CN105113007A - Method of utilizing one-step method to quickly prepare high-quality inverse opal structure photonic crystals - Google Patents
Method of utilizing one-step method to quickly prepare high-quality inverse opal structure photonic crystals Download PDFInfo
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Abstract
The invention relates to preparation methods of inverse opal structure photonic crystals, in particular to a method of utilizing one-step method to quickly prepare high-quality inverse opal structure photonic crystals, and aims to solve the problem that existing preparation methods of the inverse opal structure photonic crystals are low in mechanical performance and difficult in realizing large-area orderly arrangement or long in vertical deposition time and the problem that vertical deposition self-assembling methods are quite difficult in realizing crack-free large-area self-assembling. The method includes: 1, mixing Si (OC2H5)4, HCl and anhydrous alcohol A to obtain silica precursor, adding polymer microspheres into the silica precursor for ultrasonic dispersion, dropwise adding anhydrous alcohol B to obtain a colloid crystal mixed solution after ultrasonic dispersion, performing centrifugal self-assembling on the colloid crystal mixed solution after ultrasonic dispersion, and drying; 2, dipping a colloid crystal mixture after being dried in HF, and flushing. The method is used for utilizing the one-step method to quickly prepare the high-quality inverse opal structure photonic crystals.
Description
Technical field
The present invention relates to the preparation method of photonic crystal with inverse opal structure.
Background technology
To be size in 100 nanometers to issue to the inorganic or organic colloid micro ball of several microns in the effect of motivating force colloidal crystal is conigenous assembly behavior, thus forming two dimension or three-dimensional ordered structure, the colloid micro ball structure of this ordered arrangement is commonly called colloidal crystal, photonic crystal or synthetic proteins stone structure.Colloidal crystal becomes the base mateiral of New Generation Optical electrical part due to its excellent optical property; The ideal model system of some fundamemtal phenomenas can also be used as, may be used for dissolution process, the study mechanism of the hot issues such as phase in version process; In addition, colloidal crystal itself also can be used as template, and evaporation, photoetching technique etc. perfectly merge, for the preparation of patterning photonic crystal.
Just because of colloidal crystal and derivative thereof have broad application prospects, just make it in preparation accuracy controlling, chemical modification and novel application subject crossing, receive very big concern.Photonic crystal with inverse opal structure adopts sacrifice template synthesis usually, and as adopted evaporation-induced self-assembly in substrate of glass, plastic-substrates etc., vertical deposition self-assembly, the mode such as to spray, be coated with prepares opal photonic crystal.And then adopt the methods such as dipping, coating to fill the presoma of the classes such as silicon-dioxide, adopt the method removing opal colloidal structures such as calcining, etching afterwards again, obtain counter opal structure colloidal crystal.The usual mechanical property of the counter opal structure that these methods obtain is poor, and is difficult to realize large-area ordered arrangement.
Such as, Yan east is big etc. in the patent documentation [CN103352255A] utilizes polymer microballoon to mix with sol precursor, obtain polymeric film after growing a couple of days on the glass substrate by vertical deposition afterwards, finally by calcining removing micro polymer ball template, obtain inverse opal photonic crystal.Weak point is that this method vertical deposition time is long, and vertical deposition self-assembling method is difficult to realize the self-assembly of flawless big area.
Summary of the invention
The present invention will solve the preparation method of existing photonic crystal with inverse opal structure or to there is mechanical property poor, be difficult to realize large-area ordered arrangement, or it is long to there is the vertical deposition time, and vertical deposition self-assembling method is difficult to the problem realizing the self-assembly of flawless big area, and provide the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast.
Utilize single stage method to prepare the method for high quality photonic crystal with inverse opal structure fast, specifically carry out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 1% ~ 50% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 100rpm ~ 1000rpm, stir 1h ~ 10h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 1% ~ 10%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 1% ~ 10% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 1000r/min ~ 10000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 10min ~ 100min, obtain colloidal crystal mixture, be finally dry under the condition of 50 DEG C ~ 100 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 1% ~ 50% with mass percent is 1:(1 ~ 10); Described Si (OC
2h
5)
4be 1:(1 ~ 10 with the volume ratio of dehydrated alcohol A); Described mass percent is the polymer microballoon emulsion of 1% ~ 10% and the volume ratio of dehydrated alcohol B is 1:(1 ~ 10);
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 1% ~ 50%, dipping 30min ~ 300min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure.
The invention has the beneficial effects as follows: the present invention adopts the method for letex polymerization to prepare the good polymer microballoon of monodispersity, and mixes appropriate silica precursor in the solution, and adopt centrifugal self-assembly process, single stage method prepares photonic crystal with inverse opal structure.This method technique is simple, because the factor such as rotating speed of the amount of each monomer, emulsion concentration, whizzer can accuracy controlling in experimentation, experimental repeatability is good, can realize the quick preparation of high quality anti-protein structure photonic crystal.This invention makes the quality of photonic crystal be improved significantly, and preparing inverse opal photonic crystal has fast widened its Application Areas simultaneously.
