CN108546379A - Organic-inorganic composite Photoluminescence thin film and its preparation method and application - Google Patents
Organic-inorganic composite Photoluminescence thin film and its preparation method and application Download PDFInfo
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- CN108546379A CN108546379A CN201810671514.8A CN201810671514A CN108546379A CN 108546379 A CN108546379 A CN 108546379A CN 201810671514 A CN201810671514 A CN 201810671514A CN 108546379 A CN108546379 A CN 108546379A
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Abstract
The present invention provides a kind of organo-mineral complexing Photoluminescence thin films and its preparation method and application, belong to light function and service thin film technique field.Above-mentioned organo-mineral complexing Photoluminescence thin film includes the oxide particles with perovskite structure of polyvinylidene difluoride film and rare earth doped element；The oxide particles with perovskite structure of rare earth doped element is dispersed in polyvinylidene difluoride film；The oxide particles with perovskite structure of rare earth doped element：The volume ratio of polyvinylidene difluoride film is 1:3~12.The film has many advantages, such as that flexibility is big, transparency is high, dielectric properties are good and stability is high, and luminescent color can change as excitation wavelength changes.Organo-mineral complexing Photoluminescence thin film preparation method operating process provided by the invention is simple, and experimentation is easily controllable, low production cost, and film is efficient, is suitble to large-scale production.Organo-mineral complexing Photoluminescence thin film provided by the invention can be used in password transmission, illumination or display field.
Description
Technical field
The present invention relates to light function and service thin film technique fields, in particular to a kind of photic hair of Organic-inorganic composite
Optical thin film and its preparation method and application.
Background technology
Luminescence generated by light laminated film has the superiority of conventional composite thin-film material, and the introducing of luminescent material assigns film
Good optical property has become a research hotspot of field of functional materials at present.Luminescence generated by light laminated film is in film
Surface or it is internal introduce luminescent material, as some semiconductive luminescent materials, organic molecule fluorescent material and rare earth coordinate
Object etc., and then luminescence generated by light laminated film can have good optical property.
The main film body matrix of traditional luminescence generated by light laminated film is frequently with organic modified silicate and polyacrylonitrile etc.
High-molecular organic material, but main film body matrix generally existing made of these organic polymers is flexible less, transparency is not high
The shortcomings of.Semiconductive luminescent materials are using relatively broad, but the problems such as generally existing luminous efficiency is low, stability is poor；It is organic
Small molecule is lacked as electroluminescent material although the luminous efficiency for overcoming inorganic semiconductor luminescent material is low, stability is poor
Point, but since organic small molecule material is easy crystallization during electroluminescent, the stability of body is poor, actual application
Also fewer；Rare earth compounding has the advantages that luminous intensity is big and monochromaticjty is good, but there is photostability and thermal stability
Poor problem.
Therefore, a kind of performance stabilization is developed, the good Photoluminescence thin film of illumination effect has very important significance
With huge application value.
In view of this, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of Organic-inorganic composite Photoluminescence thin film, including Kynoar
The oxide particles with perovskite structure of the oxide particles with perovskite structure of film and rare earth doped element, rare earth doped element is equal
It is even to be scattered in polyvinylidene difluoride film.The Organic-inorganic composite Photoluminescence thin film has flexible big, transparency height, dielectric
Functional, the advantages that luminous efficiency is high and stability is high.
The second object of the present invention is to provide a kind of preparation method of Organic-inorganic composite Photoluminescence thin film, the system
Preparation Method operating process is simple, and experimentation is easily controllable, low production cost, and film is efficient, is suitble to large-scale production.
The third object of the present invention is to provide a kind of Organic-inorganic composite Photoluminescence thin film in password transmission, illumination
Or the purposes in display field.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
In a first aspect, the present invention provides a kind of Organic-inorganic composite Photoluminescence thin film, including polyvinylidene difluoride film
With the oxide particles with perovskite structure of rare earth doped element；The oxide particles with perovskite structure of the rare earth doped element is equal
It is even to be scattered in the polyvinylidene difluoride film；
The oxide particles with perovskite structure of rare earth doped element：The volume ratio of polyvinylidene difluoride film is 1:3~12.
Preferably, on the basis of technical solution provided by the invention, the perovskite structure oxide of rare earth doped element
Particle：The volume ratio of polyvinylidene difluoride film is 1:4~10；
It is further preferred that the oxide particles with perovskite structure of rare earth doped element：The volume of polyvinylidene difluoride film
Than being 1:6~10.
Preferably, on the basis of technical solution provided by the invention, the perovskite structure oxide of rare earth doped element
Chemical general formula be ABO3Or ReABO3, wherein Re is rare earth element, and A is alkaline earth element, and B is transition elements；
Preferably, one kind in Re Nd, Sm, Eu, Gd, Dy, Ho or Pr；
Preferably, one kind in A Be, Mg, Ca, Sr, Ba or Ra；
Preferably, one kind in B Ti, V, Cr, Mn or Co；
Preferably, perovskite structure oxide CaTiO3、BaTiO3Or SrTiO3。
Preferably, on the basis of technical solution provided by the invention, the perovskite structure oxide of rare earth doped element
In the standard cube of the length of side≤30nm, or in the cube of curved edge or spherical in shape.
