CN106186720A - Fluorescent photon crystal film and preparation method thereof - Google Patents
Fluorescent photon crystal film and preparation method thereof Download PDFInfo
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Abstract
The invention provides fluorescent photon crystal film, described fluorescent photon crystal comprises the composite nano-microsphere of monodispersed silicon dioxide nanosphere and carbon quantum dot, described carbon quantum dot is on the surface of described Nano microsphere, the mean diameter of described silicon dioxide nanosphere is between 170nm to 270nm, the mean diameter of described carbon quantum dot is between 2nm to 6nm, can launch indigo plant, green, red fluorescence under ultraviolet light irradiates.Present invention also offers the preparation method of fluorescent photon crystal film.Technical scheme provided by the present invention can obtain that synthesis is simple, manufacturing cycle is short, bright-colored, can the beneficial effect such as enhanced spectrum intensity.
Description
Technical field
The invention belongs to photonic crystal field, more particularly, to fluorescent photon crystal film and preparation method thereof.
Background technology
Within 1987, Yablonovitch and John proposes these new ideas of photonic crystal first, if different dielectric is normal
The dielectric material of number is according to certain regular periodicity arrangement, due to Bragg diffraction when electromagnetic wave is propagated wherein, electromagnetic wave
Meeting is modulated and forms band structure, and this band structure is called photonic band gap.Band gap it is likely to occur, i.e. between photonic band gap
Photon band gap.The periodic dielectric structures with photon band gap is exactly photonic crystal.Photonic crystal is optical due to its uniqueness
Can, such as photon band gap etc., can be widely used in photonic crystal fiber, manipulator, sensor, display, photon crystal wave-guide,
Low valve valve laser instrument etc..
Fluorescent photon crystal film, owing to having photon band gap and two kinds of performances of fluorescence simultaneously, thus in multiple fields, as
Laser instrument, sensor, display, microreactor etc., be used widely.At present, there is the system of three kinds of fluorescent photon crystal films
Preparation Method: fluorescent material is directly obtained by the first as dye molecule etc. is filled in photon crystal film；This method is simple
Easy, but, dye distribution is uneven, and dyestuff can affect the display of photon crystal film structure color；It two is to be directly synthesized
Itself having the dispersed nano microsphere of fluorescence property to carry out self assembly again and obtain, but the method has synthesis complexity, raw material comes
The shortcomings such as source is few, and fluorescence property is non-adjustable thus limit it and develop further；The third method be first synthesize monodispersed glimmering
Light composite nano-microsphere carries out self assembly again and obtains.This method is widely adopted, and major part report uses inorganic nano-crystal more
Quantum dot, such as CdSe/CdS nanocrystals quantum dots etc., as fluorescent emission unit, will be gathered by emulsion by this nanocrystals quantum dots
Close or process for modifying surface is coated to the inside of Nano microsphere or modifies on the surface of Nano microsphere.Obtain fluorescent nanometer microsphere
There is good fluorescence property, and the optical characteristics of photon crystal film itself can well be kept, but the method is also
There is certain drawback, as quantum dot synthesis relatively complicated, operating process is loaded down with trivial details, manufacturing cycle length, nanocrystals quantum dots
There is optical quenching and photobleaching, the inferior positions such as fluorescence property is unstable.
Summary of the invention
One of approach solving an above-mentioned difficult problem is to use novel quantum dot and technology of preparing.In recent years, fluorescent carbon quantum
Point, due to its excellent optical property, good biocompatibility, can be applicable to metal ion probe, probe biomolecule, life
Thing imaging, LED component, fluorescent ink, photocatalyst etc..Therefore, fluorescent carbon quantum dot is the optimal candidate solving the problems referred to above
Material.
For defect or the Improvement requirement of prior art, the invention provides fluorescent photon crystal film and preparation side thereof
Method, its object is to by silicon dioxide nanosphere and carbon quantum dot being combined, it is thus achieved that one has dual-use function, i.e. photon
Band gap and fluorescence property, fluorescent photon crystal film.Thus solve existing fluorescent photon crystal film synthesis complexity, preparation
The problems such as cycle length, poor optical properties.
