CN102345167A - Preparation method of non-close packed inverse opal photonic crystal - Google Patents
Preparation method of non-close packed inverse opal photonic crystal Download PDFInfo
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- CN102345167A CN102345167A CN2011102431573A CN201110243157A CN102345167A CN 102345167 A CN102345167 A CN 102345167A CN 2011102431573 A CN2011102431573 A CN 2011102431573A CN 201110243157 A CN201110243157 A CN 201110243157A CN 102345167 A CN102345167 A CN 102345167A
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Abstract
A preparation method of non-close packed inverse opal photonic crystals comprises the following steps: preparing SiO2 spherical particles with ethyl orthosilicate as a raw material, performing ultrasonic treatment and vertical deposition of small-size SiO2 spherical particles and large-size organic particles to obtain a dual-size colloidal crystal structure, calcining the obtained heterogeneous dual-size colloidal crystal structure at a combustion decomposition temperature of the organic particles to remove organic matter so as to obtain non-close packed inverse opal photonic crystals; the method of the invention has simple equipment, simple operations, a short preparation period, and high yield.
Description
Technical field
The present invention relates to a kind of preparation method of photonic crystal, particularly a kind of preparation method of non-close heap inverse opal photonic crystal.
Background technology
Photonic crystal is the material that a kind of specific inductivity periodical change is arranged, and the most basic characteristic is to have photon band gap.Photonic crystal can be divided into opal structural photonic crystal and photonic crystal with inverse opal structure.At present; Self-assembly method is one of main method of preparation opal structural photonic crystal; But because used colloidal spheres requires the spherical particles for narrow diameter distribution, good dispersity in the self-assembly method; Main silicon-dioxide and the polystyrene of adopting; And the specific refractory power of silicon-dioxide or polystyrene is less, has only the direction band gap.Remove colloidal crystal template then and in the space of colloidal crystal, fill high-index material, form photonic crystal with inverse opal structure, and, when the specific refractory power of packing material is enough high (n＞2.85), complete band gap will appear.But in the research and preparation process of counter opal colloidal crystal, the gap of opal colloidal crystal template is often less, is unfavorable for the new counter opal structure and the Application and Development of performance at present.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art; The object of the present invention is to provide a kind of preparation method of non-close heap inverse opal photonic crystal; The non-close heap inverse opal photonic crystal of preparation is arranged complete, adjustable gaps, and production technique is simple, the cycle is short, required equipment is simple.
To achieve these goals, the technical scheme of the present invention's employing is:
The preparation method of non-close heap inverse opal photonic crystal may further comprise the steps:
The first step is feedstock production SiO with the tetraethoxy
2Nanometer or sub-micron ball;
Second step, preparation diameter polystyrene spheres particle;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 5～8 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 2～3, then respectively with two kinds of spherical particles ultra-sonic dispersion in organic solvent, ultrasonic time is 2～3h; Two suspension-s are mixed the ultrasonic 2～3h of continued; Obtain mixing suspension, its particulate massfraction is 1%～2%, wherein: D
SiO2Expression SiO
2Diameter, D
PolystyreneThe diameter of expression polystyrene, m
SiO2Expression SiO
2Quality, m
PolystyreneThe quality of expression polystyrene;
The 4th step, the vertical immersion of substrate has been placed stably in the mixing suspension, 40～50 ℃ of following vacuum-dryings, treat that solution evaporates fully after, grow the two size photonic crystals of one deck at substrate surface;
In the 5th step, two size photonic crystals are calcined 4～6h down at 400～500 ℃, i.e. De Feimi heap inverse opal photonic crystal.
Wherein
The said the first step prepares SiO
2Nanometer or sub-micron ball are realized according to following steps:
At first, the dehydrated alcohol that tetraethoxy is dissolved in a parts by volume is configured to solution A;
Secondly, be that the dehydrated alcohol that 25%～28% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1～2 with the mass concentration of 1～5 times of tetraethoxy volume;
Then, solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.4～0.6mol/L in the mixed solution, and behind the reaction 22h, precipitation separation in 50～60 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball.
Preparation diameter polystyrene spheres particle is realized according to following steps in said second step:
At first, in round-bottomed flask, add deionized water, behind the logical nitrogen, will add vinylbenzene, controlling cinnamic concentration is 1～5mol/L, and continuing logical nitrogen and keeping temperature is 70～80 ℃;
Then; Adding concentration is the persulfate aqueous solution of 0.003～0.01mol/L, and the quality of Potassium Persulphate is 1～2% of a vinylbenzene quality, polyreaction 10～15h; Gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards.