Preferably, on the basis of technical solution provided by the invention, the perovskite structure oxide of rare earth doped element
Particle is prepared using collosol-precipitation method；
Preferably, the preparation method of the oxide particles with perovskite structure of rare earth doped element, includes the following steps：
(a) alkaline earth metal hydroxide, coupling agent, alkali metal hydroxide, rare earth element soluble-salt and solvent are mixed
It closes uniform；
(b) by mixed solution under the conditions of 155-165 DEG C oil bath heating 1.5-2.5h, obtain rare earth doped
Perovskite structure oxide colloidal sol；
(c) it by the compound colloidal sol water sedimentation of perovskite oxide structure and cleans, by the material after cleaning under the conditions of 75-85 DEG C
Dry 20-30h, obtains oxide particles with perovskite structure；
Preferably, alkaline earth metal hydroxide includes one kind in strontium hydroxide, calcium hydroxide or barium hydroxide；
Preferably, coupling agent includes that butyl titanate, three oleic acid acyloxy titanate esters of isopropyl or three hydroxy acyl metatitanic acids are different
One kind in propyl ester；
Preferably, alkali metal hydroxide includes one kind in lithium hydroxide, sodium hydroxide or potassium hydroxide；
Preferably, solvent includes one kind in polyvinylpyrrolidone, triethylene glycol or glycol ether.
Preferably, on the basis of technical solution provided by the invention, the thickness of Organic-inorganic composite Photoluminescence thin film
For 0.01~0.08mm, preferably 0.01~0.05mm, further preferably 0.01~0.03mm.
Second aspect, the present invention provides a kind of preparation method of Organic-inorganic composite Photoluminescence thin film, including it is following
Step：
The luminescence generated by light masking liquid obtained after mineral crystal particle precursor liquid and organic polymer precursor liquid are mixed is consolidated
Change, obtains Organic-inorganic composite Photoluminescence thin film；
Wherein, mineral crystal particle precursor liquid is the oxide particles with perovskite structure and N of rare earth doped element, N- diformazans
Base formamide obtains after mixing；Organic polymer precursor liquid is that Kynoar and n,N-Dimethylformamide mixing are equal
It is obtained after even.
Preferably, on the basis of technical solution provided by the invention, the perovskite structure oxide of rare earth doped element
Particle：The mass ratio of n,N-Dimethylformamide is 1:5~10；
It is further preferred that the oxide particles with perovskite structure of rare earth doped element：The matter of n,N-Dimethylformamide
Amount is than being 1:6~8.
Preferably, Kynoar：The mass ratio of N, N-METHYLFORMAMIDE are 1:6~12；
It is further preferred that Kynoar：The mass ratio of N, N-METHYLFORMAMIDE are 1:8~10.
Preferably, on the basis of technical solution provided by the invention, the preparation of Organic-inorganic composite Photoluminescence thin film
Method includes the following steps：
(a) oxide particles with perovskite structure of rare earth doped element is added in n,N-Dimethylformamide, ultrasound
Disperse 20-50min, forms mineral crystal particle precursor liquid；
(b) Kynoar is added in n,N-Dimethylformamide, mixes 80-150min, form organic polymer
Precursor liquid；
(c) mineral crystal particle precursor liquid is added in organic polymer precursor liquid, is uniformly mixed, form luminescence generated by light
Masking liquid；
(d) it is coated with the mold of luminescence generated by light masking liquid or solidification, 60-80 DEG C of dry 100- is dried in container
120min removes the Organic-inorganic composite Photoluminescence thin film after solidification from mold or container, and it is multiple to obtain organic and inorganic
Close Photoluminescence thin film；
Preferably, painting method includes the tape casting, spin coating method, spray coating method or brushing method.
The third aspect, the present invention provides a kind of Organic-inorganic composite Photoluminescence thin films in password transmission, illumination or to show
Show the purposes in field.
Compared with prior art, beneficial effects of the present invention are：
(1) present invention provides a kind of Organic-inorganic composite Photoluminescence thin film, including polyvinylidene difluoride film and adulterates dilute
The oxide particles with perovskite structure of earth elements.By select Kynoar based on matrix make film provided by the invention
Have many advantages, such as that flexibility is big, frivolous, dielectric properties are good, passes through the oxide particles with perovskite structure for selecting rare earth doped element
With polyvinylidene difluoride film it is compound so that Organic-inorganic composite Photoluminescence thin film is had luminous efficiency is high, stability is high and luminous
The advantages that color is various.
(2) preparation method of Organic-inorganic composite Photoluminescence thin film provided by the invention has operating process simple,
The advantages that experimentation is easily controllable, low production cost, and film is efficient, suitable large-scale production.
(3) Organic-inorganic composite Photoluminescence thin film provided by the invention can generate effectively under ultraviolet excitation
VISIBLE LIGHT EMISSION, while exciting light is different, luminescent color can also change, and can be used in password transmission, illumination or display field,
Advertisement or handicraft etc. can be made.