For achieving the above object, the invention provides fluorescent photon crystal film, it is characterised in that described fluorescent photon is brilliant
Body comprises the composite nano-microsphere of monodispersed silicon dioxide nanosphere and carbon quantum dot, and described carbon quantum dot is in described nanometer
On the surface of microsphere, the mean diameter of described silicon dioxide nanosphere is between 170nm to 270nm, described carbon quantum dot
Mean diameter is between 2nm to 6nm, can launch indigo plant, green, red fluorescence under ultraviolet light irradiates.
The invention provides blue-fluorescence photon crystal film, it is characterised in that described fluorescent photon crystal comprises single point
The silicon dioxide nanosphere dissipated and the composite nano-microsphere of carbon quantum dot, described carbon quantum dot is on the surface of described Nano microsphere
On, the mean diameter of described silicon dioxide nanosphere is between 170nm to 220nm, and the mean diameter of described carbon quantum dot is
Between 2nm to 6nm, the fluorescence of blueness can be launched under ultraviolet light irradiates.
The invention provides green fluorescence photon crystal film, it is characterised in that described fluorescent photon crystal comprises single point
The silicon dioxide nanosphere dissipated and the composite nano-microsphere of carbon quantum dot, described carbon quantum dot is on the surface of described Nano microsphere
On, the mean diameter of described silicon dioxide nanosphere is between 230nm to 240nm, and the mean diameter of described carbon quantum dot is
Between 2nm to 6nm, can the fluorescence of transmitting green under ultraviolet light irradiates.
The invention provides red fluorescence photon crystal film, it is characterised in that described fluorescent photon crystal comprises single point
The silicon dioxide nanosphere dissipated and the composite nano-microsphere of carbon quantum dot, described carbon quantum dot is on the surface of described Nano microsphere
On, the mean diameter of described silicon dioxide nanosphere is between 250nm to 270nm, and the mean diameter of described carbon quantum dot is
Between 2nm to 6nm, the fluorescence of redness can be launched under ultraviolet light irradiates.
Present invention also offers the preparation method of fluorescent photon crystal film, said method comprising the steps of:
(1) prepare monodisperse silica Nano microsphere: first mixed with dehydrated alcohol by tetraethyl orthosilicate, then will go from
Sub-water, ammonia, dehydrated alcohol mix with solution before, and at room temperature magnetic agitation is reacted 20 hours；Use ethanol eccentric cleaning
I.e. obtain described monodisperse silica Nano microsphere for three times；
(2) composite nano-microsphere is prepared: monodisperse silica Nano microsphere and the preparation carbon amounts that will obtain in step (1)
Precursor liquid mix homogeneously in autoclave of son point, is placed at 180 DEG C reaction 4～5 hours；Room temperature it is cooled to after reaction,
Described composite nano-microsphere is i.e. obtained three times by ethanol eccentric cleaning；
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the composite nano-microsphere obtained in step (2),
The microscope slide soaked through chloroazotic acid is perpendicularly inserted in suspension, stands to volatilize completely to solvent in 30 DEG C and i.e. obtains fluorescence light
Sub-crystal film.
By the contemplated above technical scheme of the present invention compared with prior art, it is possible to obtain following beneficial effect:
(1) carbon quantum dot and monodisperse silica Nano microsphere are directly carried out by the present invention by a step hydrothermal synthesis method
Compound, it is not necessary to the complicated and time consumption Methods For Purifications such as dialysis or silica gel chromatography, substantially reduce and prepare photon crystal film
Manufacturing cycle.
(2) compare with traditional photon crystal film, fluorescent photon crystal film prepared by the present invention, fluorescent carbon quantum dot
Introducing do not interfere with the structure color of photon crystal film, gained fluorescent photon crystal film can show bright-coloured schemochrome
Color.
(3) comparing with traditional photon crystal film, fluorescent photon crystal film prepared by the present invention is received at silicon dioxide
Rice microsphere surface introduces carbon quantum dot, can launch the fluorescence of different colours when it is irradiated by ultraviolet light, when fluorescence spectrum and light
When subband gap matches, the effect of enhanced spectrum intensity can be played.
Sum it up, the contemplated above technical scheme of the present invention is compared with prior art, it is possible to obtain synthesis simple,
Manufacturing cycle is short, bright-colored, can the beneficial effect such as enhanced spectrum intensity.