Organic solvent is ethanol, methyl alcohol, acetone, acetonitrile or Virahol in said the 3rd step.
Substrate is that slide glass, ito glass or silicon chip and other can bear the base material of calcining temperature in said the 4th step.
Substrate is before immersing mixing suspension in said the 4th step; Using earlier mass concentration successively is 1%～2% hydrofluoric acid; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1%～2%, with behind the deionized water rinsing under infrared lamp dry for standby.
Described SiO
2Spheroid can be used TiO
2, ZrO
2, A1
2O
3, Fe
2O
3, CdS, Nb
2O
5, WO
3The material higher etc. specific refractory power replaces, to widen the range of application of counter opal structure.
Compared with prior art, advantage of the present invention is:
(1) The non-close-packed prepared Inverse Opal Photonic Crystals periodic arrangement intact, and its periodic arrangement of the adjustable gap; usually densely packed photonic crystal etching to obtain non-close-packed opal structure obtained after filling corrosion Inverse Opal Photonic non-close-packed crystal, but closely packed etched single dimension photonic crystal, one of the morphology of colloidal spheres easily damaged, and the arrangement is likely to cause damage, this method uses two types of colloidal particles, wherein the inorganic particles the ratio of the gap can be controlled polystyrene particles, polystyrene is removed by calcining the silica does not cause damage, and usually 300 ~ 500 ℃ calcination to remove the organic material in a temperature range, causes the non-close-packed inverse opal structure more closely arranged.
(2) production technique is simple, and equipment is simple, and is easy and simple to handle, and preparation cycle is shorter, and productive rate is higher; At present; If recharging technology to close pile structure etching, utilization prepares the fragile colloid arrangement of non-close heap counter opal structure; And it is complicated that the relative the present invention of its technology wants; And utilize microfabrication to prepare non-close pile structure; Though its precision is high; Preparation cycle is arranged; But the non-close heap photonic crystal with inverse opal structure preparation cycle of preparation is long; Can not as self-assembly method, prepare in large area; And this technology not only can be as utilizing cycle weak point in the self-assembly method; But the advantage of large-area preparation; And because what utilize is two size photonic crystals; The damage that does not have etching to bring, productive rate is high, and technology controlling and process is stable.
(3) SiO
2Spherical particles and organic microballoon are separately preparation, do not have influencing each other in the reaction, also do not exist like dabbling difficulty among the preparation method of the resilient material of perfusion expansion performance.
Embodiment
Below in conjunction with embodiment the present invention is explained further details.
Embodiment one
The preparation method of non-close heap inverse opal photonic crystal may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 25% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1 again with the isopyknic mass concentration of tetraethoxy; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.4mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 60 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, will add vinylbenzene; Controlling cinnamic concentration is 1mol/L; Continuing logical nitrogen and keeping temperature is 80 ℃, and then, adding concentration is the persulfate aqueous solution of 0.01mol/L; The quality of Potassium Persulphate is 2% of a vinylbenzene quality; Polyreaction 15h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 5 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 3, then respectively with two kinds of spherical particles ultra-sonic dispersion in ethanol, ultrasonic time is 2h, and two suspension-s are mixed the ultrasonic 2h of continued, obtains mixing suspension, its particulate massfraction is 2%;
The 4th step; It is 1.5% hydrofluoric acid that slide glass is used mass concentration successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1.5%; With behind the deionized water rinsing under infrared lamp dry for standby, then the vertical immersion of slide glass has been placed stably in the mixing suspension, 50 ℃ of following vacuum-dryings; After treating that solution evaporates fully, grow the two size photonic crystals of one deck in slide surface;
In the 5th step, two size photonic crystals are calcined 4h down at 500 ℃, i.e. De Feimi heap inverse opal photonic crystal.