(4) Organic-inorganic composite Photoluminescence thin film provided by the invention can widen the use scope of embedded photoluminescent material,
There is important role for rare earth luminescent material device.
Description of the drawings
Fig. 1 is the stereoscan photograph of Photoluminescence thin film in embodiment 3, and wherein a is Organic-inorganic composite luminescence generated by light
The cross section transverse stereoscan photograph of film, b are the stereoscan photograph on Organic-inorganic composite Photoluminescence thin film surface；
Fig. 2 is the X-ray diffractogram of Organic-inorganic composite Photoluminescence thin film in embodiment 3；
Fig. 3 is the EDS energy spectrum diagrams of Organic-inorganic composite Photoluminescence thin film in embodiment 4；
Fig. 4 is the exciting light spectrogram of Organic-inorganic composite Photoluminescence thin film in embodiment 3；
Fig. 5 is the launching light spectrogram of Organic-inorganic composite Photoluminescence thin film in embodiment 3；
Fig. 6 is the fluorescence lifetime figure of Organic-inorganic composite Photoluminescence thin film in embodiment 3；
Fig. 7 is that the dielectric and loss angle tangent of Organic-inorganic composite Photoluminescence thin film in embodiment 3 change with frequency
Figure；
Fig. 8 is the exciting light spectrogram of Organic-inorganic composite Photoluminescence thin film in embodiment 4；
Fig. 9 is the launching light spectrogram of Organic-inorganic composite Photoluminescence thin film in embodiment 4；
Figure 10 is that the dielectric and loss angle tangent of Organic-inorganic composite Photoluminescence thin film in embodiment 4 change with frequency
Figure；
Figure 11 is the exciting light spectrogram of Organic-inorganic composite Photoluminescence thin film in embodiment 5；
Figure 12 is the launching light spectrogram of Organic-inorganic composite Photoluminescence thin film in embodiment 5；
Figure 13 is that the emission spectrum that Organic-inorganic composite Photoluminescence thin film measures in comparative example 3 compares figure；
Figure 14 be embodiment 3 in by Organic-inorganic composite Photoluminescence thin film be curled into it is rodlike after photo.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
According to the first aspect of the invention, a kind of Organic-inorganic composite Photoluminescence thin film is provided, including gathers inclined fluorine
The oxide particles with perovskite structure of vinyl film and rare earth doped element；The perovskite structure oxide of rare earth doped element
Grain is dispersed in polyvinylidene difluoride film；The oxide particles with perovskite structure of rare earth doped element：Kynoar is thin
The volume ratio of film is 1:3~12.
Polyvinylidene difluoride film is the thin-film body cured by Kynoar.
Preferably, the chemical general formula of the perovskite structure oxide of rare earth doped element is ABO3Or ReABO3, wherein Re is
Rare earth element, A are alkaline earth element, and B is transition elements；
Preferably, one kind in Re Nd, Sm, Eu, Gd, Dy, Ho or Pr；
Preferably, one kind in A Be, Mg, Ca, Sr, Ba or Ra；
Preferably, one kind in B Ti, V, Cr, Mn or Co；
Typical but non-limiting perovskite structure oxide is, for example, CaTiO3、BaTiO3Or SrTiO3。
Perovskite structure oxide as a kind of common material, by performances such as its superior dielectric, piezoelectricity by
Extensive concern.After doping with rare-earth ions, perovskite structure oxide can launch the visible light of different colours.
The oxide particles with perovskite structure of rare earth doped element：The volume ratio of polyvinylidene difluoride film is typical but unrestricted
Property is for example:1:3、1:4、1:5、1:6、1:7、1:8、1:9、1:10、1:11 or 1:12.
The present invention selects Kynoar as organic main body matrix so that thin-film material has preferable flexibility, together
When also have good dielectric properties；The oxide particles with perovskite structure of rare earth doped element may be implemented in different wavelengths of light
Under excitation, film launches the light of different colours；The perovskite structure oxide of the preferably rare earth doped element of luminescent properties is same
Kynoar carries out compound, flexible big, the stability height of formation, dielectric properties and the good Organic-inorganic composite of luminescent properties
Photoluminescence thin film.
It is preferably carried out in mode in one kind, the oxide particles with perovskite structure of rare earth doped element：Kynoar
The volume ratio of film is 1:4~10；
Preferably, the oxide particles with perovskite structure of rare earth doped element：The volume ratio of polyvinylidene difluoride film is 1:6
~10.
By the oxide particles with perovskite structure for advanced optimizing rare earth doped element：The volume of polyvinylidene difluoride film
Than that can make the Organic-inorganic composite Photoluminescence thin film obtained by preparation that there is better luminescent properties and stability.
It is preferably carried out in mode in one kind, the perovskite structure oxide of rare earth doped element is in the mark of the length of side≤30nm
Pseudo-cubic, or in the cube of curved edge or spherical in shape.
