CN106380818A - Quantum dot material and preparation method, quantum dot membrane, backlight module and display equipment - Google Patents
Quantum dot material and preparation method, quantum dot membrane, backlight module and display equipment Download PDFInfo
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- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
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Abstract
The invention discloses a quantum dot material and a preparation method, a quantum dot membrane, a backlight module and display equipment, belonging to the technical field of liquid crystal display. The preparation method of the quantum dot material comprises the following steps: (a) adding acetate of IIB-group element into a polyether ketone solution with side carboxyl, and stirring and mixing uniformly under the protection of inert gas, wherein the IIB-group element is cadmium or zinc; (b) heating the reaction system obtained in the step (a) to a preset temperature; and (c) adding selenourea or thiourea into the reaction system obtained in the step (b), and detecting the light wavelength of the reaction system, wherein the quantum dot material is obtained when the light wavelength of the reaction system reaches the preset wavelength. The growth of quantum dots is controlled by use of the coordination effect of carboxyl, then the quantum dots are uniformly dispersed in a polymer matrix, the luminous efficiency of the quantum dot membrane based on the quantum dot material is improved, the brightness of the backlight module is enhanced, and the development of high-gamut liquid crystal display equipment is facilitated.
Description
Technical field
The present invention relates to technical field of liquid crystal display, particularly to a kind of quanta point material and preparation method, quantum dot film,
Backlight module, display device.
Background technology
With the continuous development of lcd technology, consumer requires more and more higher to the colour gamut of liquid crystal display.Closely
Nian Lai, either in international consumer electronics product exhibition (CES), or in Chinese household electrical appliances fair (AWE), high color
Domain liquid crystal display all becomes the main flow of development.At present, mainly provide for liquid crystal display by using technology of quantum dots
Backlight improving the colour gamut of liquid crystal display, specifically, that is, the backlight module of liquid crystal display diffuser plate or
Quantum dot film is set above person's light guide plate.
The structure of existing quantum dot film is as shown in figure 1, main include：Quantum dot layer 1a and be attached to quantum dot layer 1a
The water oxygen barrier layer 2a on two surfaces.Wherein, quantum dot layer 1a includes polymeric matrix, and is distributed in polymeric matrix
Quantum dot (such as CdS, CdSe, CdSe/ZnS etc.).Water oxygen barrier layer 2a has aluminum oxide (Al for surface2O3) coating or its
Polyethylene terephthalate (PET) film of his inorganic matter coating, to prevent quantum dot from contacting and losing with vapor, oxygen
Effect.When preparing quantum dot film, first quantum dot is mixed to form quantum dot layer with polymer-doped, then on quantum dot layer two sides
Attach water oxygen barrier layer thus obtaining quantum dot film.
During realizing the present invention, the inventors discovered that at least there is problems with prior art：Existing amount
In son point film, quantum dot dispersion is uneven, is susceptible to reunite so that the luminous efficiency of quantum dot film is relatively low, thus affecting to carry on the back
The brightness of light module, and then affect the display effect of liquid crystal display.
Content of the invention
Based on the above, embodiment of the present invention technical problem to be solved is, provide a kind of quanta point material and
Its preparation method, and the quantum dot film based on this quanta point material, backlight module, display device, make quantum dot in polymer
Can be dispersed in matrix, prevent quantum dot from reuniting, improve the luminous efficiency of quantum dot film.
Specifically, including following technical scheme：
In a first aspect, the embodiment of the present invention provides a kind of preparation method of quanta point material, comprise the following steps：
Step a, adds the acetate of II B race element in the polyether-ketone solution have carboxyl side group, protects in inert gas
It is uniformly mixed under shield；Described II B race element is cadmium or zinc；
Step b, the temperature of the reaction system that described step a is obtained is heated to preset temperature；
Step c, adds selenourea or thiocarbamide, and detects the luminous of reaction system in the reaction system obtaining to described step b
Wavelength, when the emission wavelength of reaction system reaches preset wavelength, that is, obtains described quanta point material.
Preferably, in the described polyether-ketone with carboxyl side group the quantity of carboxyl side group and described polyether-ketone construction unit
Quantity ratio be 1:(1～4).
Preferably, the acetate of described II B race element and the rubbing of carboxyl side group in the described polyether-ketone with carboxyl side group
Your ratio is (0.5～1):1；Described selenourea or thiocarbamide are (1～1.05) with the mol ratio of the acetate of described II B race element:1.
Preferably, the preset wavelength in described step c is 510nm～550nm or 610nm～650nm.
Preferably, the described preset temperature in described step b is 100 DEG C～175 DEG C.
Preferably, the described polyether-ketone with carboxyl side group is the PAEK with carboxyl side group.
Preferably, in the described PAEK with carboxyl side group, carboxyl side group passes through phenyl ring with PAEK main chain even
Connect.
Preferably, contain naphthalene nucleus in the PAEK main chain of the described PAEK with carboxyl side group.
Preferably, the chemical constitution of the described PAEK with carboxyl side group is as follows：
Second aspect, the embodiment of the present invention provides a kind of quanta point material preparing using above-mentioned preparation method.
The third aspect, the embodiment of the present invention provides a kind of quantum dot film, and this quantum dot film includes：By above-mentioned quantum dot material
The quantum dot layer that material is formed；And, it is attached to the PET film lamella on described two surfaces of quantum dot layer.
