CN110400890A - Non- regular microcavity Colloidal Quantum Dots electroluminescent device of one kind and preparation method thereof - Google Patents
Non- regular microcavity Colloidal Quantum Dots electroluminescent device of one kind and preparation method thereof Download PDFInfo
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Abstract
Non- regular microcavity Colloidal Quantum Dots electroluminescent device of one kind and preparation method thereof belongs to quantum dot light emitting technical field, it is therefore intended that the optically and electrically performance for solving the problems, such as that tradition MQLED enhancing quanta point electroluminescent of the existing technology faces is difficult to take into account.The present invention includes substrate, bottom mirror, anode modification layer, hole transmission layer, luminescent layer, electron transfer layer, cathode buffer layer and top mirror；The bottom mirror successively includes height index dielectric layer, filled layer and transparent electrode layer；The height index dielectric layer includes the alternate height index dielectric material of growth periodicity, and filled layer is broad stopband low absorption dielectric material；The bragg wavelength of the bottom mirror is identical with the intrinsic emission wavelength of quanta point material；The total optical thickness of the filled layer, transparent electrode layer, anode modification layer, hole transmission layer, luminescent layer, electron transfer layer, cathode buffer layer is equal to the integral multiple of tiny cavity light-emitting half-wavelength.
Description
Technical field
The invention belongs to quantum dot light emitting technical fields, and in particular to a kind of non-regular microcavity Colloidal Quantum Dots electroluminescent
Device and preparation method thereof.
Background technique
There is luminous efficiency height, monochromaticjty by the quanta point electroluminescent device (QLED) of luminescent layer of Colloidal Quantum Dots
The advantages such as good, solution processable, preparation cost be low, show wide application prospect in display and lighting area.And the effect that shines
Rate is one of the key index that QLED moves towards application.With novel quantum dot occur and electroluminescent principle, exciton relaxation mechanism,
The researchs such as device architecture optimizes and charge effectively transports continue deeply, and the luminous efficiency of QLED realizes great-leap-forward development, mesh
Before have been approached commercialization OLED efficiency.Although above-mentioned important research progress is achieved, it will be appreciated, however, that in QLED device
Because of the presence of nano functional layer, so that surface emissivity mode reduces, and waveguide mode is then obviously increased.Due to transparent electrode and
The interface of the interface of glass substrate and glass substrate and air can be totally reflected, and the light extraction efficiency of device is lower, seriously
Constrain the development and application of QLED.How to reduce total reflection effect in QLED device, improve optically coupling to device to outside
The ratio (light extraction efficiency) in space causes the extensive concern of people.It is existing to pass through the methods of change substrate light output surface pattern difficulty
To be obviously improved the light extraction efficiency of device.The luminous efficiency for promoting QLED device, not only helps and overcomes needing for the field QLED
The problem of solution, it helps break through it in the key technology bottleneck of efficient display and lighting area application.
Planar wave micro-cavity structure is introduced into luminescent device, using its regulation to optical mode, can effectively improve
Device light emitting efficiency, while significantly improving device spectral monochromaticjty.Planar wave microcavity, which is not only widely used in high-performance, to be had
Organic electro luminescent and laser device also constantly obtain important research progress in terms of QLED.But up to the present, using plane
Optical microcavity enhancing quantum dot (QD) electroluminescent correlative study has not been reported.Mainly by following several respects reason, (1)
There are big optical scatterings in QLED device, are unfavorable for microcavity to the Effective Regulation of optical mode；(2) exciton recombination zone of QD is difficult
With completely overlapped with the standing wave antinode of conventional microcavity, cause resonant check effect that can not maximize；(3) QLED device architecture is unfavorable
In the long adjusting of the chamber of microcavity.
Summary of the invention
It is an object of the invention to propose non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind and preparation method thereof,
The optically and electrically performance for solving the problems, such as that tradition MQLED enhancing QD electroluminescent of the existing technology faces is difficult to take into account.
To achieve the above object, the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind of the invention successively includes lining
Bottom, bottom mirror, anode modification layer, hole transmission layer, luminescent layer, electron transfer layer, cathode buffer layer and top mirror；
The bottom mirror successively includes height index dielectric layer, filled layer and transparent electrode layer；The height folding
The rate dielectric layer of penetrating includes the alternate height index dielectric material of growth periodicity, and filled layer is broad stopband low absorption medium material
Material；Bragg wavelength (the λ of the bottom mirrorBragg) identical with the intrinsic emission wavelength of quanta point material；
The filled layer, transparent electrode layer, anode modification layer, hole transmission layer, luminescent layer, electron transfer layer, cathode are slow
Rush the integral multiple that the total optical thickness of layer is equal to tiny cavity light-emitting half-wavelength.
The height index dielectric material of the bottom mirror is TiO2/SiO2Or Ta2O5/SiO2Or HfO2/SiO2, high
The optical thickness that low refractive index dielectric material forms film is 1/4 λBragg, logarithm is 2.5-5.5 pairs.