Using the particle of the perovskite structure oxide of uniform rare earth doped element, is conducive to it and is evenly distributed on
In polymer matrix.
It is preferably carried out in mode in one kind, the oxide particles with perovskite structure of rare earth doped element is heavy using colloidal sol-
It is prepared by shallow lake method；
Preferably, the preparation method of the oxide particles with perovskite structure of rare earth doped element, includes the following steps：
(a) alkaline earth metal hydroxide, coupling agent, alkali metal hydroxide, rare earth element soluble-salt and solvent are mixed
It closes uniform；
(b) by mixed solution under the conditions of 155-165 DEG C oil bath heating 1.5-2.5h, it is molten to obtain perovskite oxide
Glue；
(c) it by the water sedimentation of perovskite oxide colloidal sol and cleans, the material after cleaning is dry under the conditions of 75-85 DEG C
20-30h obtains oxide particles with perovskite structure；
Preferably, alkaline earth metal hydroxide includes one kind in strontium hydroxide, calcium hydroxide or barium hydroxide；
Preferably, coupling agent includes that butyl titanate, three oleic acid acyloxy titanate esters of isopropyl or three hydroxy acyl metatitanic acids are different
One kind in propyl ester；
Preferably, alkali metal hydroxide includes one kind in lithium hydroxide, sodium hydroxide or potassium hydroxide；
Preferably, solvent includes one kind in polyvinylpyrrolidone, triethylene glycol or glycol ether.
Collosol-precipitation method is to send out the presoma (such as silylating reagent, metal alkoxide) of facile hydrolysis with water in a solvent
Colloidal sol is made by hydrolysis and polycondensation process in raw reaction, and further polycondensation obtains gel.
Oil bath heating temperature it is typical but non-limiting be, for example, 155 DEG C, 156 DEG C, 157 DEG C, 158 DEG C, 159 DEG C, 160
DEG C, 161 DEG C, 162 DEG C, 163 DEG C, 164 DEG C or 165 DEG C；
The typical but non-limiting oil bath heating time is, for example, 1.5h, 1.8h, 2h, 2.3h or 2.5h；
Drying temperature it is typical but non-limiting be, for example, 75 DEG C, 76 DEG C, 77 DEG C, 78 DEG C, 79 DEG C, 80 DEG C, 81 DEG C, 82
DEG C, 83 DEG C, 84 DEG C or 85 DEG C；
Drying time it is typical but non-limiting be, for example, 20h, 21h, 22h, 23h, for 24 hours, 25h, 26h, 27h, 28h, 29h
Or 30h.
The oxide particles with perovskite structure of rare earth doped element can be prepared by above-mentioned preparation method, preferably make
The raw material used in Preparation Method can be the rare earth doped element being prepared oxide particles with perovskite structure size it is uniform,
Good luminous performance.
It is preferably carried out in mode in one kind, the thickness of Organic-inorganic composite Photoluminescence thin film is 0.01~0.08mm；
The thickness of film is typical but non-limiting be, for example, 0.01mm, 0.02mm, 0.03mm, 0.04mm, 0.05mm,
0.06mm, 0.07mm or 0.08mm；
The thickness of control Organic-inorganic composite Photoluminescence thin film can control the flexibility and transparency of film.
According to the second aspect of the invention, a kind of preparation method of Organic-inorganic composite Photoluminescence thin film is provided,
Include the following steps：
The luminescence generated by light masking liquid obtained after mineral crystal particle precursor liquid and organic polymer precursor liquid are mixed is consolidated
Change, obtains Organic-inorganic composite Photoluminescence thin film；
Wherein, mineral crystal particle precursor liquid is the oxide particles with perovskite structure and N of rare earth doped element, N- diformazans
Base formamide obtains after mixing；Organic polymer precursor liquid is that Kynoar and n,N-Dimethylformamide mixing are equal
It is obtained after even.
The preparation method of Organic-inorganic composite Photoluminescence thin film provided by the invention has low production cost, experiment
The advantages that process is easily controllable, suitable large-scale production.
It is preferably carried out in mode in one kind, the oxide particles with perovskite structure of rare earth doped element：N, N- dimethyl
The mass ratio of formamide is 1:5~10, further preferably 1:6~8；
The oxide particles with perovskite structure of rare earth doped element：The mass ratio of n,N-Dimethylformamide is typical but non-limit
Property processed is, for example, 1:5、1:6、1:7、1:8、1:9 or 1:10.
Pass through the further preferably oxide particles with perovskite structure of rare earth doped element and n,N-Dimethylformamide
Mass ratio can make in mineral crystal particle precursor liquid distribution of particles evenly.
It is preferably carried out in mode in one kind, Kynoar：The mass ratio of N, N-METHYLFORMAMIDE are 1:6~12, into
One step is preferably 1:8~10；
Kynoar：N, the typical but non-limiting mass ratio of N-METHYLFORMAMIDE is, for example, 1:6、1:7、1:8、1:
9、1:10、1:11 or 1:12.
By further preferred Kynoar and N, the mass ratio of N methylformamide can make the THIN COMPOSITE being prepared
Film keeps preferable dielectric properties.