Fourth aspect, the embodiment of the present invention provides a kind of backlight module, and this backlight module includes above-mentioned quantum dot film.
5th aspect, the embodiment of the present invention provides a kind of liquid crystal display, and this liquid crystal display includes the above-mentioned back of the body
Light module.
The beneficial effect of technical scheme provided in an embodiment of the present invention：
Embodiments provide a kind of method preparing quanta point material by fabricated in situ, to have carboxyl side
The polyether-ketone of base, as polymeric matrix, using the coordination between carboxyl and II B element, controls quantum dot in polymer
Growth position in matrix, makes quantum dot fully dispersed in polymeric matrix.With quantum dot material provided in an embodiment of the present invention
Material is prepared quantum dot film and can be prevented effectively from quantum dot reunion, reduces quantum dot Duplication, thus improving the luminous of quantum dot film
Efficiency, and then lift the brightness of backlight module and the display effect of liquid crystal display, promote high colour gamut liquid crystal display
Development.
Brief description
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, will make to required in embodiment description below
Accompanying drawing be briefly described it should be apparent that, drawings in the following description are only some embodiments of the present invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the structural representation of existing quantum dot film；
Fig. 2 is the flow chart of the preparation method of quanta point material provided in an embodiment of the present invention；
Fig. 3 is the structural representation of quanta point material provided in an embodiment of the present invention；
Fig. 4 is the structural representation of quantum dot film provided in an embodiment of the present invention；
Fig. 5 is the structural representation of backlight module provided in an embodiment of the present invention.
The reference of in figure represents respectively：
1st, quantum dot layer, 11, polyether-ketone strand, 12, quantum dot；
2nd, PET film lamella；
A, backboard-reflector plate；
B, quantum dot film；
C, diaphragm group；
D, construction package；
1a, the quantum dot layer of existing quantum dot film；
2a, the water oxygen barrier layer of existing quantum dot film.
Specific embodiment
For making technical scheme and advantage clearer, below in conjunction with accompanying drawing embodiment of the present invention is made into
One step ground describes in detail.Unless otherwise defined, all technical terms used by the embodiment of the present invention are respectively provided with and art technology
The identical implication that personnel are generally understood that.
In a first aspect, the embodiment of the present invention provides a kind of preparation method of quanta point material, referring to Fig. 2, this preparation method
Comprise the following steps：
Step 1, adds the acetate of II B race element in the polyether-ketone solution have carboxyl side group, protects in inert gas
It is uniformly mixed under shield；II B race element is cadmium or zinc.
Step 2, the temperature of the reaction system that step 1 is obtained is heated to preset temperature.
Step 3, addition selenourea or thiocarbamide in the reaction system obtaining to step 2, and detect the emission wavelength of reaction system,
When the emission wavelength of reaction system reaches preset wavelength, that is, obtain quanta point material.
In existing quantum dot film, quantum dot is directly mixed with polymeric matrix, but quantum dot be inorganic matter and
Its particle diameter is usually nanoscale, and polymeric matrix is organic matter, and this results in quantum dot and is susceptible in polymeric matrix
Reunite so that quantum dot is overlapping.In photoluminescent process, amount quantum dot overlap can make the light of light excitation quantum point generation again
Secondary by other quantum dots absorb excite again, thus lead to quantum dot film luminous efficiency relatively low, impact backlight module brightness.
As can be seen here, by improving dispersive property in polymeric matrix for the quantum dot, prevent quantum dot from reuniting, reduce the weight of quantum dot
Folded rate is to improve the effective way of quantum dot film luminous efficiency, thus lifting backlight module brightness, improves liquid crystal display
Display effect.
Part is added to control the size of quantum dot and to divide in the preparation process of quantum dot it will usually in reaction system
Scattered property.
Based on the above, embodiments provide a kind of side preparing quanta point material by fabricated in situ
Method, the quanta point material of gained is quantum dot polyether-ketone composite.Specifically, made with the polyether-ketone with carboxyl side group
For polymeric matrix, using carboxyl as part, participate in the brilliant nucleation of quantum dot nano and growth, thus controlling quantum dot poly-
Growth position in compound matrix, in the quanta point material thus preparing, quantum dot can fully divide in polymeric matrix
Dissipate.Quantum dot film being prepared with this quanta point material and can be prevented effectively from quantum dot reunion, reducing quantum dot Duplication, thus improving
The luminous efficiency of quantum dot film, and then lift the brightness of backlight module and the display effect of liquid crystal display, promote high color
The development of domain liquid crystal display.
Polyether-ketone why is selected as polymeric matrix in the embodiment of the present invention, mainly due to：Polyether-ketone transparent
The optical properties such as property meet the requirement to polymeric matrix for the quantum dot film；And the modifying and decorating of polyether-ketone is relatively easy to, easily
Carboxyl side group is introduced in its molecular structure；Additionally, polyether-ketone also have higher degree of crystallinity, preferable resistance to elevated temperatures and
Higher rigidity, can play the effect of water oxygen obstruct, therefore, quantum based on quanta point material provided in an embodiment of the present invention
Water oxygen barrier layer can not be needed in point film, on the one hand can reduce the cost of quantum dot film, on the other hand improve quantum dot film
Light transmittance.