Embodiment two
The preparation method of non-close heap inverse opal photonic crystal may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 28% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 2 again with the mass concentration of 5 times of tetraethoxy volumes; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.6mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 50 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, will add vinylbenzene; Controlling cinnamic concentration is 5mol/L; Continuing logical nitrogen and keeping temperature is 70 ℃, and then, adding concentration is the persulfate aqueous solution of 0.003mol/L; The quality of Potassium Persulphate is 2% of a vinylbenzene quality; Polyreaction 10h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 8 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 2, then respectively with two kinds of spherical particles ultra-sonic dispersion in methyl alcohol, ultrasonic time is 2h, and two suspension-s are mixed the ultrasonic 3h of continued, obtains mixing suspension, its particulate massfraction is 1%;
The 4th step; It is 1% hydrofluoric acid that ito glass is used mass concentration successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1%; With behind the deionized water rinsing under infrared lamp dry for standby, then the vertical immersion of ito glass has been placed stably in the mixing suspension, 40 ℃ of following vacuum-dryings; After treating that solution evaporates fully, go out the two size photonic crystals of one deck in the ito glass surface growth;
In the 5th step, two size photonic crystals are calcined 6h down at 400 ℃, i.e. De Feimi heap inverse opal photonic crystal.
Embodiment three
The preparation method of non-close heap inverse opal photonic crystal may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 25% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1.5 again with the mass concentration of 3 times of tetraethoxy volumes; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.5mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 55 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, add vinylbenzene; Controlling cinnamic concentration is 2mol/L; Continuing logical nitrogen and keeping temperature is 70 ℃, and then, adding concentration is the persulfate aqueous solution of 0.005mol/L; The quality of Potassium Persulphate is 1.5% of a vinylbenzene quality; Polyreaction 12h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 6 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 3, then respectively with two kinds of spherical particles ultra-sonic dispersion in acetone, ultrasonic time is 3h, and two suspension-s are mixed the ultrasonic 2h of continued, obtains mixing suspension, its particulate massfraction is 1.5%;
The 4th step; It is 2% hydrofluoric acid that silicon chip is used mass concentration successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 2%; With behind the deionized water rinsing under infrared lamp dry for standby, then the vertical immersion of silicon chip has been placed stably in the mixing suspension, 40 ℃ of following vacuum-dryings; After treating that solution evaporates fully, grow the two size photonic crystals of one deck at silicon chip surface;
In the 5th step, two size photonic crystals are calcined 5h down at 450 ℃, i.e. De Feimi heap inverse opal photonic crystal.
Embodiment four
The preparation method of non-close heap inverse opal photonic crystal may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 28% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 2 again with the mass concentration of 2 times of tetraethoxy volumes; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.4mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 50 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, will add vinylbenzene; Controlling cinnamic concentration is 3mol/L; Continuing logical nitrogen and keeping temperature is 70 ℃, and then, adding concentration is the persulfate aqueous solution of 0.008mol/L; The quality of Potassium Persulphate is 2% of a vinylbenzene quality; Polyreaction 12h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 7 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 2, then respectively with two kinds of spherical particles ultra-sonic dispersion in acetonitrile, ultrasonic time is 2h, and two suspension-s are mixed the ultrasonic 2h of continued, obtains mixing suspension, its particulate massfraction is 2%;
The 4th step; It is 2% hydrofluoric acid that slide glass is used mass concentration successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 2%; With behind the deionized water rinsing under infrared lamp dry for standby, then the vertical immersion of slide glass has been placed stably in the mixing suspension, 40 ℃ of following vacuum-dryings; After treating that solution evaporates fully, grow the two size photonic crystals of one deck in slide surface;
In the 5th step, two size photonic crystals are calcined 5h down at 400 ℃, i.e. De Feimi heap inverse opal photonic crystal.
Embodiment five
The preparation method of non-close heap inverse opal photonic crystal may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 25% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1.5 again with the mass concentration of 4 times of tetraethoxy volumes; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.4mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 60 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, will add vinylbenzene; Controlling cinnamic concentration is 5mol/L; Continuing logical nitrogen and keeping temperature is 80 ℃, and then, adding concentration is the persulfate aqueous solution of 0.006mol/L; The quality of Potassium Persulphate is 2% of a vinylbenzene quality; Polyreaction 15h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 7 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 2.5, then respectively with two kinds of spherical particles ultra-sonic dispersion in Virahol, ultrasonic time is 3h, and two suspension-s are mixed the ultrasonic 3h of continued, obtains mixing suspension, its particulate massfraction is 2%;
The 4th step; It is 1.5% hydrofluoric acid that silicon chip is used mass concentration successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1.5%; With behind the deionized water rinsing under infrared lamp dry for standby, then the vertical immersion of silicon chip has been placed stably in the mixing suspension, 50 ℃ of following vacuum-dryings; After treating that solution evaporates fully, grow the two size photonic crystals of one deck at silicon chip surface;
In the 5th step, two size photonic crystals are calcined 5h down at 500 ℃, i.e. De Feimi heap inverse opal photonic crystal.