It is preferably carried out in mode in one kind, the preparation method of Organic-inorganic composite Photoluminescence thin film, including following step
Suddenly：
(a) oxide particles with perovskite structure of rare earth doped element is added in n,N-Dimethylformamide, ultrasound
Disperse 20-50min, forms mineral crystal particle precursor liquid；
(b) Kynoar is added in n,N-Dimethylformamide, mixes 80-150min, form organic polymer
Precursor liquid；
(c) mineral crystal particle precursor liquid is added in organic polymer precursor liquid, is uniformly mixed, form luminescence generated by light
Masking liquid；
(d) it is coated with the mold of luminescence generated by light masking liquid or solidification, 60-80 DEG C of dry 100- is dried in container
120min removes the Organic-inorganic composite Photoluminescence thin film after solidification from mold or container, and it is multiple to obtain organic and inorganic
Close Photoluminescence thin film.
Ultrasonic disperse can make the oxide particles with perovskite structure of rare earth doped element rapidly and uniformly be distributed in N, N-
In dimethylformamide, the ultrasonic disperse time is typical but non-limiting for example,：20min、25min、30min、35min、
40min, 45min or 50min；
Mixing can be such that Kynoar is uniformly dissolved in n,N dimethylformamide, incorporation time typical case but non-limit
Property processed is, for example, 80min, 90min, 100min, 110min, 120min, 130min, 140min or 150min；
Freeze-day with constant temperature can make the quick curing molding of luminescence generated by light masking liquid of coating, shorten the production time, drying temperature
It is typical but non-limiting be, for example, 60 DEG C, 61 DEG C, 62 DEG C, 63 DEG C, 64 DEG C, 65 DEG C, 66 DEG C, 67 DEG C, 68 DEG C, 69 DEG C, 70 DEG C,
71 DEG C, 72 DEG C, 73 DEG C, 74 DEG C, 75 DEG C, 76 DEG C, 77 DEG C, 78 DEG C, 79 DEG C or 80 DEG C；
Drying time it is typical but non-limiting be, for example, 100min, 101min, 102min, 103min, 104min,
105min、106min、107min、108min、109min、110min、111min、112min、113min、114min、115min、
116min, 117min, 118min, 119min or 120min；
Preferably, painting method includes the tape casting, spin coating method, spray coating method or brushing method.
Coating is that luminescence generated by light masking liquid is added in mold or container, is formed on its surface a kind of film layer, the present invention
In painting method the thicknesses of layers to be formed can be made uniform, area is big, stability is high.
According to the third aspect of the present invention, provide a kind of Organic-inorganic composite Photoluminescence thin film transmit in password,
Purposes in illumination or display field.
Organic-inorganic composite Photoluminescence thin film can generate effective visible light hair under ultraviolet excitation in the present invention
It penetrates, while exciting light is different, luminescent color can also change, and can be used in password transmission, illumination or display field, can also make
Advertisement or handicraft etc..
In password transmission field, it can be used for password transition material and password screen display material；
In lighting area, can be used in the light source device of LED lamp, charactron and LED backlight；
In display field, it can be used for computer display screen, mobile phone display screen or tv display screen.
In order to further appreciate that the present invention, the method for the present invention and effect are done further in detail with reference to specific embodiment
Explanation.Each raw material of the present invention can pass through commercially available acquisition.
Embodiment 1
A kind of Organic-inorganic composite Photoluminescence thin film, including polyvinylidene difluoride film and doping Pr3+SrTiO3
Grain；Adulterate Pr3+SrTiO3Even particulate dispersion is in polyvinylidene difluoride film；
Adulterate Pr3+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is 1:3.
The preparation method of above-mentioned Organic-inorganic composite Photoluminescence thin film, includes the following steps：
(1) by the doping Pr after annealing3+SrTiO3Particle is added in n,N-Dimethylformamide, ultrasonic disperse
20min forms mineral crystal particle precursor liquid；
(2) Kynoar is added in n,N-Dimethylformamide, mixes 80min, form organic polymer forerunner
Liquid；
(3) Pr will be adulterated3+SrTiO3Particle precursor liquid is added in organic polymer precursor liquid, is uniformly mixed, and is formed
Luminescence generated by light masking liquid；
(4) luminescence generated by light masking liquid is coated uniformly on using curtain coating cladding process above the sheet glass of surfacing；
(5) it is coated with the mold of luminescence generated by light masking liquid or solidification is dried in container, 60 DEG C of dry 120min will consolidate
Organic-inorganic composite Photoluminescence thin film after change is removed from mold or container, and it is thin to obtain Organic-inorganic composite luminescence generated by light
Film；
Wherein, Pr is adulterated3+SrTiO3Particle and the mass ratio of n,N dimethylformamide are 1:5；
The mass ratio of Kynoar and N, N methylformamide are 1:6.