1 whole technological process is simple, without the need to specific installation and technique.
The microballoon polymolecularity PDI that counter opal obtained by 2 forms photonic crystal because of it in centrifugal process improves, and can obtain high-quality photon crystal structure, and because doping makes its density higher, physical strength is higher, and quality is high.
3, prepare large-area photonic crystal with inverse opal structure, under scale is 3 μm, still can reaches ordered arrangement, flawless.
The method of the present invention for utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment one;
Fig. 2 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment two;
Fig. 3 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment three;
Fig. 4 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment four.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the single stage method that utilizes described in present embodiment prepares the method for high quality photonic crystal with inverse opal structure fast, specifically carries out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 1% ~ 50% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 100rpm ~ 1000rpm, stir 1h ~ 10h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 1% ~ 10%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 1% ~ 10% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 1000r/min ~ 10000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 10min ~ 100min, obtain colloidal crystal mixture, be finally dry under the condition of 50 DEG C ~ 100 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 1% ~ 50% with mass percent is 1:(1 ~ 10); Described Si (OC
2h
5)
4be 1:(1 ~ 10 with the volume ratio of dehydrated alcohol A); Described mass percent is the polymer microballoon emulsion of 1% ~ 10% and the volume ratio of dehydrated alcohol B is 1:(1 ~ 10);
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 1% ~ 50%, dipping 30min ~ 300min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure.
The beneficial effect of present embodiment is: present embodiment adopts the method for letex polymerization to prepare the good polymer microballoon of monodispersity, and mix appropriate silica precursor in the solution, adopt centrifugal self-assembly process, single stage method prepares photonic crystal with inverse opal structure.This method technique is simple, because the factor such as rotating speed of the amount of each monomer, emulsion concentration, whizzer can accuracy controlling in experimentation, experimental repeatability is good, can realize the quick preparation of high quality anti-protein structure photonic crystal.This invention makes the quality of photonic crystal be improved significantly, and preparing inverse opal photonic crystal has fast widened its Application Areas simultaneously.
1 whole technological process is simple, without the need to specific installation and technique.
The microballoon polymolecularity PDI that counter opal obtained by 2 forms photonic crystal because of it in centrifugal process improves, and can obtain high-quality photon crystal structure, and because doping makes its density higher, physical strength is higher, and quality is high.
3, prepare large-area photonic crystal with inverse opal structure, under scale is 3 μm, still can reaches ordered arrangement, flawless.
In preparation process, silica precursor is mixed mutually with polymer microballoon, because polymer microballoon is soft shell, and silica precursor is small-particle, the gap between polymer microballoon can be filled up in the process of centrifugal self-assembly, the physical strength of the sample of raising.
Embodiment two: present embodiment and embodiment one unlike: the polymer microballoon described in step one is Styrene And Chloroalkyl Acrylates microballoon.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two are unlike Si (OC described in step one
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:1.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are unlike Si (OC described in step one
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:2.Other is identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four are unlike Si (OC described in step one
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:3.Other is identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are unlike Si (OC described in step one
2h
5)
4be 1:2 with the volume ratio of dehydrated alcohol A.Other is identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are unlike Si (OC described in step one
2h
5)
4be 1:3 with the volume ratio of dehydrated alcohol A.Other is identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the mass percent described in step one is the polymer microballoon emulsion of 1% and the volume ratio of dehydrated alcohol B is 1:1.Other is identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the mass percent described in step one is the polymer microballoon emulsion of 2% and the volume ratio of dehydrated alcohol B is 1:2.Other is identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: the mass percent described in step one is the polymer microballoon emulsion of 3% and the volume ratio of dehydrated alcohol B is 1:3.Other is identical with embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten unlike: the mass percent described in step one is the polymer microballoon emulsion of 5% and the volume ratio of dehydrated alcohol B is 1:4.Other is identical with embodiment one to ten.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The single stage method that utilizes described in the present embodiment prepares the method for high quality photonic crystal with inverse opal structure fast, specifically carries out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 10% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 300rpm, stir 1h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 1%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 1% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 1000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 100min, obtain colloidal crystal mixture, be finally dry under the condition of 60 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:2; Described Si (OC
2h
5)
4be 1:3 with the volume ratio of dehydrated alcohol A; Described mass percent is the polymer microballoon emulsion of 1% and the volume ratio of dehydrated alcohol B is 1:1;
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 5%, dipping 30min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure;
Polymer microballoon described in step one is Styrene And Chloroalkyl Acrylates microballoon.
Embodiment two:
The single stage method that utilizes described in the present embodiment prepares the method for high quality photonic crystal with inverse opal structure fast, specifically carries out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 10% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 300rpm, stir 1h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 2%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 2% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 3000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 30min, obtain colloidal crystal mixture, be finally dry under the condition of 50 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:1; Described Si (OC
2h
5)
4be 1:3 with the volume ratio of dehydrated alcohol A; Described mass percent is the polymer microballoon emulsion of 2% and the volume ratio of dehydrated alcohol B is 1:2;
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 10%, dipping 40min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure;
Polymer microballoon described in step one is Styrene And Chloroalkyl Acrylates microballoon.
