙古民族大学 A kind of method for improving InAs single quantum dot fluorescence extraction efficiencies
CN109813698A (en) * 2018-12-29 2019-05-28 安徽中科赛飞尔科技有限公司 The method of the modified Raman technology detection polypeptide toxin in deactivation Nano silver grain surface
CN109813698B (en) * 2018-12-29 2021-12-07 安徽中科赛飞尔科技有限公司 Method for detecting polypeptide toxin by surface modification Raman technology of inert silver nanoparticles
CN110028949A (en) * 2019-03-22 2019-07-19 深圳市华星光电技术有限公司 The compound membrane preparation method of quantum dot, backlight module
CN114686210A (en) * 2020-12-30 2022-07-01 Tcl科技集团股份有限公司 Quantum dot material, preparation method thereof and photoelectric device
CN112645593A (en) * 2021-01-15 2021-04-13 北京师范大学 Material for enhancing rare earth ion glass luminescence by using metal core-shell particles and method thereof
CN114752371A (en) * 2022-03-18 2022-07-15 嘉庚创新实验室 Plasmon structure for regulating and controlling molecular luminescence and preparation method thereof
CN114752371B (en) * 2022-03-18 2023-11-03 嘉庚创新实验室 Plasmon structure for regulating and controlling molecular luminescence and preparation method thereof
CN114874764A (en) * 2022-05-12 2022-08-09 东南大学 Preparation method of perovskite thin film with enhanced luminescence property

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