Embodiment six～embodiment 12
Different be unique with embodiment one used TiO respectively
2, ZrO
2, Al
2O
3, Fe
2O
3, CdS, Nb
2O
5, WO
3Substitute SiO
2Spherical particles.
More than among each embodiment, the organic solvent that the spherical particles ultra-sonic dispersion is used can also have other multiple choices; Among each embodiment, substrate can be other the carrier that can bear final calcining temperature such as slide glass, ito glass or silicon chip.
Claims (10)
1. the preparation method of non-close heap inverse opal photonic crystal is characterized in that, may further comprise the steps:
The first step is feedstock production SiO with the tetraethoxy
2Nanometer or sub-micron ball;
Second step, preparation diameter polystyrene spheres particle;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 5～8 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 2～3, then respectively with two kinds of spherical particles ultra-sonic dispersion in organic solvent, ultrasonic time is 2～3h; Two suspension-s are mixed the ultrasonic 2～3h of continued; Obtain mixing suspension, its particulate massfraction is 1%～2%, wherein: D
SiO2Expression SiO
2Diameter, D
PolystyreneThe diameter of expression polystyrene, m
SiO2Expression SiO
2Quality, m
PolystyreneThe quality of expression polystyrene;
The 4th step, the vertical immersion of substrate has been placed stably in the mixing suspension, 40～50 ℃ of following vacuum-dryings, treat that solution evaporates fully after, grow the two size photonic crystals of one deck at substrate surface;
In the 5th step, two size photonic crystals are calcined 4～6h down at 400～500 ℃, i.e. De Feimi heap inverse opal photonic crystal.
2. the preparation method of non-close heap inverse opal photonic crystal according to claim 1 is characterized in that, the said the first step prepares SiO
2Nanometer or sub-micron ball are realized according to following steps:
At first, the dehydrated alcohol that tetraethoxy is dissolved in a parts by volume is configured to solution A;
Secondly, be that the dehydrated alcohol that 25%～28% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1～2 with the mass concentration of 1～5 times of tetraethoxy volume;
Then, solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.4～0.6mol/L in the mixed solution, and behind the reaction 22h, precipitation separation in 50～60 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball.
3. the preparation method of non-close heap inverse opal photonic crystal according to claim 1 is characterized in that, preparation diameter polystyrene spheres particle is realized according to following steps in said second step:
At first, in round-bottomed flask, add deionized water, behind the logical nitrogen, add vinylbenzene, controlling cinnamic concentration is 1～5mol/L, and continuing logical nitrogen and keeping temperature is 70～80 ℃;
Then; Adding concentration is the persulfate aqueous solution of 0.003～0.01mol/L, and the quality of Potassium Persulphate is 1～2% of a vinylbenzene quality, polyreaction 10～15h; Gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards.
4. the preparation method of non-close heap inverse opal photonic crystal according to claim 1 is characterized in that, organic solvent is ethanol, methyl alcohol, acetone, acetonitrile or Virahol in said the 3rd step.
5. the preparation method of non-close heap inverse opal photonic crystal according to claim 1 is characterized in that, substrate is slide glass, ito glass or silicon chip in said the 4th step.
6. the preparation method of non-close heap inverse opal photonic crystal according to claim 1; It is characterized in that; Substrate is before immersing mixing suspension in said the 4th step; Using earlier mass concentration successively is 1%～2% hydrofluoric acid; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1%～2%, with behind the deionized water rinsing under infrared lamp dry for standby.
7. the preparation method of non-close heap inverse opal photonic crystal according to claim 1 is characterized in that, uses TiO
2, ZrO
2, Al
2O
3, Fe
2O
3, CdS, Nb
2O
5Or WO
3Substitute described SiO
2Spheroid.