The filling layer material is SiO2Or LiF or Al2O3, with a thickness of 5-500 nanometers.
The transparent electrode layer is that transparent conductive metal oxide film is ITO or IVO, and transparent electrode layer forms film
Optical thickness be 1/4 λBragg。
The substrate material is glass (SiO2) or sapphire (Al2O3) or silicon (Si) or silicon carbide (SiC)；With a thickness of
150-3000 microns.
The anode modification layer is with a thickness of 10-60 nanometers；The thickness of hole transport layer is 10-80 nanometers；It is described to shine
Layer is with a thickness of 10-60 nanometers；The electron transport layer thickness is 10-80 nanometers；The cathode buffer layer is received with a thickness of 0.5-2
Rice.
The top mirror can be thick metal electrode either composite reflector composition, and composite reflector is by thin metal
Electrode and top distributed bragg reflector mirror composition.
It is described thickness metal electrode with a thickness of 80-300 nanometers；The thin metal electrode with a thickness of 10-30 nanometers.
The λ of the top distributed bragg reflector mirrorBraggIt is identical with the intrinsic emission wavelength of quantum dot.
The structure of top distributed bragg reflector mirror is the height index dielectric material composition of periodical alternating growth.
The height index dielectric material of top distributed bragg reflector mirror is ZnS/MgF2Or ZnSe/MgF2；Height is rolled over
Penetrating rate dielectric material and forming the optical thickness of film is 1/4 λBragg。
A kind of non-regular microcavity Colloidal Quantum Dots electroluminescent device preparation method the following steps are included:
Step 1: it is anti-as the bottom of microcavity that non-regular conductive profile formula Bragg mirror is prepared in rigid substrate
Penetrate mirror；
Step 2: the bottom mirror obtained in step 1 etches pattern using yellow light technique, obtains patterned
Bottom mirror；
Step 3: be sequentially prepared in the transparent electrode of patterned bottom mirror anode modification layer, hole transmission layer,
Luminescent layer and electron transfer layer；
Step 4: it is sequentially prepared cathode buffer layer on the electron transport layer and by thick metal electrode or by thin metal
Top mirror of the composite reflector of electrode and top distributed bragg reflector mirror composition as microcavity.
The non-regular conductive profile formula Bragg mirror is prepared using electron beam evaporation method.
The top distributed bragg reflector mirror is prepared using electron beam evaporation method.
The invention has the benefit that the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind of the invention and its system
Preparation Method realizes the regulation to QD radiation recombination resonant check by non-regular microcavity design, can effectively improve Colloidal Quantum Dots
The luminous efficiency of electroluminescent device.The optically and electrically performance that the present invention is faced for tradition MQLED enhancing QD electroluminescent
It is difficult to the problem of taking into account, proposes to overcome conventional microcavity chamber is long mutually to restrict with QLED functional layer thickness by non-regular microcavity design
The problem of, realize the flexible modulation to QD radiation recombination resonant check；Effectively inhibit the light scattering inside MQLED, realizes current-carrying
The balance injection and transmission of son；It is realized eventually by non-regular optical microcavity design and QD electroluminescent efficiency is obviously improved.
It realizes the flexible modulation long to optical field distribution and chamber, finally obtains efficient MQLED, it will be to the practicalization for promoting QLED
It has very important significance.
Detailed description of the invention
One kind non-regular microcavity Colloidal Quantum Dots EL device structure schematic diagram Fig. 1 of the invention；
Fig. 2 be the non-regular microcavity Colloidal Quantum Dots electroluminescent device electroluminescent spectrum of embodiment T4 and comparative example C1 without
The comparison of chamber Colloidal Quantum Dots electroluminescent device electroluminescent spectrum；
Fig. 3 is comparative example C1 and the comparison of embodiment T4 VA characteristic curve；
Fig. 4 is comparative example C1 and embodiment T4 brightness as voltage change curve compares；
Fig. 5 is comparative example C1 and embodiment T4 current efficiency with current density change curve comparison；
Fig. 6 is that embodiment T1, T2, T3, T4, T5, T6 normalize later electroluminescent spectrum comparison；
The luminescent spectrum full width at half maximum and current efficiency that Fig. 7 is embodiment T1, T2, T3, T4, T5, T6 are with microcavity device
The change curve of part emission wavelength compares；
Wherein: 1, substrate, 2, bottom mirror, the 201, first high refractive index layer, the 202, first low-index layer, 203, fill out
Fill layer, 204, transparent electrode layer, 3, anode modification layer, 4, hole transmission layer, 5, luminescent layer, 6, electron transfer layer, 7, cathode it is slow
Rush layer, 8, top mirror, 801, electrode layer, the 802, second high refractive index layer, the 803, second low-index layer.
Specific embodiment
Embodiments of the present invention are described further with reference to the accompanying drawing.