It will be appreciated by persons skilled in the art that in quanta point material provided in an embodiment of the present invention, can be according to reality
The specific composition needing selection quantum dot on border, such as CdSe, CdS, ZnSe or ZnS.
As a kind of optional embodiment of the embodiment of the present invention, can with the carboxyl side group in polyether-ketone molecule be first
A kind of part quantum dot of growth, then add the raw material of another quantum dot in gained system, thus forming core shell structure
Quantum dot.
In the embodiment of the present invention, can be gathered by being dissolved in polyether-ketone that is commercially available or having prepared in solvent
Ether ketone solution it is also possible to directly using polyether-ketone prepare when reaction system as polyether-ketone solution.
Inert gas in step 1 can be the inert gas commonly used in the art such as nitrogen, argon gas.
Further, in the embodiment of the present invention, there is the quantity of carboxyl side group and polyether-ketone in the polyether-ketone of carboxyl side group
The ratio of the quantity of construction unit be preferably 1:(1～4), for example, can be 1:1、1:2、1:3、1:4 etc..If carboxyl side group
Quantity and polyether-ketone the quantity of construction unit ratio excessive, that is, the carboxyl side group that has in polyether-ketone strand
Quantity is excessive, and quantum dot nano nucleus quantity can be made excessive, is easily caused quantum dot and reunites.If the quantity of carboxyl side group with
The ratio of the quantity of the construction unit of polyether-ketone is too small, that is, the quantity mistake of the carbonyl side base having in polyether-ketone strand
Few, quantum dot nano nucleus quantity can be made very few, may result in the brightness of quantum dot film based on this quanta point material relatively
Low.
Similarly, in the embodiment of the present invention, the acetate of II B race element with there is carboxyl in the polyether-ketone of carboxyl side group
The mol ratio of side base is preferably (0.5～1):1, can be for example 0.5:1、0.6:1、0.7:1、0.8:1、0.9:1、1:1 etc., selenium
Urea or thiocarbamide are slightly in excess in the acetate of II B race element, the mol ratio of selenourea or thiocarbamide and the acetate of II B race element
Can be (1～1.05):1.
Further, the emission wavelength of quantum dot changes with the carrying out of reaction, therefore, the embodiment of the present invention
In step 3, the emission wavelength of detection reaction system is detected, when the wavelength of reaction system reaches preset wavelength, you can
Stop reaction.The quantum dot used of generally liquid crystal display is red light quantum point and green light quantum point, and therefore, the present invention is real
Apply in example, preset wavelength is the corresponding wavelength of green glow or the corresponding wavelength of ruddiness, is specifically as follows 510nm～550nm, for example
510nm, 520nm, 530nm, 540nm, 550nm etc., or 610nm～650nm, such as 610nm, 620nm, 630nm, 640nm,
650nm etc..
The size of Quantum Dots Growth in the embodiment of the present invention, can be controlled by controlling reaction temperature, and then controlled quentity controlled variable
The emission wavelength of son point, for the quantum dot for liquid crystal display for the preparation, the preset temperature in step 2 can be
100 DEG C～175 DEG C, such as 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 175 DEG C etc., at this
In individual temperature range, between 2～10nm, emission wavelength is in visible-range for the particle diameter of quantum dot.Preset temperature specifically counts
Value needs to be determined according to different quantum dots, taking CdSe quantum dot as a example, the emission wavelength of the quantum dot generating at 130 DEG C
For 530nm about green, at 150 DEG C generate quantum dot emission wavelength be 625nm about redness.
Further, polyether-ketone can be divided into PAEK (PEAK), PEKK according to specific molecular structure
(PEKK), polyetherketoneetherketoneketone (PEKEKK), polyether ether ketone ketone (PEEKK) etc..Wherein contain benzene in PAEK molecular backbone
Ring, has higher rigidity, more preferable resistance to elevated temperatures and water and oxygen barrier property.Therefore, in the embodiment of the present invention, preferably with
The PAEK (the such as structure shown in formula (I)) with carboxyl side group as polymeric matrix, more preferably to have carboxyl side
The entirely fragrant type PAEK of base is as polymeric matrix.Carboxyl side group can be directly connected with PAEK main chain it is also possible to lead to
Cross other groups, such as alkyl chain, phenyl ring etc. are connected with PAEK main chain.In the embodiment of the present invention, carboxyl side group is preferably logical
Cross phenyl ring to be connected with PAEK main chain, carboxyl side group may be located at ortho position, contraposition or the meta of phenyl ring.In order to carry further
The rigidity of high PAEK, resistance to elevated temperatures and water and oxygen barrier property, can introduce naphthalene nucleus in PAEK molecular backbone.
Comprehensive the above, in quanta point material provided in an embodiment of the present invention, preferably to have as shown in following formula (II)
Chemical constitution entirely fragrant type PAEK as polymeric matrix：
Contain naphthalene nucleus in this full virtue type PAEK molecular structure, there is high-crystallinity, high compactness, high rigidity and good
Good resistance to elevated temperatures, can effectively play the effect of water oxygen obstruct, prevent quantum dot to lose efficacy because water oxygen contacts, based on this
Fragrant type PAEK does not need to arrange water oxygen barrier layer as the quantum dot film of the quanta point material of polymeric matrix entirely, thus dropping
The cost of low quantum dot film and improve the light transmittance of quantum dot film.