8. the preparation method of non-close heap inverse opal photonic crystal is characterized in that, may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 25% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1 again with the isopyknic mass concentration of tetraethoxy; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.4mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 60 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, will add vinylbenzene; Controlling cinnamic concentration is 1mol/L; Continuing logical nitrogen and keeping temperature is 80 ℃, and then, adding concentration is the persulfate aqueous solution of 0.01mol/L; The quality of Potassium Persulphate is 2% of a vinylbenzene quality; Polyreaction 15h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 5 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 3, then respectively with two kinds of spherical particles ultra-sonic dispersion in organic solvent, ultrasonic time is 2h, and two suspension-s are mixed the ultrasonic 2h of continued, obtains mixing suspension, its particulate massfraction is 2%, wherein: D
SiO2Expression SiO
2Diameter, D
PolystyreneThe diameter of expression polystyrene, m
SiO2Expression SiO
2Quality, m
PolystyreneThe quality of expression polystyrene, described organic solvent is ethanol, methyl alcohol, acetone, acetonitrile or Virahol;
The 4th step; It is 1.5% hydrofluoric acid that mass concentration is used in substrate successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1.5%; With behind the deionized water rinsing under infrared lamp dry for standby; Then the vertical immersion of substrate has been placed stably in the mixing suspension; 50 ℃ of following vacuum-dryings; After treating that solution evaporates fully; Grow the two size photonic crystals of one deck at substrate surface, said substrate is slide glass, ito glass or silicon chip;
In the 5th step, two size photonic crystals are calcined 4h down at 500 ℃, i.e. De Feimi heap inverse opal photonic crystal.
9. the preparation method of non-close heap inverse opal photonic crystal is characterized in that, may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 28% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 2 again with the mass concentration of 5 times of tetraethoxy volumes; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.6mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 50 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, add vinylbenzene; Controlling cinnamic concentration is 5mol/L; Continuing logical nitrogen and keeping temperature is 70 ℃, and then, adding concentration is the persulfate aqueous solution of 0.003mol/L; The quality of Potassium Persulphate is 2% of a vinylbenzene quality; Polyreaction 10h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 8 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 2, then respectively with two kinds of spherical particles ultra-sonic dispersion in organic solvent, ultrasonic time is 2h, and two suspension-s are mixed the ultrasonic 3h of continued, obtains mixing suspension, its particulate massfraction is 1%, wherein: D
SiO2Expression SiO
2Diameter, D
PolystyreneThe diameter of expression polystyrene, m
SiO2Expression SiO
2Quality, m
PolystyreneThe quality of expression polystyrene, described organic solvent is ethanol, methyl alcohol, acetone, acetonitrile or Virahol;
The 4th step; It is 1% hydrofluoric acid that mass concentration is used in substrate successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 1%; With behind the deionized water rinsing under infrared lamp dry for standby; Then the vertical immersion of substrate has been placed stably in the mixing suspension; 40 ℃ of following vacuum-dryings; After treating that solution evaporates fully; Grow the two size photonic crystals of one deck at substrate surface, said substrate is slide glass, ito glass or silicon chip;
In the 5th step, two size photonic crystals are calcined 6h down at 400 ℃, i.e. De Feimi heap inverse opal photonic crystal.
10. the preparation method of non-close heap inverse opal photonic crystal is characterized in that, may further comprise the steps:
The first step; The dehydrated alcohol that earlier tetraethoxy is dissolved in a parts by volume is configured to solution A, is that the dehydrated alcohol that 25% ammoniacal liquor is dissolved in the b parts by volume is configured to solution B, a: b=1: 1.5 again with the mass concentration of 3 times of tetraethoxy volumes; Then; Solution A is placed magnetic agitation equipment, under not stopping stirring, solution B is added in the solution A, the concentration of tetraethoxy is 0.5mol/L in the mixed solution; Behind the reaction 22h; Precipitation separation in 55 ℃ of dryings, obtains SiO behind the centrifuge washing
2Nanometer or sub-micron ball;
Second step; In round-bottomed flask, add earlier deionized water, behind the logical nitrogen, add vinylbenzene; Controlling cinnamic concentration is 2mol/L; Continuing logical nitrogen and keeping temperature is 70 ℃, and then, adding concentration is the persulfate aqueous solution of 0.005mol/L; The quality of Potassium Persulphate is 1.5% of a vinylbenzene quality; Polyreaction 12h, gained suspension-s absolute ethanol washing, vacuum lyophilization 3h promptly obtains the diameter polystyrene spheres particle afterwards;
The 3rd step was D with particle diameter ratio
SiO2: D
PolystyreneTwo kinds of spherical particles of=1: 6 are m by mass ratio
SiO2: m
PolystyreneRespectively take by weighing at=1: 3, then respectively with two kinds of spherical particles ultra-sonic dispersion in organic solvent, ultrasonic time is 3h, and two suspension-s are mixed the ultrasonic 2h of continued, obtains mixing suspension, its particulate massfraction is 1.5%, wherein: D
SiO2Expression SiO
2Diameter, D
PolystyreneThe diameter of expression polystyrene, m
SiO2Expression SiO
2Quality, m
PolystyreneThe quality of expression polystyrene, described organic solvent is ethanol, methyl alcohol, acetone, acetonitrile or Virahol;
The 4th step; It is 2% hydrofluoric acid that mass concentration is used in substrate successively; Volume ratio is the vitriol oil-hydrogen peroxide mixed solution of 7: 3; And mass concentration is each ultrasonic cleaning 15min of sodium hydroxide solution of 2%; With behind the deionized water rinsing under infrared lamp dry for standby; Then the vertical immersion of substrate has been placed stably in the mixing suspension; 40 ℃ of following vacuum-dryings; After treating that solution evaporates fully; Grow the two size photonic crystals of one deck at substrate surface, said substrate is slide glass, ito glass or silicon chip;
In the 5th step, two size photonic crystals are calcined 5h down at 450 ℃, i.e. De Feimi heap inverse opal photonic crystal.