Accompanying drawing explanation
Fig. 1 is the preparation process schematic diagram of fluorescent photon crystal film；
Fig. 2 is the transmission electron microscope photo of the composite nano-microsphere of silicon dioxide nanosphere and carbon quantum dot；A: low resolution
Transmission electron microscope photo under rate；Transmission electron microscope photo under B: high-resolution
Fig. 3 is the optical photograph of fluorescent photon crystal film, and structure color is blue；
Fig. 4 is the fluorescent optics photo of fluorescent photon crystal film；
Fig. 5 is the transmission electron microscope picture of silicon dioxide nanosphere and carbon quantum dot；The transmission electricity of 5A:2nm carbon quantum dot
Mirror picture；The transmission electron microscope picture of 5B:220nm silicon dioxide nanosphere；The transmission of 5C:250nm silicon dioxide nanosphere
Electron microscopic picture；
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.If additionally, technical characteristic involved in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
The fluorescent photon crystal film that the present invention provides, including monodisperse silica Nano microsphere and the carbon amounts on surface thereof
Sub-point: described monodisperse silica Nano microsphere particle diameter is between 170nm to 270nm.Described silicon dioxide nanosphere
Particle diameter determines the structure color of the photonic crystal that the present invention provides.Mean diameter between 170nm to 220nm, 230nm arrives
The photon crystal film that silicon dioxide nanosphere between 240nm, between 250nm to 270nm assembles shows blue, green respectively
And redness.
The invention provides fluorescent photon crystal film, it is characterised in that described fluorescent photon crystal comprises monodispersed
Silicon dioxide nanosphere and the composite nano-microsphere of carbon quantum dot, described carbon quantum dot is at described silicon dioxide nanosphere
On surface, the mean diameter of described silicon dioxide nanosphere is between 170nm to 270nm, the average particle of described carbon quantum dot
Footpath is between 2nm to 6nm, can launch indigo plant, green, red fluorescence under ultraviolet light irradiates.
The invention provides blue-fluorescence photon crystal film, it is characterised in that described fluorescent photon crystal comprises single point
Dissipating silicon dioxide nanosphere and the composite nano-microsphere of carbon quantum dot, the mean diameter of described silicon dioxide nanosphere is
Between 170nm to 220nm, the mean diameter of described carbon quantum dot is between 2nm to 6nm, can launch indigo plant under ultraviolet light irradiates
The fluorescence of color.
The invention provides green fluorescence photon crystal film, it is characterised in that described fluorescent photon crystal comprises single point
Dissipating silicon dioxide nanosphere and the composite nano-microsphere of carbon quantum dot, the mean diameter of described silicon dioxide nanosphere is
Between 230nm to 240nm, the mean diameter of described carbon quantum dot is between 2nm to 6nm, can launch green under ultraviolet light irradiates
The fluorescence of color.
The invention provides red fluorescence photon crystal film, it is characterised in that described fluorescent photon crystal comprises single point
Dissipating silicon dioxide nanosphere and the composite nano-microsphere of carbon quantum dot, the mean diameter of described silicon dioxide nanosphere is
Between 250nm to 270nm, the mean diameter of described carbon quantum dot is between 2nm to 6nm, can launch red under ultraviolet light irradiates
The fluorescence of color.
At present, the synthetic method of carbon quantum dot, such as hydrothermal synthesis method etc., the most fairly simple, but the purification of carbon quantum dot
Relatively complicated.It is generally required to the methods such as dialysis, silica gel column chromatography purify, its cycle length, operation complexity.The present invention uses one
Step hydrothermal synthesis method can prepare the composite nano-microsphere of silicon dioxide nanosphere and carbon quantum dot, by simple centrifugation
I.e. can get the composite nano-microsphere of purification, thus enormously simplify the tedious steps that carbon quantum dot purifies；After purification compound
Nano microsphere obtains fluorescent photon crystal film by self-assembling technique.
Described carbon quantum dot is launched the color precursor liquid prepared therefrom of fluorescence and is determined, launches the carbon quantum dot of different wave length
Precursor liquid used is different.The carbon quantum dot launching blue-fluorescence can be prepared when precursor liquid is citric acid and ethylenediamine；Forerunner
The carbon quantum dot of transmitting green fluorescence can be prepared when liquid is glucose；Transmitting red fluorescence can be prepared when precursor liquid is p-phenylenediamine
Carbon quantum dot.Solvent prepared by described carbon quantum dot is all deionized water；The mean diameter of described carbon quantum dot is 2～6nm
Between.