Referring to attached drawing 1, the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind of the invention successively include substrate 1,
Bottom mirror 2, anode modification layer 3, hole transmission layer 4, luminescent layer 5, electron transfer layer 6, cathode buffer layer 7 and top reflective
Mirror 8；
The bottom mirror 2 successively includes height index dielectric layer, filled layer 203 and transparent electrode layer 204；It is described
Height index dielectric layer includes alternate first high refractive index layer 201 of growth periodicity and the first low-index layer 202, filling
Layer 203 is broad stopband low absorption dielectric material；Bragg wavelength (the λ of the bottom mirror 2Bragg) and quanta point material sheet
Optical wavelength of levying is identical；
The filled layer 203, transparent electrode layer 204, anode modification layer 3, hole transmission layer 4, luminescent layer 5, electron-transport
The total optical thickness of layer 6, cathode buffer layer 7 is equal to the integral multiple of tiny cavity light-emitting half-wavelength.
The height index dielectric material of the bottom mirror 2 is TiO2/SiO2Or Ta2O5/SiO2Or HfO2/SiO2,
Refractive index is respectively 2.38/1.46,2.23/1.46,2.06/1.46；The optics that height index dielectric material forms film is thick
Degree is 1/4 λBragg, logarithm is 2.5-5.5 pairs.
203 material of filled layer is SiO2Or LiF or Al2O3, with a thickness of 5-500 nanometers, refractive index is respectively 1.4,
1.46、1.76。
It is ITO or IVO that the transparent electrode layer 204, which is transparent conductive metal oxide film, and refractive index is respectively
2.05/2.12, it is 1/4 λ that transparent electrode layer 204, which forms the optical thickness of film,Bragg。
1 material of substrate is glass (SiO2) or sapphire (Al2O3) or silicon (Si) or silicon carbide (SiC)；With a thickness of
150-3000 microns.
The material of the anode modification layer 3 is polythiofuran derivative poly- (3,4- ethylenedioxythiophene) (PEDOT) doping
Polystyrolsulfon acid (PSS) (PEDOT:PSS), with a thickness of 10-60 nanometers, refractive index 1.55；The material of the hole transmission layer 4
Material is polyvinylcarbazole (PVK), with a thickness of 10-80 nanometers, refractive index 1.59；The material of the luminescent layer 5 is colloid quantum
Point (QD), with a thickness of 10-60 nanometers, refractive index 1.75；The material of the electron transfer layer 6 is Zinc oxide nanoparticle
(ZnO), with a thickness of 10-80 nanometers, refractive index 2.01；The material of the cathode buffer layer 7 is LiF, is received with a thickness of 0.5-2
Rice, refractive index 1.41.
The top mirror 8 can be thick metal electrode either composite reflector, and composite reflector is by thin metal electricity
Pole and top distributed bragg reflector mirror composition.
The material of thick metal electrode is Al or Ag, with a thickness of 80-300 nanometers；The material of thin metal electrode be Al or
Ag, with a thickness of 10-30 nanometers.
The λ of the top distributed bragg reflector mirrorBraggIt is identical with the intrinsic emission wavelength of quantum dot.
The structure of top distributed bragg reflector mirror is the second high refractive index layer 802 and second of periodical alternating growth
Index layer 803 forms.
The height index dielectric material of top distributed bragg reflector mirror is ZnS/MgF2Or ZnSe/MgF2, refractive index
Respectively 2.35/1.38,2.48/1.38；The optical thickness that height index dielectric material forms film is 1/4 λBragg。
The light that non-regular micro-cavity quantum point electroluminescent device issues goes out light from 1 side of substrate.
A kind of non-regular microcavity Colloidal Quantum Dots electroluminescent device preparation method the following steps are included:
Step 1: bottom of the non-regular conductive profile formula Bragg mirror as microcavity is prepared in rigid substrate 1
Reflecting mirror 2；
Step 2: the bottom mirror 2 obtained in step 1 etches pattern using yellow light technique, obtains patterned
Bottom mirror 2；
Step 3: anode modification layer 3, hole transport are sequentially prepared in the transparent electrode of patterned bottom mirror 2
Layer 4, luminescent layer 5 and electron transfer layer 6；
Step 4: cathode buffer layer 7 is sequentially prepared on the electron transfer layer 6 and by thick metal electrode or by thin gold
Belong to top mirror 8 of the composite reflector of electrode and top distributed bragg reflector mirror composition as microcavity.
The non-regular conductive profile formula Bragg mirror is prepared using electron beam evaporation method.
The top distributed bragg reflector mirror is prepared using electron beam evaporation method.