Embodiment 2
A kind of Organic-inorganic composite Photoluminescence thin film, including polyvinylidene difluoride film and doping Pr3+SrTiO3
Grain；Adulterate Pr3+SrTiO3Even particulate dispersion is in polyvinylidene difluoride film；
Adulterate Pr3+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is 1:12.
The preparation method of above-mentioned Organic-inorganic composite Photoluminescence thin film, includes the following steps：
(1) by the doping Pr after annealing3+SrTiO3Particle is added in n,N-Dimethylformamide, ultrasonic disperse
50min forms mineral crystal particle precursor liquid；
(2) Kynoar is added in n,N-Dimethylformamide, mixes 120min, form organic polymer forerunner
Liquid；
(3) mineral crystal particle precursor liquid is added in organic polymer precursor liquid, is uniformly mixed, form luminescence generated by light
Masking liquid；
(4) luminescence generated by light masking liquid is coated uniformly on using curtain coating cladding process above the sheet glass of surfacing；
(5) it is coated with the mold of luminescence generated by light masking liquid or solidification is dried in container, 80 DEG C of dry 100min will consolidate
Organic-inorganic composite Photoluminescence thin film after change is removed from mold or container, and it is thin to obtain Organic-inorganic composite luminescence generated by light
Film；
Wherein, Pr is adulterated3+SrTiO3Particle and the mass ratio of n,N dimethylformamide are 1:10；
The mass ratio of Kynoar and N, N methylformamide are 1:8.
Embodiment 3
A kind of Organic-inorganic composite Photoluminescence thin film, including polyvinylidene difluoride film and doping Pr3+SrTiO3
Grain；Adulterate Pr3+SrTiO3Even particulate dispersion is in polyvinylidene difluoride film；
Adulterate Pr3+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is 1:6.
The preparation method of above-mentioned Organic-inorganic composite Photoluminescence thin film, includes the following steps：
(1) by the doping Pr after annealing3+SrTiO3Particle is added in n,N-Dimethylformamide, ultrasonic disperse
35min forms mineral crystal particle precursor liquid；
(2) Kynoar is added in n,N-Dimethylformamide, mixes 110min, form organic polymer forerunner
Liquid；
(3) mineral crystal particle precursor liquid is added in organic polymer precursor liquid, is uniformly mixed, form luminescence generated by light
Masking liquid；
(4) luminescence generated by light masking liquid is coated uniformly on using curtain coating cladding process above the sheet glass of surfacing；
(5) it is coated with the mold of luminescence generated by light masking liquid or solidification is dried in container, 70 DEG C of dry 110min will consolidate
Organic-inorganic composite Photoluminescence thin film after change is removed from mold or container, and it is thin to obtain Organic-inorganic composite luminescence generated by light
Film；
Wherein, Pr is adulterated3+SrTiO3Particle and the mass ratio of n,N dimethylformamide are 1:8；
The mass ratio of Kynoar and N, N methylformamide are 1:7.
Embodiment 4
Difference lies in the doping Pr that will be made annealing treatment with embodiment 3 for the present embodiment3+SrTiO3Particle replace with not into
The doping Pr of row annealing3+SrTiO3Particle.
Embodiment 5
Difference lies in the doping Pr that will be made annealing treatment with embodiment 3 for the present embodiment3+SrTiO3Particle replaces with annealing
Doping Pr before processing and after annealing3+SrTiO3Granulate mixture, wherein mixing before annealing and after annealing
Miscellaneous Pr3+SrTiO3The mass ratio of particle is 1:1.
Embodiment 6
Difference lies in will adulterate Pr with embodiment 3 for the present embodiment3+SrTiO3Particle replaces with doping Pr3+CaTiO3
Particle.
Embodiment 7
Difference lies in will adulterate Pr with embodiment 3 for the present embodiment3+SrTiO3Particle replaces with doping Pr3+BaTiO3
Particle.
Embodiment 8
The present embodiment is that Pr will be adulterated with the difference of embodiment 33+SrTiO3Particle replaces with rare earth doped element Eu2+
SrTiO3Particle.
Comparative example 1
Difference lies in doping Pr for this comparative example embodiment 33+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is
1:1。
Comparative example 2
Difference lies in doping Pr for this comparative example embodiment 33+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is
1:15。
Comparative example 3
Difference lies in will adulterate Pr with embodiment 3 for this comparative example3+SrTiO3Particle replaces with niobic acid sodium potassium lithium.
Comparative example 4
Difference lies in polyvinylidene difluoride film is replaced with polyacrylonitrile film with embodiment 3 for this comparative example.
Experimental example 1
Light is carried out to the Organic-inorganic composite Photoluminescence thin film that embodiment 1-8 and comparative example 1-4 preparation methods are obtained
Spectrum detection and flexible detection, assay method use the conventional method of this field.Testing result is as shown in table 1.
Table 1
The exciting light and hair for the Organic-inorganic composite Photoluminescence thin film that embodiment 1-8 is prepared as can be seen from Table 1
Optical wavelength is penetrated, in 50287-112300, luminescent color has red, white green and orange red relative light intensity.As can be seen from Table 1
The exciting light and wavelength of transmitted light for the Organic-inorganic composite Photoluminescence thin film that comparative example 1-4 is prepared, relative light intensity exist
Between 6747-130950, light color is mainly red.