The invention provides the preparation method of fluorescent photon crystal film, said method comprising the steps of:
(1) prepare monodisperse silica Nano microsphere: first mixed with dehydrated alcohol by tetraethyl orthosilicate, then will go from
Sub-water, ammonia, dehydrated alcohol mix with solution before, and at room temperature magnetic agitation is reacted 20 hours；Use ethanol eccentric cleaning
I.e. obtain described monodisperse silica Nano microsphere for three times；
(2) composite nano-microsphere is prepared: monodisperse silica Nano microsphere and the preparation carbon amounts that will obtain in step (1)
Precursor liquid mix homogeneously in autoclave of son point, reacts 4～5 hours at 180 DEG C.It is cooled to room temperature after reaction, uses
Ethanol eccentric cleaning i.e. obtains described composite nano-microsphere three times；
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the composite nano-microsphere obtained in step (2),
The microscope slide soaked through chloroazotic acid is perpendicularly inserted in suspension, stands to volatilize completely to solvent in 30 DEG C and i.e. obtains fluorescence light
Sub-crystal film；
Wherein, in step (1), the ratio of the quality of tetraethyl orthosilicate and ethanol is 2～3:50；
Wherein, in step (1), the ratio of the quality of deionized water, ammonia, dehydrated alcohol is 2～3:4～8:40；
Wherein, ammonia used in step (1), deionized water, the ratio of tetraethyl orthosilicate be 1.68～3.7:0.53～
1.44:1, the consumption of ammonia, deionized water and tetraethyl orthosilicate three can control the mean diameter of silicon dioxide nanosphere；
Wherein, the precursor liquid in step (2) is citric acid, ethylenediamine；The grain of the silicon dioxide nanosphere in step (2)
Footpath is between 170nm to 220nm；
Wherein, the precursor liquid in step (2) is glucose；In step (2), the particle diameter of silicon dioxide nanosphere is at 230nm
Between 240nm；
Wherein, the precursor liquid in step (2) is p-phenylenediamine；In step (2), the particle diameter of silicon dioxide nanosphere exists
Between 250nm to 270nm；
Wherein, in step (3), the mass ratio of composite nano-microsphere and dehydrated alcohol is 1～5:100.
The invention provides the preparation method of blue-fluorescence photon crystal film, comprise the following steps:
(1) prepare monodisperse silica Nano microsphere: first mixed with dehydrated alcohol by tetraethyl orthosilicate, then will go from
Sub-water, ammonia, dehydrated alcohol mix with solution before, and at room temperature magnetic agitation is reacted 20 hours, then uses ethanol eccentric cleaning
Three times and get final product；
(2) the monodisperse silica Nano microsphere that step (1) obtains is joined preparation and launch the carbon amounts of blue-fluorescence
The precursor liquid of son point prepares silicon dioxide nanosphere/carbon quantum dot composite nano-microsphere: add a certain amount of in a kettle.
Citric acid, ethylenediamine, deionized water, silicon dioxide nanosphere, be placed at 180 DEG C reaction 5 hours, be cooled to room temperature, mistake
Filter sub-cloud large-size particle thing, after by ethanol eccentric cleaning three times and get final product；
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the composite nano-microsphere obtained in step (2),
The microscope slide soaked through chloroazotic acid is perpendicularly inserted in suspension, stands to solvent at 30 DEG C and is evaporated completely and get final product；
Wherein, in step (1), the ratio of the quality of tetraethyl orthosilicate and ethanol is 2～3:50；
Wherein, in step (1), the ratio of the quality of deionized water, ammonia, dehydrated alcohol is 2～3:4～8:40；
Wherein, ammonia used in step (1), deionized water, the ratio of tetraethyl orthosilicate be 1.68～3.7:0.53～
1.44:1,
Wherein, the particle diameter of the silicon dioxide nanosphere in step (2) is between 170nm to 220nm；
Wherein, the mass ratio of citric acid, ethylenediamine and the deionized water in step (2) is 1:1:20；Wherein, described two
Silicon oxide/carbon quantum dot composite nanoparticle suspension, its mass fraction is 1% to 5%.