Specifically:
1) it successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 150-3000 microns of rigid substrate 11, fills
Enter fixture, be placed in substrate frame, be put into electron beam coater, prepares preparation bottom mirror 22；It vacuumizes and gradually
Cavity temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1
×10-2Pascal, under conditions of Hall source assists, periodically alternately preparation TiO first2/SiO2Or Ta2O5/SiO2Or HfO2/
SiO2, continue to produce the SiO with a thickness of 5-500 nanometers2Or LiF or Al2O3And 0.5 the period ITO or IVO, evaporation rate
Control is in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, and 0.20~0.25 nm/sec and 0.15~0.25 nanometer/
Second；The optical thickness in each period is 1/2 bragg wavelength；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 22 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is that 1000-5000 turns every by adjusting spin coater rotation speed
Minute, so that PEDOT:PSS is formed the anode modification layer 33 of one layer of 10-60 nanometer thickness on the surface of transparent electrode, is put into 120 DEG C
Baking oven in heat 30 points of kinds, then naturally cool to room temperature (23 DEG C)；The above-mentioned pattern bottom for being coated with PEDOT:PSS is anti-
It penetrates mirror 22 to be transferred in glove box, and places it on spin coater bracket, the PVK solution that a certain concentration is uniformly mixed is uniform
Drop is on aforesaid substrate, and adjusting spin coater revolving speed is 1000-5000 rpms, and spin coating obtains 10-80 nanometer thickness after 1 minute
Hole transmission layer 44 is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；In
Spin coater is continued to use on above-mentioned hole transmission layer 44 and prepares luminescent layer 55, and adjusting spin coater revolving speed is 1000-4000 revolutions per minute
Clock, spin coating obtain the luminescent layer 55 of 10-60 nanometer thickness after 50 seconds, be placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, so
After naturally cool to room temperature (23 DEG C)；Spin coater is continued to use on above-mentioned luminescent layer 55 and prepares electron transfer layer 66, adjusts rotation
Painting machine revolving speed is 1000-5500 rpms, and spin coating obtains the electron transfer layer 66 of 10-80 nanometer thickness after 1 minute, be placed on gloves
10 points of kinds are heated in case in 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, initially evaporate
The cathode buffer layer 77 of 0.5-2 nanometer thickness；Then start to prepare top mirror 88, evaporate the thick metal electricity of 80-300 nanometer thickness
Pole layer 801 or the product that first obtains step 2) are put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, steam first
The cathode buffer layer 77 for sending out 0.5-2 nanometer thickness continues the thin metal electrode layer 801 of 10-30 nanometers of evaporation, then again puts product
Enter into electron beam coater, when vacuum degree is up to 2 × 10-3When Pascal, 4.5 period ZnS/MgF are alternately prepared2Or ZnSe/
MgF2, evaporation rate control is in 0.3~0.4 nm/sec and 0.3~0.35 nm/sec；The optical thickness in each period is 1/2
Prague central wavelength.
4) after preparation is completed, taking-up is tested under the conditions of atmosphere at room temperature.
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated, it should be understood that described herein specific examples are only used to explain the present invention, is not used to limit
The fixed present invention.
Comparative example C1:
1) glass lined with patterned ITO electrodes that will be successively cleaned up using deionized water, acetone, EtOH Sonicate
Bottom 1 is placed on the bracket of spin coater, and by 0.22 micron of aqueous filtering head, PEDOT:PSS is uniformly filled to entire piece,
By adjusting 2500 rpms of spin coater rotation speed, PEDOT:PSS is made to form one layer 35 nanometers on the surface of ITO electrode
Thick film is put into 120 DEG C of baking oven and heats 30 points of kinds, then naturally cools to room temperature (23 DEG C)；
2) the PEDOT:PSS substrate 1 that is coated with for obtaining step 1) is transmitted in glove box, is placed on the bracket of spin coater
On, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml uniformly drips on aforesaid substrate, adjusts spin coater
Revolving speed be 2500 rpms, spin coating 1 minute after PEDOT:PSS surface formed one layer of 40 nanometer thickness film, be placed on hand
30 points of kinds are heated in casing in 140 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；It is continued to use on PVK layers above-mentioned
Spin coater prepares luminescent layer 5, and the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration 10mg/ml, adjusts
After 2000 rpms of spin coater revolving speed, spin coating 50 seconds of section, the film of one layer of 35 nanometer thickness is formed on the surface of PVK, is placed on hand
10 points of kinds are heated in casing in 90 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；Rotation is continued to use on QD layers above-mentioned
Painting machine prepares electron transfer layer 6ZnO, and the solvent of ZnO solution is n-butanol, and concentration 35mg/ml, adjusting spin coater revolving speed is
The film for forming one layer of 45 nanometer thickness after 1500 rpms, spin coating 1 minute on the surface of QD, is placed in glove box 120 DEG C
10 points of kinds are heated in thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Al of 120 nanometer thickness.