Second aspect, the embodiment of the present invention provides a kind of quanta point material preparing using above-mentioned preparation method.
Fig. 3 shows the structure of quanta point material provided in an embodiment of the present invention.As shown in figure 3, the embodiment of the present invention carries
For quanta point material in there is the polyether-ketone of carboxyl side group as polymeric matrix, quantum dot 12 is evenly distributed on carboxylic
On the strand 11 of the polyether-ketone of base side base, between quantum dot 12, there is no overlap, thus improving the amount based on this quanta point material
The luminous efficiency of son point film, and then lift the brightness of backlight module and the display effect of liquid crystal display.
The third aspect, the embodiment of the present invention provides a kind of quantum dot film, and referring to Fig. 4, this quantum dot film includes：By above-mentioned
The quantum dot layer 1 that quanta point material is formed；And, it is attached to the PET film lamella 2 on 1 two surfaces of quantum dot layer.
In quantum dot film provided in an embodiment of the present invention, the quantum dot 12 in quantum dot layer 1 is evenly distributed on carboxyl
On the strand 11 of the polyether-ketone of side base, between quantum dot 12, there is no overlap, therefore, this quantum dot film has higher luminous effect
Rate, thus lift backlight module brightness.
Simultaneously as polyether-ketone can play the effect of water oxygen obstruct, therefore, quantum dot film provided in an embodiment of the present invention
Middle can be it may not be necessary to water oxygen barrier layer, thus on the one hand reducing the one-tenth of quantum dot film using common optics PET film piece
This, on the other hand improve the light transmittance of quantum dot film.
Quantum dot film provided in an embodiment of the present invention can be prepared by following methods：
It is coated with quanta point material provided in an embodiment of the present invention on one layer of PET film lamella 2 first, when quanta point material is solid
After changing (being heating and curing or ultraviolet light polymerization) formation quantum dot layer 1, attaching another layer of PET film lamella 2, thus obtaining above-mentioned
Quantum dot film.
Be can be seen that due to quanta point material provided in an embodiment of the present invention by above-mentioned preparation method is quantum dot and polymerization
The composite of thing matrix, mixes the techniques such as glue during therefore eliminating traditional quantum dot film preparation, simplifies quantum dot film
Preparation technology, improves quantum dot film working (machining) efficiency, cost-effective.
In quantum dot film provided in an embodiment of the present invention, the emission wavelength of quanta point material used (is distributed in polyether-ketone
The emission wavelength of the quantum dot on strand) selected according to actual needs, for the quantum dot for liquid crystal display
For film, quanta point material is red light quantum point material and green light quantum point material.
Fourth aspect, the embodiment of the present invention provides a kind of backlight module, and this backlight module includes above-mentioned quantum dot film.
Specifically, referring to Fig. 5, backlight module provided in an embodiment of the present invention includes the backboard-reflector plate setting gradually
A, quantum dot film B, diaphragm group C and construction package D, wherein, quantum dot film B is quantum dot provided in an embodiment of the present invention
Film.Backboard-reflector plate A includes the assemblies such as backboard, lamp bar, light guide plate/diffuser plate, diffusion plate support, and diaphragm group C includes spreading
Piece, construction package includes glue frame fore shell etc..Concrete set-up mode in backlight module for the quantum dot film B adopts this area routine skill
Art means, will not be described here.
Because quantum dot film provided in an embodiment of the present invention has higher luminous efficiency, therefore, based on this quantum dot film
Backlight module there is higher brightness.
5th aspect, the embodiment of the present invention provides a kind of liquid crystal display, the backlight module in this liquid crystal display
For above-mentioned backlight module.
Due in backlight module provided in an embodiment of the present invention, there is higher brightness, be thus advantageous to improve the present invention in fact
The display performance of the liquid crystal display of example offer is provided.
Liquid crystal display described in the embodiment of the present invention is specifically as follows LCD TV, notebook computer screen, puts down
Any product with display function such as plate computer, mobile phone or part.Especially for ULED (Ultra Light
Emitting Diode) for TV, after applying backlight module provided in an embodiment of the present invention, not only there is higher colour gamut,
And because the brightness of backlight module is higher, it is possible to reduce the use of increment diaphragm, thus reducing the efficiency grade of ULED product,
Improve ULED product competitiveness.
Below by specific embodiment, technical scheme is described in detail.
In the examples below, raw materials used unreceipted production firm and specification person be can by city available from normal
Rule product.
Embodiment 1
The present embodiment provides a kind of quanta point material and preparation method thereof, and this quanta point material is to have shown in formula (II)
The entirely fragrant type PAEK with carboxyl side group as polymeric matrix, using the coordination growth in situ CdSe of carboxyl side group
Quantum dot, controls the distribution of CdSe quantum dot, makes CdSe quantum dot dispersed in polymeric matrix, prevent CdSe quantum dot
Reunite, meanwhile, the entirely fragrant type PAEK shown in formula (II) has high-crystallinity, high compactness, high rigidity and good resistance to
High-temperature behavior, can play a protective role to CdSe quantum dot, prevent CdSe quantum dot to lose efficacy because water oxygen contacts.