In the Organic-inorganic composite Photoluminescence thin film that embodiment 1-8 is prepared, the phase of embodiment 6-8 and embodiment 3
To luminous intensity difference, compared with Example 3, difference lies in the perovskite structure oxides of rare earth doped element by embodiment 6-8
The type of grain is different, this shows the calcium titanium of the relative light intensity and rare earth doped element of Organic-inorganic composite Photoluminescence thin film
The type of mine structure oxide particle is related.The variant rare earth element type with doping of the luminous color of embodiment 4,6,8 and
Luminescence mechanism is related, and embodiment 6 is related with the rare earth element of doping to material emission in 8, and material is luminous main in embodiment 4
It is related with the Lacking oxygen in material.
The relative light intensity of comparative example 1 is higher than embodiment 3, and 2 relative light intensity of comparative example is less than embodiment 3, comparative example 1,2
Difference lies in doping Pr with embodiment 33+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is different, adulterates Pr3+'s
SrTiO3The accounting of particle is higher, and relative light intensity is bigger.The relative light intensity of comparative example 3 be less than embodiment 3, comparative example 3 with
Difference lies in will adulterate Pr for embodiment 33+SrTiO3Particle replaces with niobic acid sodium potassium lithium, the hair of niobic acid sodium potassium lithium light-emitting particles
Optical property is good not as good as the oxide particles with perovskite structure of rare earth doped element.
Experimental example 2
The Organic-inorganic composite Photoluminescence thin film that embodiment 1-8 and comparative example 1-4 preparation methods are obtained is carried out soft
Property detection, pliability tester under prescribed conditions, when pliability instrument plate gauge head by sample be pressed into crack in certain depth (about
When 8mm), the sum of big vectors of Z of frictional force are known as pliability at the counter-bending power and sample of sample itself and gap, with milli- newton
(mN) it indicates, softness values are smaller, illustrate that sample is more soft.Testing result is as shown in table 2.
Table 2
The pliability for the Organic-inorganic composite Photoluminescence thin film that embodiment 1-8 preparation methods obtain as can be seen from Table 2
Between 322-425mN, the Organic-inorganic composite Photoluminescence thin film softness values that comparative example 1-4 preparation methods obtain exist value
Between 314-585mN.Softness values are smaller, illustrate that sample is more soft.Figure 14 is in embodiment 3 that Organic-inorganic composite is photic
Light-emitting film be curled into it is rodlike after photo, it is seen that the flexibility for the Organic-inorganic composite Photoluminescence thin film that the present invention is prepared into
Preferably.
Pr is adulterated in embodiment 13+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is 1:3, it mixes in embodiment 2
Miscellaneous Pr3+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is 1:12, Pr is adulterated in embodiment 33+SrTiO3Particle：
The volume ratio of polyvinylidene difluoride film is 1:6, Pr is adulterated in comparative example 13+SrTiO3Particle：The volume of polyvinylidene difluoride film
Than being 1:1, comparative example 2 adulterates Pr3+SrTiO3Particle：The volume ratio of polyvinylidene difluoride film is 1:15.Wherein comparative example 2 is made
The softness values of the machine-inorganic compounding Photoluminescence thin film obtained are 314, flexible maximum；Machine-inorganic compounding made from embodiment 1
The softness values of Photoluminescence thin film are 425, flexible minimum.This shows the perovskite structure oxide of rare earth doped element
Grain：The volume ratio of polyvinylidene difluoride film is different, and polyvinylidene difluoride film accounting is higher, and softness values are smaller, flexible bigger.
The difference of comparative example 4 and embodiment 3 is that polyvinylidene difluoride film is replaced with polyacrylonitrile film, and comparative example 4 is made
The Organic-inorganic composite Photoluminescence thin film softness values that Preparation Method obtains are 585, hence it is evident that are had less than what implementation 3 was prepared
Machine-inorganic compounding Photoluminescence thin film softness values 383.It is flexible big that this shows that the polyvinylidene difluoride film that the present invention uses has
The advantages of.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of Organic-inorganic composite Photoluminescence thin film, which is characterized in that including polyvinylidene difluoride film and rare earth doped member
The oxide particles with perovskite structure of element；The oxide particles with perovskite structure of the rare earth doped element is dispersed in described
In polyvinylidene difluoride film；
The oxide particles with perovskite structure of rare earth doped element：The volume ratio of polyvinylidene difluoride film is 1:3~12.