Embodiment T1:
1) successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 1.1 millimeters of K9 glass substrate 1, it is packed into folder
Tool, is placed in substrate frame, is put into electron beam coater, prepares preparation bottom mirror 2；It vacuumizes and gradually by cavity
Temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1 × 10-2
Pascal alternately prepares the TiO in 3.5 periods under conditions of Hall source assists first2/SiO2, continued growth LiF and 0.5
The ITO in period, evaporation rate are controlled in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, 0.2~0.25 nm/sec
With 0.15~0.25 nm/sec；TiO2、SiO2, LiF and ITO physical thickness be 66.1,106.38,18 and 68 nanometers；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 2 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is 2500 rpms by adjusting spin coater rotation speed,
So that PEDOT:PSS is formed the film of one layer of 35 nanometer thickness on the surface of ITO electrode, is put into 30 points of heating in 120 DEG C of baking oven
Kind, then naturally cool to room temperature (23 DEG C)；The sample for being coated with PEDOT:PSS is transferred in glove box, and is placed it in
On spin coater bracket, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml is uniformly dripped in aforesaid substrate
On, one layer of 38 nanometer thickness is formed on the surface of PEDOT:PSS after adjusting 2450 rpms of spin coater revolving speed, spin coating 1 minute
Film is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；PVK layers above-mentioned
On continue to use spin coater and prepare luminescent layer 5, the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration is
10mg/ml after adjusting spin coater revolving speed is 2100 rpms, spin coating 50 seconds, forms one layer of 32 nanometer thickness on the surface of PVK
Film is placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；On above-mentioned QD layer
It continues to use spin coater and prepares electron transfer layer 6ZnO, the solvent of ZnO solution is n-butanol, and concentration 35mg/ml adjusts spin coating
Machine revolving speed be 2000 rpms, spin coating 1 minute after QD surface formed one layer of 32 nanometer thickness film, be placed in glove box
10 points of kinds are heated in 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Ag of 120 nanometer thickness.
Embodiment T2:
1) successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 1.1 millimeters of K9 glass substrate 1, it is packed into folder
Tool, is placed in substrate frame, is put into electron beam coater, prepares preparation bottom mirror 2；It vacuumizes and gradually by cavity
Temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1 × 10-2
Pascal alternately prepares the TiO in 3.5 periods under conditions of Hall source assists first2/SiO2, continued growth LiF and 0.5
The ITO in period, evaporation rate are controlled in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, 0.2~0.25 nm/sec
With 0.15~0.25 nm/sec；TiO2、SiO2, LiF and ITO physical thickness be 66.1,106.38,26 and 68 nanometers；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 2 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is 2400 rpms by adjusting spin coater rotation speed,
So that PEDOT:PSS is formed the film of one layer of 37 nanometer thickness on the surface of ITO electrode, is put into 30 points of heating in 120 DEG C of baking oven
Kind, then naturally cool to room temperature (23 DEG C)；The sample for being coated with PEDOT:PSS is transferred in glove box, and is placed it in
On spin coater bracket, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml is uniformly dripped in aforesaid substrate
On, one layer of 38 nanometer thickness is formed on the surface of PEDOT:PSS after adjusting 2450 rpms of spin coater revolving speed, spin coating 1 minute
Film is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；PVK layers above-mentioned
On continue to use spin coater and prepare luminescent layer 5, the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration is
10mg/ml after adjusting spin coater revolving speed is 2100 rpms, spin coating 50 seconds, forms one layer of 32 nanometer thickness on the surface of PVK
Film is placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；On above-mentioned QD layer
It continues to use spin coater and prepares electron transfer layer 6ZnO, the solvent of ZnO solution is n-butanol, and concentration 35mg/ml adjusts spin coating
Machine revolving speed be 1900 rpms, spin coating 1 minute after QD surface formed one layer of 34.5 nanometer thickness film, be placed on glove box
10 points of kinds are heated in interior 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Ag of 120 nanometer thickness.
Embodiment T3:
1) successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 1.1 millimeters of K9 glass substrate 1, it is packed into folder
Tool, is placed in substrate frame, is put into electron beam coater, prepares preparation bottom mirror 2；It vacuumizes and gradually by cavity
Temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1 × 10-2
Pascal alternately prepares the TiO in 3.5 periods under conditions of Hall source assists first2/SiO2, continued growth LiF and 0.5
The ITO in period, evaporation rate are controlled in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, 0.2~0.25 nm/sec
With 0.15~0.25 nm/sec；TiO2、SiO2, LiF and ITO physical thickness be 66.1,106.38,36 and 68 nanometers；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 2 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is 2300 rpms by adjusting spin coater rotation speed,
So that PEDOT:PSS is formed the film of one layer of 41 nanometer thickness on the surface of ITO electrode, is put into 30 points of heating in 120 DEG C of baking oven
Kind, then naturally cool to room temperature (23 DEG C)；The sample for being coated with PEDOT:PSS is transferred in glove box, and is placed it in
On spin coater bracket, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml is uniformly dripped in aforesaid substrate
On, one layer of 38 nanometer thickness is formed on the surface of PEDOT:PSS after adjusting 2450 rpms of spin coater revolving speed, spin coating 1 minute
Film is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；PVK layers above-mentioned
On continue to use spin coater and prepare luminescent layer 5, the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration is
10mg/ml after adjusting spin coater revolving speed is 2100 rpms, spin coating 50 seconds, forms one layer of 32 nanometer thickness on the surface of PVK
Film is placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；On above-mentioned QD layer
It continues to use spin coater and prepares electron transfer layer 6ZnO, the solvent of ZnO solution is n-butanol, and concentration 35mg/ml adjusts spin coating
Machine revolving speed be 1800 rpms, spin coating 1 minute after QD surface formed one layer of 37.5 nanometer thickness film, be placed on glove box
10 points of kinds are heated in interior 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Ag of 120 nanometer thickness.