The preparation method of the quanta point material that the present embodiment provides is as follows：
Step 101, prepares the entirely fragrant type PAEK shown in above-mentioned formula (II) first, specific as follows：
Step 1011,0.1mol Isosorbide-5-Nitrae-naphthalenedicarboxylic acid (compound shown in formula (III)) is added in three-necked bottle and uses chlorine
Change sulfoxide dissolving, the Isosorbide-5-Nitrae-naphthalenedicarboxylic acid after being purified with re crystallization from toluene after heat backflow 24h, by the Isosorbide-5-Nitrae-naphthalene two after purification
Formic acid cryogenic vacuum is dried；
Step 1012, adds fluorobenzene 100g in the Isosorbide-5-Nitrae-naphthalenedicarboxylic acid after the purification obtaining to step 1011, at 0～4 DEG C
It is uniformly mixed, be then slowly added into AlCl3To saturation, after 1h is stirred at room temperature, reacts 10h at 80 DEG C, be subsequently cooled to
Room temperature；
Step 1013, is added in the system that step 1012 is obtained in appropriate hydrochloric acid solution, after separating out moisture, with steaming
The remaining grease of distilled water cleaning 8 times；
Step 1014, adds proper amount of methanol to separate out precipitation in the grease obtaining to step 1013, with toluene and DMF (N,
N '-dimethyl formamide) precipitation separating out is recrystallized, gained solid obtains Isosorbide-5-Nitrae-two (4- fluorobenzene acyl after 24h is dried
Base) naphthalene (compound shown in formula IV)；
Step 1015, by above-mentioned Isosorbide-5-Nitrae-two (4- fluorobenzene acyl) naphthalene 0.02mol and 3- trifluoromethylbenzene for hydroquinones (formula
(V) compound shown in) 0.02mol add reaction vessel in, add 0.02mol Anhydrous potassium carbonate, 0.02mol toluene and
0.02mol sulfolane, heats azeotropic, continues to be warming up to 200 DEG C after 2h removes water, reacts 6h, obtain containing methyl fluoride side chain
PAEK (compound shown in Formula IV), is subsequently adding the acidifying of appropriate carboxylic acid, trifluoromethyl is acidified obtain for carboxyl above-mentioned
The entirely fragrant type PAEK with carboxyl side group shown in formula (II).
Step 102, then prepares quanta point material provided in an embodiment of the present invention, specific as follows：
Step 1021, the PAEK shown in above-mentioned for 0.1mol formula (II) is dissolved in 20ml DMF and obtains PAEK
Solution, adds 0.02mol cadmium acetate, in N in gained PAEK solution2Lower stirring at normal temperature 2h of protection makes cadmium acetate and poly- virtue
Ether ketone mixes；
Step 1022, step 1021 gained reaction system is heated to preset temperature, is subsequently adding the selenium being dissolved in DMF
Urea, selenourea is 1.01 with the mol ratio of cadmium acetate:1；Wherein, prepare green light quantum point material and be then heated to 130 DEG C, prepare ruddiness
Quanta point material is then heated to 150 DEG C；
Step 1023, the emission wavelength of detecting step 1022 gained reaction system, when emission wavelength reaches preset wavelength simultaneously
When no longer changing, obtain final product the quanta point material of the present embodiment offer, the reaction time is 15min；Wherein, red light quantum point material
, near 625nm, the emission wavelength of green light quantum point material is near 530nm for the emission wavelength of material.
Embodiment 2
The present embodiment provides a kind of quanta point material and preparation method thereof, and this quanta point material is to have embodiment 1 Chinese style
(II) there is the entirely fragrant type PAEK of carboxyl side group as polymeric matrix shown in, the coordination using carboxyl side group is former
Position growth CdSe quantum dot, controls the distribution of CdSe quantum dot, makes CdSe quantum dot dispersed in polymeric matrix, prevent
CdSe quantum dot is reunited, meanwhile, the entirely fragrant type PAEK shown in formula (II) have high-crystallinity, high compactness, high rigidity with
And good resistance to elevated temperatures, CdSe quantum dot can be played a protective role, prevent CdSe quantum dot from losing because water oxygen contacts
Effect.