Embodiment three:
The single stage method that utilizes described in the present embodiment prepares the method for high quality photonic crystal with inverse opal structure fast, specifically carries out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 10% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 300rpm, stir 1h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 3%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 3% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 4000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 40min, obtain colloidal crystal mixture, be finally dry under the condition of 45 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:2; Described Si (OC
2h
5)
4be 1:2 with the volume ratio of dehydrated alcohol A; Described mass percent is the polymer microballoon emulsion of 3% and the volume ratio of dehydrated alcohol B is 1:3;
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 15%, dipping 30min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure;
Polymer microballoon described in step one is Styrene And Chloroalkyl Acrylates microballoon.
Embodiment four:
The single stage method that utilizes described in the present embodiment prepares the method for high quality photonic crystal with inverse opal structure fast, specifically carries out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 10% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 300rpm, stir 1h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 5%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 5% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 5000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 30min, obtain colloidal crystal mixture, be finally dry under the condition of 40 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:3; Described Si (OC
2h
5)
4be 1:3 with the volume ratio of dehydrated alcohol A; Described mass percent is the polymer microballoon emulsion of 5% and the volume ratio of dehydrated alcohol B is 1:4;
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 20%, dipping 20min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure;
Polymer microballoon described in step one is Styrene And Chloroalkyl Acrylates microballoon.
Fig. 1 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment one; Fig. 2 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment two; Fig. 3 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment three; Fig. 4 is the scanning electron microscope (SEM) photograph of high quality photonic crystal with inverse opal structure prepared by embodiment four.As seen from the figure, embodiment one to four all can prepare large-area photonic crystal with inverse opal structure, under scale is 3 μm, still can reach ordered arrangement, flawless, therefore, high quality photonic crystal with inverse opal structure physical strength prepared by the present invention is higher, and quality is high.
Claims (10)
1. utilize single stage method to prepare the method for high quality photonic crystal with inverse opal structure fast, it is characterized in that the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure is fast carried out according to following steps:
One, by Si (OC
2h
5)
4, mass percent be 1% ~ 50% HCl and dehydrated alcohol A mix after, under room temperature and stirring velocity are 100rpm ~ 1000rpm, stir 1h ~ 10h, obtain silica precursor, polymer microballoon is joined ultrasonic disperse in silica precursor, obtain the polymer microballoon emulsion that mass percent is 1% ~ 10%, be drip dehydrated alcohol B in the polymer microballoon emulsion of 1% ~ 10% to mass percent, ultrasonic after mixing, obtain the colloidal crystal mixing solutions after ultrasonic disperse, be under the condition of 1000r/min ~ 10000r/min at rotating speed, colloidal crystal mixing solutions after ultrasonic disperse is carried out centrifugal self-assembly, centrifugal 10min ~ 100min, obtain colloidal crystal mixture, be finally dry under the condition of 50 DEG C ~ 100 DEG C in temperature by colloidal crystal mixture, obtain the colloidal crystal mixture after drying,
Described Si (OC
2h
5)
4the volume ratio being the HCl of 1% ~ 50% with mass percent is 1:(1 ~ 10); Described Si (OC
2h
5)
4be 1:(1 ~ 10 with the volume ratio of dehydrated alcohol A); Described mass percent is the polymer microballoon emulsion of 1% ~ 10% and the volume ratio of dehydrated alcohol B is 1:(1 ~ 10);
Two, by dry after colloidal crystal impregnation mixture in mass percent be the HF of 1% ~ 50%, dipping 30min ~ 300min, then use deionized water rinsing, obtain high quality photonic crystal with inverse opal structure.
2. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the polymer microballoon described in step one is Styrene And Chloroalkyl Acrylates microballoon.
3. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the Si (OC described in step one
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:1.
4. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the Si (OC described in step one
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:2.
5. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the Si (OC described in step one
2h
5)
4the volume ratio being the HCl of 10% with mass percent is 1:3.
6. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the Si (OC described in step one
2h
5)
4be 1:2 with the volume ratio of dehydrated alcohol A.
7. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the Si (OC described in step one
2h
5)
4be 1:3 with the volume ratio of dehydrated alcohol A.
8. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the mass percent described in step one be the polymer microballoon emulsion of 1% and the volume ratio of dehydrated alcohol B is 1:1.
9. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the mass percent described in step one be the polymer microballoon emulsion of 2% and the volume ratio of dehydrated alcohol B is 1:2.
10. the method utilizing single stage method to prepare high quality photonic crystal with inverse opal structure fast according to claim 1, is characterized in that the mass percent described in step one be the polymer microballoon emulsion of 3% and the volume ratio of dehydrated alcohol B is 1:3.
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