Embodiment T4:
1) successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 1.1 millimeters of K9 glass substrate 1, it is packed into folder
Tool, is placed in substrate frame, is put into electron beam coater, prepares preparation bottom mirror 2；It vacuumizes and gradually by cavity
Temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1 × 10-2
Pascal alternately prepares the TiO in 3.5 periods under conditions of Hall source assists first2/SiO2, continued growth LiF and 0.5
The ITO in period, evaporation rate are controlled in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, 0.2~0.25 nm/sec
With 0.15~0.25 nm/sec；TiO2、SiO2, LiF and ITO physical thickness be 66.1,106.38,48 and 68 nanometers；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 2 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is 2200 rpms by adjusting spin coater rotation speed,
So that PEDOT:PSS is formed the film of one layer of 44 nanometer thickness on the surface of ITO electrode, is put into 30 points of heating in 120 DEG C of baking oven
Kind, then naturally cool to room temperature (23 DEG C)；The sample for being coated with PEDOT:PSS is transferred in glove box, and is placed it in
On spin coater bracket, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml is uniformly dripped in aforesaid substrate
On, one layer of 38 nanometer thickness is formed on the surface of PEDOT:PSS after adjusting 2450 rpms of spin coater revolving speed, spin coating 1 minute
Film is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；PVK layers above-mentioned
On continue to use spin coater and prepare luminescent layer 5, the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration is
10mg/ml after adjusting spin coater revolving speed is 2100 rpms, spin coating 50 seconds, forms one layer of 32 nanometer thickness on the surface of PVK
Film is placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；On above-mentioned QD layer
It continues to use spin coater and prepares electron transfer layer 6ZnO, the solvent of ZnO solution is n-butanol, and concentration 35mg/ml adjusts spin coating
Machine revolving speed be 1800 rpms, spin coating 1 minute after QD surface formed one layer of 37.5 nanometer thickness film, be placed on glove box
10 points of kinds are heated in interior 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Ag of 120 nanometer thickness.
Embodiment T5:
1) successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 1.1 millimeters of K9 glass substrate 1, it is packed into folder
Tool, is placed in substrate frame, is put into electron beam coater, prepares preparation bottom mirror 2；It vacuumizes and gradually by cavity
Temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1 × 10-2
Pascal alternately prepares the TiO in 3.5 periods under conditions of Hall source assists first2/SiO2, continued growth LiF and 0.5
The ITO in period, evaporation rate are controlled in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, 0.2~0.25 nm/sec
With 0.15~0.25 nm/sec；TiO2、SiO2, LiF and ITO physical thickness be 66.1,106.38,56 and 68 nanometers；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 2 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is 2200 rpms by adjusting spin coater rotation speed,
So that PEDOT:PSS is formed the film of one layer of 44 nanometer thickness on the surface of ITO electrode, is put into 30 points of heating in 120 DEG C of baking oven
Kind, then naturally cool to room temperature (23 DEG C)；The sample for being coated with PEDOT:PSS is transferred in glove box, and is placed it in
On spin coater bracket, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml is uniformly dripped in aforesaid substrate
On, one layer of 38 nanometer thickness is formed on the surface of PEDOT:PSS after adjusting 2450 rpms of spin coater revolving speed, spin coating 1 minute
Film is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；PVK layers above-mentioned
On continue to use spin coater and prepare luminescent layer 5, the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration is
10mg/ml after adjusting spin coater revolving speed is 2100 rpms, spin coating 50 seconds, forms one layer of 32 nanometer thickness on the surface of PVK
Film is placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；On above-mentioned QD layer
It continues to use spin coater and prepares electron transfer layer 6ZnO, the solvent of ZnO solution is n-butanol, and concentration 35mg/ml adjusts spin coating
Machine revolving speed be 1700 rpms, spin coating 1 minute after QD surface formed one layer of 41 nanometer thickness film, be placed in glove box
10 points of kinds are heated in 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Ag of 120 nanometer thickness.