Wherein, in step (3), the mass ratio of composite nano-microsphere and dehydrated alcohol is 1～5:100.
The invention provides the preparation method of green fluorescence photon crystal film, comprise the following steps:
(1) prepare monodisperse silica Nano microsphere: first mixed with dehydrated alcohol by tetraethyl orthosilicate, then will go from
Sub-water, ammonia, dehydrated alcohol mix with solution before, and at room temperature magnetic agitation is reacted 20 hours, then uses ethanol eccentric cleaning
Three times and get final product；
(2) the monodisperse silica Nano microsphere that step (1) obtains is joined prepare the carbon amounts of transmitting green fluorescence
The precursor liquid of son point prepares silicon dioxide nanosphere/carbon quantum dot composite nano-microsphere: add a certain amount of in a kettle.
Glucose, deionized water, silicon dioxide nanosphere, be placed at 180 DEG C reaction 4 hours, be cooled to room temperature, be filtered to remove down
Layer large-size particle thing, after by ethanol eccentric cleaning three times and get final product；
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the composite nano-microsphere obtained in step (2),
The microscope slide soaked through chloroazotic acid is perpendicularly inserted in suspension, stands to solvent at 30 DEG C and is evaporated completely and get final product；
Wherein, in step (1), the ratio of the quality of tetraethyl orthosilicate and ethanol is 2～3:50；
Wherein, in step (1), the ratio of the quality of deionized water, ammonia, dehydrated alcohol is 2～3:4～8:40；
Wherein, ammonia used in step (1), deionized water, the ratio of tetraethyl orthosilicate be 1.68～3.7:0.53～
1.44:1,
Wherein, the particle diameter of the silicon dioxide nanosphere in step (2) is between 230nm to 240nm；
Wherein, in step (2), the mass ratio of glucose and deionized water is 1:30；
Wherein, in step (3), the mass ratio of composite nano-microsphere and dehydrated alcohol is 1～5:100；
The invention provides the preparation method of red fluorescence photon crystal film, comprise the following steps:
(1) prepare monodisperse silica Nano microsphere: first mixed with dehydrated alcohol by tetraethyl orthosilicate, then will go from
Sub-water, ammonia, dehydrated alcohol mix with solution before, and at room temperature magnetic agitation is reacted 20 hours, then uses ethanol eccentric cleaning
Three times and get final product；
(2) the monodisperse silica Nano microsphere that step (1) obtains is joined preparation and launch the carbon amounts of red fluorescence
The precursor liquid of son point prepares silicon dioxide nanosphere/carbon quantum dot composite nano-microsphere: add a certain amount of in a kettle.
P-phenylenediamine, dehydrated alcohol, silicon dioxide nanosphere, be placed at 180 DEG C reaction 5 hours, be cooled to room temperature, be filtered to remove
Lower floor's large-size particle thing, after by ethanol eccentric cleaning three times and get final product；
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the composite nano-microsphere obtained in step (2),
The microscope slide soaked through chloroazotic acid is perpendicularly inserted in suspension, stands to solvent at 30 DEG C and is evaporated completely and get final product；
Wherein, the particle diameter of the silicon dioxide nanosphere in step (2) is between 250nm to 270nm；
Wherein, in step (2), the mass ratio of p-phenylenediamine and dehydrated alcohol is 1:100；
Wherein, in step (1), the ratio of the quality of tetraethyl orthosilicate and ethanol is 2～3:50；
Wherein, in step (1), the ratio of the quality of deionized water, ammonia, dehydrated alcohol is 2～3:4～8:40；
Wherein, ammonia used in step (1), deionized water, the ratio of tetraethyl orthosilicate be 1.68～3.7:0.53～
1.44:1；
Wherein, in step (3), the mass ratio of composite nano-microsphere and dehydrated alcohol is 1～5:100；
Embodiment:
The preparation of embodiment 1 blue-fluorescence photon crystal film
A kind of blue-fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot, is shown in Fig. 2；
The particle diameter of described silicon dioxide nanosphere is 170nm, and the particle diameter of carbon quantum dot is 2nm.Prepare monodisperse silica nanometer
In microsphere, ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 1.85:1.39:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.08mL tetraethyl orthosilicate
Close uniformly, then by 2.91mL deionized water, 3.85mL ammonia, 40mL dehydrated alcohol at mix homogeneously, in room temperature and magnetic agitation
Lower mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 0.42g citric acid, 535 μ L ethylenediamines, is placed in 180 DEG C of baking ovens reaction 5 hours, its
Solvent is deionized water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and is evaporated completely and get final product, see Fig. 3 and 4 in 30 DEG C of baking ovens.