The preparation method of the quanta point material that the present embodiment provides is as follows：
Step 201, prepares the entirely fragrant type PAEK shown in above-mentioned formula (II) first, specific as follows：
Step 2011,0.1mol Isosorbide-5-Nitrae-naphthalenedicarboxylic acid (compound shown in formula (III) in embodiment 1) is added three necks
Dissolve in bottle and with thionyl chloride, the Isosorbide-5-Nitrae-naphthalenedicarboxylic acid after being purified with re crystallization from toluene after heat backflow 24h, after purifying
1,4- naphthalenedicarboxylic acid cryogenic vacuum dry；
Step 2012, adds fluorobenzene 100g in the Isosorbide-5-Nitrae-naphthalenedicarboxylic acid after the purification obtaining to step 2011, at 0～4 DEG C
It is uniformly mixed, be then slowly added into AlCl3To saturation, after 1h is stirred at room temperature, reacts 5h at 100 DEG C, be subsequently cooled to
Room temperature；
Step 2013, is added in the system that step 2012 is obtained in appropriate hydrochloric acid solution, after separating out moisture, with steaming
The remaining grease of distilled water cleaning 10 times；
Step 2014, adds proper amount of methanol to separate out precipitation in the grease obtaining to step 2013, with toluene and DMF (N,
N '-dimethyl formamide) precipitation separating out is recrystallized, gained solid obtains Isosorbide-5-Nitrae-two (4- fluorobenzene acyl after 24h is dried
Base) naphthalene (compound shown in formula (IV) in embodiment 1)；
Step 2015, will be (real for hydroquinones to above-mentioned Isosorbide-5-Nitrae-two (4- fluorobenzene acyl) naphthalene 0.02mol and 3- trifluoromethylbenzene
Apply the compound shown in formula (V) in example 1) 0.02mol add reaction vessel in, add 0.02mol Anhydrous potassium carbonate,
0.02mol toluene and 0.02mol sulfolane, heat azeotropic, continue to be warming up to 250 DEG C after 5h removes water, react 4h, contained
The PAEK (compound shown in formula (VI) in embodiment 1) of methyl fluoride side chain, is subsequently adding appropriate carboxylic acid acidifying, by trifluoro
Methyl acid turns to carboxyl and obtains the entirely fragrant type PAEK with carboxyl side group shown in above-mentioned formula (II).
Step 202, then prepares quanta point material provided in an embodiment of the present invention, specific as follows：
Step 2021, the PAEK shown in above-mentioned for 0.1mol formula (II) is dissolved in 20ml DMF and obtains PAEK
Solution, adds 0.03mol cadmium acetate, in N in gained PAEK solution2Lower stirring at normal temperature 2h of protection makes cadmium acetate and poly- virtue
Ether ketone mixes；
Step 2022, step 2021 gained reaction system is heated to preset temperature, is subsequently adding the selenium being dissolved in DMF
Urea, selenourea is 1.05 with the mol ratio of cadmium acetate:1；Wherein, prepare green light quantum point material and be then heated to 130 DEG C, prepare ruddiness
Quanta point material is then heated to 150 DEG C；
Step 2023, the emission wavelength of detecting step 2022 gained reaction system, when emission wavelength reaches preset wavelength simultaneously
When no longer changing, obtain final product the quanta point material of the present embodiment offer, the reaction time is 15min；Wherein, red light quantum point material
, near 625nm, the emission wavelength of green light quantum point material is near 530nm for the emission wavelength of material.
Embodiment 3
The present embodiment provides a kind of quanta point material and preparation method thereof, and this quanta point material is to have embodiment 1 Chinese style
(II) there is the entirely fragrant type PAEK of carboxyl side group as polymeric matrix shown in, the coordination using carboxyl side group is former
Position growth CdSe quantum dot, controls the distribution of CdSe quantum dot, makes CdSe quantum dot dispersed in polymeric matrix, prevent
CdSe quantum dot is reunited, meanwhile, the entirely fragrant type PAEK shown in formula (II) have high-crystallinity, high compactness, high rigidity with
And good resistance to elevated temperatures, CdSe quantum dot can be played a protective role, prevent CdSe quantum dot from losing because water oxygen contacts
Effect.
The preparation method of the quanta point material that the present embodiment provides is as follows：
Step 301, prepares the entirely fragrant type PAEK shown in above-mentioned formula (II) first, specific as follows：
Step 3011,0.1mol Isosorbide-5-Nitrae-naphthalenedicarboxylic acid (compound shown in formula (III) in embodiment 1) is added three necks
Dissolve in bottle and with thionyl chloride, the Isosorbide-5-Nitrae-naphthalenedicarboxylic acid after being purified with re crystallization from toluene after heat backflow 24h, after purifying
1,4- naphthalenedicarboxylic acid cryogenic vacuum dry；
Step 3012, adds fluorobenzene 100g in the Isosorbide-5-Nitrae-naphthalenedicarboxylic acid after the purification obtaining to step 3011, at 0～4 DEG C
It is uniformly mixed, be then slowly added into AlCl3To saturation, after 1h is stirred at room temperature, reacts 7h at 90 DEG C, be subsequently cooled to room
Temperature；
Step 3013, is added in the system that step 3012 is obtained in appropriate hydrochloric acid solution, after separating out moisture, with steaming
The remaining grease of distilled water cleaning 9 times；
Step 3014, adds proper amount of methanol to separate out precipitation in the grease obtaining to step 3013, with toluene and DMF (N,
N '-dimethyl formamide) precipitation separating out is recrystallized, gained solid obtains Isosorbide-5-Nitrae-two (4- fluorobenzene acyl after 24h is dried
Base) naphthalene (compound shown in above-mentioned formula (IV))；
Step 3015, will be (real for hydroquinones to above-mentioned Isosorbide-5-Nitrae-two (4- fluorobenzene acyl) naphthalene 0.02mol and 3- trifluoromethylbenzene
Apply the compound shown in formula (V) in example 1) 0.02mol add reaction vessel in, add 0.02mol Anhydrous potassium carbonate,
0.02mol toluene and 0.02mol sulfolane, heat azeotropic, continue to be warming up to 230 DEG C after 3h removes water, react 5h, contained
The PAEK (compound shown in formula (VI) in embodiment 1) of methyl fluoride side chain, is subsequently adding appropriate carboxylic acid acidifying, by trifluoro
Methyl acid turns to carboxyl and obtains the entirely fragrant type PAEK with carboxyl side group shown in above-mentioned formula (II).