Embodiment T6:
1) successively using deionized water, acetone, EtOH Sonicate cleaning with a thickness of 1.1 millimeters of K9 glass substrate 1, it is packed into folder
Tool, is placed in substrate frame, is put into electron beam coater, prepares preparation bottom mirror 2；It vacuumizes and gradually by cavity
Temperature is increased to 200 DEG C, when ontology vacuum reaches 2 × 10-3After Pascal, high pure oxygen is filled and by vacuum degree control 1 × 10-2
Pascal alternately prepares the TiO in 3.5 periods under conditions of Hall source assists first2/SiO2, continued growth LiF and 0.5
The ITO in period, evaporation rate are controlled in 0.20~0.25 nm/sec, 0.25~0.30 nm/sec, 0.2~0.25 nm/sec
With 0.15~0.25 nm/sec；TiO2、SiO2, LiF and ITO physical thickness be 66.1,106.38,66 and 68 nanometers；
2) bottom mirror 2 that step 1) obtains is etched into pattern using yellow light technique, successively uses deionized water, third
Ketone, EtOH Sonicate cleaning.Then the bottom mirror 2 that will be patterned into is placed on the bracket of spin coater, passes through 0.22 micron
PEDOT:PSS is uniformly filled entire piece by aqueous filtering head, is 2150 rpms by adjusting spin coater rotation speed,
So that PEDOT:PSS is formed the film of one layer of 46 nanometer thickness on the surface of ITO electrode, is put into 30 points of heating in 120 DEG C of baking oven
Kind, then naturally cool to room temperature (23 DEG C)；The sample for being coated with PEDOT:PSS is transferred in glove box, and is placed it in
On spin coater bracket, solving homogeneously in high-purity chlorobenzene, concentration is that the PVK solution of 8mg/ml is uniformly dripped in aforesaid substrate
On, one layer of 38 nanometer thickness is formed on the surface of PEDOT:PSS after adjusting 2450 rpms of spin coater revolving speed, spin coating 1 minute
Film is placed in glove box 30 points of kinds of heating in 140 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；PVK layers above-mentioned
On continue to use spin coater and prepare luminescent layer 5, the QD used is feux rouges CdSe/ZnS quantum dot, is dissolved in toluene, concentration is
10mg/ml after adjusting spin coater revolving speed is 2100 rpms, spin coating 50 seconds, forms one layer of 32 nanometer thickness on the surface of PVK
Film is placed in glove box 10 points of kinds of heating in 90 DEG C of thermal station, then naturally cools to room temperature (23 DEG C)；On above-mentioned QD layer
It continues to use spin coater and prepares electron transfer layer 6ZnO, the solvent of ZnO solution is n-butanol, and concentration 35mg/ml adjusts spin coating
Machine revolving speed be 1600 rpms, spin coating 1 minute after QD surface formed one layer of 44 nanometer thickness film, be placed in glove box
10 points of kinds are heated in 120 DEG C of thermal station, then naturally cool to room temperature (23 DEG C)；
3) product for obtaining step 2) is put into vacuum coating, when vacuum degree is up to 4 × 10-4When Pascal, 1 is successively evaporated
The cathode buffer layer 7LiF of the nanometer thickness and metal electrode layer 801Ag of 120 nanometer thickness.
It is recognized that by above multiple embodiment and comparative examples:
Fig. 2 is embodiment T4 (micro-cavity quantum point luminescent device) electroluminescent spectrum and comparative example C1 (no chamber quantum dot hair
Optical device) electroluminescent spectrum comparison.From fig. 2 it can be seen that the electroluminescent spectrum compared to comparison C1, embodiment T4
The full width at half maximum of the electroluminescent spectrum of middle micro chamber device obviously narrows, and peak strength is obviously improved.
Fig. 3 is comparative example C1 and the comparison of embodiment T4 VA characteristic curve.It can be seen in figure 3 that comparative example C1 and reality
The VA characteristic curve for applying a T4 is similar, and the introducing of optical microcavity injects spy without substantially influencing the electricity of embodiment T4
Property.
Fig. 4 is comparative example C1 and embodiment T4 brightness as voltage change curve compares.It can be seen from figure 4 that comparison
Brightness or maximum brightness of the example C1 either under identical operating voltage are all significantly lower than the brightness of embodiment T4, illustrate structure
Reasonable non-regular optical microcavity can be obviously improved the light emission luminance of quanta point electroluminescent device.
Fig. 5 is comparative example C1 and embodiment T4 current efficiency with current density change curve comparison.It can from Fig. 5
It arrives, current efficiency or maximum current efficiency of the comparative example C1 either under identical working current density are all significantly lower than implementation
The current efficiency of example T4, illustrates that structurally reasonable non-regular optical microcavity can be obviously improved quanta point electroluminescent device
Luminous efficiency.
Fig. 6 is that embodiment T1, T2, T3, T4, T5, T6 normalize later electroluminescent spectrum comparison.It can be with from Fig. 6
See, the spectral characteristic of micro chamber device has very big difference in different embodiments, by filled layer 203 in change embodiment and not
The thickness of congenerous layer can use optical microcavity and obtain the adjustable efficient microcavity Colloidal Quantum Dots electroluminescent of emission wavelength
Device.
The electroluminescent spectrum full width at half maximum and current efficiency that Fig. 7 is embodiment T1, T2, T3, T4, T5, T6 are with microcavity
The change curve of device emission wavelength compares.It will be seen from figure 6 that in different embodiments non-regular micro chamber device electroluminescent hair
Light characteristic is influenced very greatly by emission wavelength, and the non-regular micro chamber device emission wavelength in embodiment is intrinsic closer to quanta point material
The half-breadth overall at spectral luminescence peak, corresponding spectrum is narrower, and current efficiency is higher.