2. Organic-inorganic composite Photoluminescence thin film according to claim 1, which is characterized in that rare earth doped element
Oxide particles with perovskite structure：The volume ratio of polyvinylidene difluoride film is 1：4~10；
Preferably, the oxide particles with perovskite structure of rare earth doped element：The volume ratio of polyvinylidene difluoride film is 1:6~
10。
3. Organic-inorganic composite Photoluminescence thin film according to claim 1, which is characterized in that rare earth doped element
The chemical general formula of perovskite structure oxide is ABO3Or ReABO3, wherein Re is rare earth element, and A is alkaline earth element, and B is transition
Element；
Preferably, one kind in Re Nd, Sm, Eu, Gd, Dy, Ho or Pr；
Preferably, one kind in A Be, Mg, Ca, Sr, Ba or Ra；
Preferably, one kind in B Ti, V, Cr, Mn or Co；
Preferably, perovskite structure oxide CaTiO3、BaTiO3Or SrTiO3。
4. according to claim 1-3 any one of them Organic-inorganic composite Photoluminescence thin films, which is characterized in that doping is dilute
The perovskite structure oxide of earth elements is in the standard cube of the length of side≤30nm, or in the cube of curved edge, or is in ball
Shape.
5. according to claim 1-3 any one of them Organic-inorganic composite Photoluminescence thin films, which is characterized in that doping is dilute
The oxide particles with perovskite structure of earth elements is prepared using collosol-precipitation method；
Preferably, the preparation method of the oxide particles with perovskite structure of rare earth doped element, includes the following steps：
(a) alkaline earth metal hydroxide, coupling agent, alkali metal hydroxide, rare earth element soluble-salt and solvent are mixed equal
It is even；
(b) by mixed solution under the conditions of 155-165 DEG C oil bath heating 1.5-2.5h, obtain the calcium titanium of rare earth doped element
Mine oxide sol；
(c) by the water sedimentation of perovskite oxide colloidal sol and clean, by the material after cleaning under the conditions of 75-85 DEG C dry 20-
30h obtains oxide particles with perovskite structure；
Preferably, alkaline earth metal hydroxide includes one kind in strontium hydroxide, calcium hydroxide or barium hydroxide；
Preferably, coupling agent includes butyl titanate, three oleic acid acyloxy titanate esters of isopropyl or three hydroxy acyl isopropyl titanates
In one kind；
Preferably, alkali metal hydroxide includes one kind in lithium hydroxide, sodium hydroxide or potassium hydroxide；
Preferably, solvent includes one kind in polyvinylpyrrolidone, triethylene glycol or glycol ether.
6. according to claim 1-3 any one of them Organic-inorganic composite Photoluminescence thin films, which is characterized in that organic-nothing
The thickness of the compound Photoluminescence thin film of machine be 0.01~0.08mm, preferably 0.01~0.05mm, further preferably 0.01~
0.03mm。
7. a kind of preparation method according to any one of the claim 1-6 Organic-inorganic composite Photoluminescence thin films, feature
It is, includes the following steps：
The luminescence generated by light masking liquid obtained after mineral crystal particle precursor liquid and organic polymer precursor liquid are mixed cures, and obtains
To Organic-inorganic composite Photoluminescence thin film；
The mineral crystal particle precursor liquid is the oxide particles with perovskite structure and N of rare earth doped element, N- dimethyl methyls
What amide obtained after mixing；
The organic polymer precursor liquid is that Kynoar and n,N-Dimethylformamide obtain after mixing.
8. the preparation method of Organic-inorganic composite Photoluminescence thin film according to claim 7, which is characterized in that doping
The oxide particles with perovskite structure of rare earth element：The mass ratio of n,N-Dimethylformamide is 1:5~10；
Preferably, the oxide particles with perovskite structure of rare earth doped element：The mass ratio of n,N-Dimethylformamide is 1:6~
8；
Preferably, Kynoar：The mass ratio of N, N-METHYLFORMAMIDE are 1:6~12；
Preferably, Kynoar：The mass ratio of N, N-METHYLFORMAMIDE are 1:8~10.
9. the preparation method of Organic-inorganic composite Photoluminescence thin film according to claim 7 or 8, which is characterized in that packet
Include following steps：
(a) oxide particles with perovskite structure of rare earth doped element is added in n,N-Dimethylformamide, ultrasonic disperse
20-50min forms mineral crystal particle precursor liquid；
(b) Kynoar is added in n,N-Dimethylformamide, mixes 80-150min, form organic polymer forerunner
Liquid；
(c) mineral crystal particle precursor liquid is added in organic polymer precursor liquid, is uniformly mixed, formed luminescence generated by light and apply
Liquid；
(d) it is coated with the mold of luminescence generated by light masking liquid or container is dried solidification, 60-80 DEG C of dry 100-120min,
Organic-inorganic composite Photoluminescence thin film after solidification is removed from mold or container, obtains the photic hair of Organic-inorganic composite
Optical thin film；
Preferably, painting method includes the tape casting, spin coating method, spray coating method or brushing method.
10. a kind of claim 1-6 any one of them Organic-inorganic composite Photoluminescence thin films or claim 7-9 are any
Organic-inorganic composite Photoluminescence thin film exists made from the preparation method of Organic-inorganic composite Photoluminescence thin film described in
Purposes in password transmission, illumination or display field.
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| CN109705860A (en) * | 2018-12-10 | 2019-05-03 | 吉林大学 | CsPbBr3Nanocrystalline-PVDF sub-micro ball composite material and its application |
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