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| CN102586873A (en) * | 2012-03-07 | 2012-07-18 | 北京交通大学 | One-step preparation method for Al2O3 reverse opal structure |
| CN103352255A (en) * | 2013-06-23 | 2013-10-16 | 安泰科技股份有限公司 | Preparation method of photonic crystal with inverse opal structure |
| CN103483609A (en) * | 2013-09-25 | 2014-01-01 | 青岛大学 | Preparation method of non-close-packed photonic crystal film |
| CN104891579A (en) * | 2015-05-28 | 2015-09-09 | 扬州大学 | Vertical deposition synthetic method of inverse opal structure Co3O4@SiO2 nano coating material |
| CN108560043A (en) * | 2018-02-01 | 2018-09-21 | 中国工程物理研究院激光聚变研究中心 | One kind can self-supporting colloidal crystal and its simple and effective preparation method |
| CN108947337A (en) * | 2018-06-22 | 2018-12-07 | 东莞市夏日东升首饰有限公司 | A kind of preparation method of artificial opals |
| CN110577370A (en) * | 2019-10-24 | 2019-12-17 | 南京工程学院 | Amorphous photonic crystal structure color film capable of being used outdoors and preparation method thereof |
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| CN101655610A (en) * | 2009-09-11 | 2010-02-24 | 中国科学院长春应用化学研究所 | Preparation method of inverse opal hydrogel photonic crystal with hybridized structure |
| WO2010119247A2 (en) * | 2009-04-14 | 2010-10-21 | De La Rue International Limited | Security device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2010119247A2 (en) * | 2009-04-14 | 2010-10-21 | De La Rue International Limited | Security device |
| CN101655610A (en) * | 2009-09-11 | 2010-02-24 | 中国科学院长春应用化学研究所 | Preparation method of inverse opal hydrogel photonic crystal with hybridized structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102586873A (en) * | 2012-03-07 | 2012-07-18 | 北京交通大学 | One-step preparation method for Al2O3 reverse opal structure |
| CN102586873B (en) * | 2012-03-07 | 2014-12-24 | 北京交通大学 | One-step preparation method for Al2O3 reverse opal structure |
| CN103352255A (en) * | 2013-06-23 | 2013-10-16 | 安泰科技股份有限公司 | Preparation method of photonic crystal with inverse opal structure |
| CN103352255B (en) * | 2013-06-23 | 2016-03-02 | 安泰科技股份有限公司 | A kind of preparation method with the photonic crystal of counter opal structure |
| CN103483609A (en) * | 2013-09-25 | 2014-01-01 | 青岛大学 | Preparation method of non-close-packed photonic crystal film |
| CN103483609B (en) * | 2013-09-25 | 2016-01-20 | 青岛大学 | A kind of preparation method of not closed packing photon crystal film |
| CN104891579A (en) * | 2015-05-28 | 2015-09-09 | 扬州大学 | Vertical deposition synthetic method of inverse opal structure Co3O4@SiO2 nano coating material |
| CN108560043A (en) * | 2018-02-01 | 2018-09-21 | 中国工程物理研究院激光聚变研究中心 | One kind can self-supporting colloidal crystal and its simple and effective preparation method |
| CN108947337A (en) * | 2018-06-22 | 2018-12-07 | 东莞市夏日东升首饰有限公司 | A kind of preparation method of artificial opals |
| CN110577370A (en) * | 2019-10-24 | 2019-12-17 | 南京工程学院 | Amorphous photonic crystal structure color film capable of being used outdoors and preparation method thereof |
| CN110577370B (en) * | 2019-10-24 | 2022-02-11 | 南京工程学院 | Amorphous photonic crystal structure color film capable of being used outdoors and preparation method thereof |
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