Step 302, then prepares quanta point material provided in an embodiment of the present invention, specific as follows：
Step 3021, the PAEK shown in above-mentioned for 0.1mol formula (II) is dissolved in 20ml DMF and obtains PAEK
Solution, adds 0.04mol cadmium acetate, in N in gained PAEK solution2Lower stirring at normal temperature 2h of protection makes cadmium acetate and poly- virtue
Ether ketone mixes；
Step 3022, step 3021 gained reaction system is heated to preset temperature, is subsequently adding the selenium being dissolved in DMF
Urea, selenourea is 1.03 with the mol ratio of cadmium acetate:1；Wherein, prepare green light quantum point material and be then heated to 130 DEG C, prepare ruddiness
Quanta point material is then heated to 150 DEG C；
Step 3023, the emission wavelength of detecting step 3022 gained reaction system, when emission wavelength reaches preset wavelength simultaneously
When no longer changing, obtain final product the quanta point material of the present embodiment offer, the reaction time is 15min；Wherein, red light quantum point material
, near 625nm, the emission wavelength of green light quantum point material is near 530nm for the emission wavelength of material.
Embodiment 4
It is utilized respectively the quanta point material that above-described embodiment 1～3 prepares in the present embodiment and prepare quantum dot film, and right
The water and oxygen barrier property of gained quantum dot film and luminous efficiency are tested.
The method preparing quantum dot film using the quanta point material of embodiment 1～3 is as follows：
Above-mentioned quanta point material is coated with one layer of optics PET film piece, heating makes quanta point material solidify to form first
Quantum dot layer, then attach another layer of optics PET film piece, thus obtaining quantum dot film.
Water and oxygen barrier property is tested
OTR oxygen transmission rate according to the quantum dot film to the present embodiment for the method for ISO15105-2 is tested, result table
Bright, the quantum dot film of the quanta point material based on embodiment 1～3 oxygen under conditions of 23 DEG C of temperature, relative humidity 90%
Transmitance (OTR) is all 5 × 10-3ml/(m2× day × Mpa) below.
Moisture-vapor transmission according to the quantum dot film to the present embodiment for the method for ISO151066-2 is tested, result
Show, the quantum dot film of the quanta point material based on embodiment 1～3 water under conditions of 40 DEG C of temperature, relative humidity 100%
Vapor transmission rates (WVTR) are all 5 × 10-2g/(m2× day) below.
Above-mentioned quantum dot film and the part such as backboard, lamp bar, light guide plate are assembled into backlight module, after lighting backlight, survey
The colourity change of examination backlight and brightness decay situation.Result shows, the backlight module of the quanta point material based on embodiment 1～3
Backlight colourity change all within 0.008, brightness decay is within 5%.
It is seen from the above data that being had well based on the quantum dot film of quanta point material provided in an embodiment of the present invention
Water oxygen barrier, using common optics PET film, on the one hand greatly reduce the cost of quantum dot film, on the other hand
Be conducive to increasing the light transmittance of quantum dot film.
Luminous efficiency is tested
The part such as quantum dot film and backboard, lamp bar, light guide plate is assembled into backlight module, using CS-2000 type light splitting spoke
Penetrate luminance meter and test the power of blue light backlight and the power of the light through quantum dot film respectively, through the power of the light of quantum dot film
It is the luminous efficiency of quantum dot film with the ratio of the power of blue light backlight.Specifically test process is：
Blue backlight is placed on the board of CS-2000 type spectroradio luminance meter, by the quantum dot film in backlight module
Take out, replace with and quantum dot film mist degree identical diffusion sheet, test is using the light work(of the central point of backlight module of diffusion sheet
Rate, the power of as above-mentioned blue light backlight, result is 300mW m-2；Then diffusion sheet is taken out from backlight module, will be by reality
Apply the quantum dot film that the quanta point material of example 1～3 prepares to be reinstalled in backlight module, the central point of test backlight module
Luminous power, the power of the light of as above-mentioned transmission quantum dot film, the test result of the quantum dot film of 3 embodiments is averaged
For 120mW m-2, thus can obtain, the luminous efficiency of the quantum dot film based on quanta point material provided in an embodiment of the present invention is
40%.
According to above-mentioned method of testing, the luminous efficiency of existing quantum dot film is tested.
In existing quantum dot film, quantum dot adopts CdSe quantum dot, and polymeric matrix adopts polymethyl methacrylate
(PMMA) be coated on after, CdSe quantum dot being mixed with PMMA one layer of water oxygen Obstruct membrane (surface covering aluminum oxide coating
PET film) on, attach another layer of water oxygen Obstruct membrane again after PMMA solidification, obtain existing common quantum dot film.Wherein, CdSe
The mass ratio of quantum dot and PMMA is respectively according to the quality of quantum dot in the quanta point material of embodiment 1～3 and polymeric matrix
Ratio setting, in the quanta point material of embodiment 1～3, quantum dot and the mass ratio of polymeric matrix are according to feeding intake in preparation process
Ratio is calculated.