The preparation of embodiment 2 green fluorescence photon crystal film
A kind of green fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 230nm, and the particle diameter of carbon quantum dot is 2nm, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 1.85:1.44:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.08mL tetraethyl orthosilicate
Close uniformly, then by 3.0mL deionized water, 3.85mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 1.2g glucose, is placed in 180 DEG C of baking ovens reaction 5 hours, and its solvent is deionization
Water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 3 red fluorescence photon crystal film
A kind of red fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
Silicon oxide particle diameter is 250nm, and the particle diameter of carbon quantum dot is 2nm, sees Fig. 5 A and C, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 3.7:1.07:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.08mL tetraethyl orthosilicate
Close uniformly, then by 2.23mL deionized water, 7.7mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 0.9g p-phenylenediamine, be placed in 180 DEG C of baking ovens reaction 5 hours, its solvent for go from
Sub-water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 4 blue-fluorescence photon crystal film
A kind of blue-fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 190nm, and the particle diameter of carbon quantum dot is 2nm, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 1.68:1.31:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.29mL tetraethyl orthosilicate
Close uniformly, then by 3.0mL deionized water, 3.85mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 0.42g citric acid, 535 μ L ethylenediamines, is placed in 180 DEG C of baking ovens reaction 5 hours, its
Solvent is deionized water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 5 green fluorescence photon crystal film
A kind of green fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 240nm, and the particle diameter of carbon quantum dot is 2nm, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 3.36:0.97:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.29mL tetraethyl orthosilicate
Close uniformly, then by 2.23mL deionized water, 7.7mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 1.2g glucose, is placed in 180 DEG C of baking ovens reaction 5 hours, and its solvent is deionization
Water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 6 red fluorescence photon crystal film
A kind of red fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 270nm, and the particle diameter of carbon quantum dot is 2nm, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 1.85:0.53:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 4.16mL tetraethyl orthosilicate
Close uniformly, then by 2.23mL deionized water, 7.7mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 0.9g p-phenylenediamine, be placed in 180 DEG C of baking ovens reaction 5 hours, its solvent for go from
Sub-water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 7 blue-fluorescence photon crystal film
A kind of blue-fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 220nm, sees Fig. 5 B, and the particle diameter of carbon quantum dot is 6nm, prepares monodisperse silica nanometer
In microsphere, ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 1.68:1.31:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.29mL tetraethyl orthosilicate
Close uniformly, then by 3.0mL deionized water, 3.85mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 0.42g citric acid, 1270 μ L ethylenediamines, is placed in 180 DEG C of baking ovens reaction 5 hours,
Its solvent is deionized water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 8 green fluorescence photon crystal film
A kind of green fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 240nm, and the particle diameter of carbon quantum dot is 6nm, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 3.36:0.97:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 2.29mL tetraethyl orthosilicate
Close uniformly, then by 2.23mL deionized water, 7.7mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 1.5g glucose, is placed in 180 DEG C of baking ovens reaction 5 hours, and its solvent is deionization
Water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
The preparation of embodiment 9 red fluorescence photon crystal film
A kind of red fluorescence photon crystal film, including monodisperse silica Nano microsphere and carbon quantum dot；Described two
The particle diameter of silicon oxide Nano microsphere is 270nm, and the particle diameter of carbon quantum dot is 6nm, prepares in monodisperse silica Nano microsphere
Ammonia used, deionized water, the ratio of tetraethyl orthosilicate are 1.85:0.53:1.
(1) monodisperse silica Nano microsphere is prepared: first mixed with 50mL dehydrated alcohol by 4.16mL tetraethyl orthosilicate
Close uniformly, then by 2.23mL deionized water, 7.7mL ammonia, 40mL dehydrated alcohol at mix homogeneously, under room temperature and magnetic agitation
Mixing above two solution, continuous stirring is reacted 20 hours.Use ethanol eccentric cleaning three times after reaction and get final product.