It can be seen that comparing with comparative example C1 without chamber Colloidal Quantum Dots electroluminescent device, structurally reasonable is non-regular
Optical microcavity embodiment T4 has higher electroluminescent efficiency (being 5 times or more of comparative example C1 device efficiency).Non- regular light
Learning microcavity can be by the electroluminescence characters of Effective Regulation Colloidal Quantum Dots, to be obviously improved the electroluminescent hair of Colloidal Quantum Dots
Light efficiency illustrates that the method for the present invention has apparent advantage in terms of improving Colloidal Quantum Dots electroluminescent device luminous efficiency.
Claims (10)
1. a kind of non-regular microcavity Colloidal Quantum Dots electroluminescent device, which is characterized in that successively anti-including substrate (1), bottom
Penetrate mirror (2), anode modification layer (3), hole transmission layer (4), luminescent layer (5), electron transfer layer (6), cathode buffer layer (7) and top
Portion's reflecting mirror (8)；
The bottom mirror (2) successively includes height index dielectric layer, filled layer (203) and transparent electrode layer (204)；Institute
Stating height index dielectric layer includes the alternate height index dielectric material of growth periodicity, and filled layer (203) is broad stopband
Low absorption dielectric material；The bragg wavelength of the bottom mirror (2) is identical with the intrinsic emission wavelength of quanta point material；
The filled layer (203), transparent electrode layer (204), anode modification layer (3), hole transmission layer (4), luminescent layer (5), electricity
The total optical thickness of sub- transport layer (6), cathode buffer layer (7) is equal to the integral multiple of tiny cavity light-emitting half-wavelength.
2. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 1, which is characterized in that described
The height index dielectric material of bottom mirror (2) is TiO2/SiO2Or Ta2O5/SiO2Or HfO2/SiO2, high low-refraction
The optical thickness that dielectric material forms film is 1/4 bragg wavelength, and logarithm is 2.5-5.5 pairs；Filled layer (203) material
For SiO2Or LiF or Al2O3, with a thickness of 5-500 nanometers.
3. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 1, which is characterized in that described
It is ITO or IVO that transparent electrode layer (204), which is transparent conductive metal oxide film, and transparent electrode layer (204) forms film
Optical thickness is 1/4 bragg wavelength.
4. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 1, which is characterized in that described
Substrate (1) material is glass or sapphire or silicon or silicon carbide；With a thickness of 150-3000 microns.
5. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 1, which is characterized in that described
Anode modification layer (3) is with a thickness of 10-60 nanometers；The hole transmission layer (4) is with a thickness of 10-80 nanometers；The luminescent layer (5) is thick
Degree is 10-60 nanometers；The electron transfer layer (6) is with a thickness of 10-80 nanometers；The cathode buffer layer (7) is received with a thickness of 0.5-2
Rice.
6. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 1, which is characterized in that described
Top mirror (8) is formed by thick metal electrode or by composite reflector, and composite reflector is by thin metal electrode and top part
Cloth Bragg mirror composition.
7. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 6, which is characterized in that described
Thick metal electrode with a thickness of 80-300 nanometers；The thin metal electrode with a thickness of 10-30 nanometers.
8. the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind according to claim 6, which is characterized in that described
The bragg wavelength of top distributed bragg reflector mirror is identical with the intrinsic emission wavelength of quantum dot；The top distribution cloth
The structure of glug reflecting mirror is made of the height index dielectric material of periodical alternating growth；The top distributed Bragg
The height index dielectric material of reflecting mirror is ZnS/MgF2Or ZnSe/MgF2；The light of height index dielectric material formation film
It learns with a thickness of 1/4 bragg wavelength.
9. special based on the preparation method of the non-regular microcavity Colloidal Quantum Dots electroluminescent device of one kind described in claim 1
Sign is, comprising the following steps:
Step 1: it is anti-as the bottom of microcavity that non-regular conductive profile formula Bragg mirror is prepared on rigid substrate (1)
Penetrate mirror (2)；
Step 2: the bottom mirror obtained in step 1 (2) etches pattern using yellow light technique, obtains patterned bottom
Portion's reflecting mirror (2)；
Step 3: anode modification layer (3), hole transport are sequentially prepared in the transparent electrode of patterned bottom mirror (2)
Layer (4), luminescent layer (5) and electron transfer layer (6)；
Step 4: cathode buffer layer (7) is sequentially prepared on the electron transfer layer (6) and by thick metal electrode or by thin gold
Belong to top mirror (8) of the composite reflector of electrode and top distributed bragg reflector mirror composition as microcavity.
10. preparation method according to claim 9, which is characterized in that described non-regular conductive profile formula Prague is anti-
Mirror and top distributed bragg reflector mirror is penetrated to prepare using electron beam evaporation method.
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