Mean value using the luminous power of the central point of the backlight module of existing common quantum dot film is 102mW m-2,
Thus can obtain, the luminous efficiency of existing quantum dot film is 34%.
Can be seen that the quantum dot film based on quanta point material provided in an embodiment of the present invention preparation from above test result
In, because quantum dot is uniformly dispersed and not using water oxygen Obstruct membrane, therefore luminous efficiency is compared with existing quantum dot film
Improve 17%, be conducive to lifting the brightness of backlight module, reduce the power consumption of liquid crystal display.
To sum up, the embodiment of the present invention has prepared a kind of quantum dot using the method for fabricated in situ and has had carboxyl side group
Polyether-ketone be combined quanta point material.Using the carboxyl in the polyether-ketone molecule with carboxyl side group as joining that quantum dot synthesizes
Body, controls the growth of quantum dot, makes quantum dot dispersed in polymeric matrix, prevents quantum dot from reuniting, reduces quantum dot
Duplication, thus improving the luminous efficiency of quantum dot film, and then the brightness of lifting backlight module, be conducive to raising liquid crystal display to set
Standby display effect, also helps the power consumption reducing liquid crystal display.Meanwhile, quanta point material provided in an embodiment of the present invention
Also there is water and oxygen barrier property, particularly using PAEK as the water and oxygen barrier property of the quanta point material of polymeric matrix more
Good, so that quantum dot film does not need water oxygen barrier layer, significantly reduce the cost of quantum point, and save after water oxygen barrier layer also
The light transmittance of quantum dot film can be improved, improve the display effect of liquid crystal display further, be conducive to high colour gamut liquid crystal
Show the development of equipment.
The above is for only for ease of those skilled in the art and understands technical scheme, not in order to limit
The present invention.All any modification, equivalent substitution and improvement within the spirit and principles in the present invention, made etc., should be included in this
Within the protection domain of invention.
Claims (10)
1. a kind of preparation method of quanta point material is it is characterised in that comprise the following steps：
Step a, adds the acetate of II B race element, in the polyether-ketone solution have carboxyl side group under inert gas shielding
It is uniformly mixed；Described II B race element is cadmium or zinc；
Step b, the temperature of the reaction system that described step a is obtained is heated to preset temperature；
Step c, addition selenourea or thiocarbamide in the reaction system obtaining to described step b, and detect the emission wavelength of reaction system,
When the emission wavelength of reaction system reaches preset wavelength, that is, obtain described quanta point material.
2. preparation method according to claim 1 is it is characterised in that carboxyl side in the described polyether-ketone with carboxyl side group
The ratio of the quantity of the construction unit of the quantity of base and described polyether-ketone is 1:(1～4)；The acetate of described II B race element with
In the described polyether-ketone with carboxyl side group, the mol ratio of carboxyl side group is (0.5～1):1；Described selenourea or thiocarbamide and described II
The mol ratio of the acetate of B race element is (1～1.05):1.
3. preparation method according to claim 1 it is characterised in that preset wavelength in described step c be 510nm～
550nm or 610nm～650nm；Described preset temperature in described step b is 100 DEG C～175 DEG C.
4. the preparation method according to any one of claims 1 to 3 is it is characterised in that the described polyethers with carboxyl side group
Ketone is the PAEK with carboxyl side group.
5. preparation method according to claim 4 is it is characterised in that carboxyl in the described PAEK with carboxyl side group
Side base is connected with PAEK main chain by phenyl ring；Contain in the PAEK main chain of the described PAEK with carboxyl side group
Naphthalene nucleus.
6. preparation method according to claim 5 is it is characterised in that the chemistry of the described PAEK with carboxyl side group
Structure is as follows：
7. the quanta point material that the preparation method described in a kind of any one using claim 1～6 prepares.
8. a kind of quantum dot film is it is characterised in that include：
The quantum dot layer being formed by the quanta point material described in claim 7；
And,
It is attached to the PET film lamella on described two surfaces of quantum dot layer.
9. a kind of backlight module is it is characterised in that include the quantum dot film described in claim 8.
10. a kind of liquid crystal display is it is characterised in that include the backlight module described in claim 9.
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| CN107359264A (en) * | 2017-08-03 | 2017-11-17 | 青岛海信电器股份有限公司 | A kind of QLED, preparation method and display device |
| CN107359264B (en) * | 2017-08-03 | 2019-12-31 | 青岛海信电器股份有限公司 | QLED, preparation method and display device |
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| CN111638573A (en) * | 2019-03-01 | 2020-09-08 | 苏州星烁纳米科技有限公司 | Quantum dot polaroid and display device |
| CN111638573B (en) * | 2019-03-01 | 2022-12-02 | 苏州星烁纳米科技有限公司 | Quantum dot polaroid and display device |
| CN111665586A (en) * | 2019-03-08 | 2020-09-15 | 苏州星烁纳米科技有限公司 | Quantum dot polaroid and display device |
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Address after: 266555 Qingdao economic and Technological Development Zone, Shandong, Hong Kong Road, No. 218 Patentee after: Hisense Video Technology Co., Ltd Address before: 266555 Qingdao economic and Technological Development Zone, Shandong, Hong Kong Road, No. 218 Patentee before: HISENSE ELECTRIC Co.,Ltd. |