(2) monodisperse silica/carbon quantum dot composite nano-microsphere is prepared: the silica nanometer that will obtain in (1)
Microsphere is mixed homogeneously in reactor with 1.2g p-phenylenediamine, be placed in 180 DEG C of baking ovens reaction 5 hours, its solvent for go from
Sub-water.It is cooled to room temperature after having reacted, uses ethanol eccentric cleaning three times and get final product.
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the complex microsphere obtained in (2), through chloroazotic acid
The microscope slide soaked is perpendicularly inserted in suspension, stands to solvent and be evaporated completely and get final product in 30 DEG C of baking ovens.
As it will be easily appreciated by one skilled in the art that and the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, all should comprise
Within protection scope of the present invention.
Claims (11)
1. fluorescent photon crystal film, it is characterised in that it is micro-that described fluorescent photon crystal comprises monodispersed silica nanometer
Ball and the composite nano-microsphere of carbon quantum dot, described carbon quantum dot is on the surface of described Nano microsphere, and described silicon dioxide is received
The mean diameter of meter Wei Qiu is between 170nm to 270nm, and the mean diameter of described carbon quantum dot is between 2nm to 6nm, at purple
Outer light can launch blueness, green, red fluorescence under irradiating.
2. fluorescent photon crystal film as claimed in claim 1, it is characterised in that described silicon dioxide nanosphere average
Particle diameter, between 170nm to 220nm, between 230nm to 240nm, between 250nm to 270nm, shows blue, green and red respectively
Color.
3. fluorescent photon crystal film as claimed in claim 1, it is characterised in that described carbon quantum dot is closed by a step hydro-thermal
Prepared by one-tenth method.
4. the preparation method of the fluorescent photon crystal film as described in claims 1 to 3 any one, it is characterised in that include
Following steps:
(1) monodisperse silica Nano microsphere is prepared: first mixed with dehydrated alcohol by tetraethyl orthosilicate, then by deionization
Water, ammonia, dehydrated alcohol mix with solution before, and at room temperature magnetic agitation is reacted 20 hours, then by ethanol eccentric cleaning three
Secondary, i.e. obtain monodisperse silica Nano microsphere；
(2) composite nano-microsphere is prepared: monodisperse silica Nano microsphere and the preparation carbon quantum dot that will obtain in step (1)
Precursor liquid mix homogeneously in autoclave, be placed at 180 DEG C reaction 4～5 hours；It is cooled to room temperature after reaction, uses second
Alcohol eccentric cleaning i.e. obtains described composite nano-microsphere three times；
(3) fluorescent photon crystal film is prepared: be distributed in ethanol by the composite nano-microsphere obtained in step (2), passing through
The microscope slide that chloroazotic acid soaked is perpendicularly inserted in suspension, stands in 30 DEG C and volatilizees to solvent that i.e. to obtain fluorescent photon brilliant completely
Body thin film.
5. preparation method as claimed in claim 4, it is characterised in that tetraethyl orthosilicate and the quality of ethanol in step (1)
Ratio is 2～3:50.
6. preparation method as claimed in claim 4, it is characterised in that deionized water in step (1), ammonia, dehydrated alcohol
Mass ratio is 2～3:4～8:40.
7. preparation method as claimed in claim 4, it is characterised in that ammonia, deionized water, positive silicic acid used in step (1)
The mass ratio of tetra-ethyl ester is 1.68～3.7:0.53～1.44:1.
8. preparation method as claimed in claim 4, it is characterised in that the precursor liquid in step (2) is citric acid, ethylenediamine；
The particle diameter of the silicon dioxide nanosphere in step (2) is between 170nm to 220nm.
9. preparation method as claimed in claim 4, it is characterised in that the precursor liquid in step (2) is glucose；Step (2)
The particle diameter of middle silicon dioxide nanosphere is between 230nm to 240nm.
10. preparation method as claimed in claim 4, it is characterised in that the precursor liquid in step (2) is p-phenylenediamine；Step
(2) in, the particle diameter of silicon dioxide nanosphere is between 250nm to 270nm.
11. preparation methoies as claimed in claim 4, it is characterised in that composite nano-microsphere and dehydrated alcohol in step (3)
Mass ratio is 1～5:100.
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