CN110304636A - A kind of method that vacuum filtration prepares photo crystal thick - Google Patents
A kind of method that vacuum filtration prepares photo crystal thick Download PDFInfo
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- CN110304636A CN110304636A CN201910571987.5A CN201910571987A CN110304636A CN 110304636 A CN110304636 A CN 110304636A CN 201910571987 A CN201910571987 A CN 201910571987A CN 110304636 A CN110304636 A CN 110304636A
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- crystal thick
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- 239000013078 crystal Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000003828 vacuum filtration Methods 0.000 title claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000004005 microsphere Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000009792 diffusion process Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 15
- 239000004038 photonic crystal Substances 0.000 description 13
- 238000001914 filtration Methods 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- 230000007547 defect Effects 0.000 description 7
- 238000000967 suction filtration Methods 0.000 description 6
- 239000004793 Polystyrene Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920002223 polystyrene Polymers 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 239000004926 polymethyl methacrylate Substances 0.000 description 3
- 229920001940 conductive polymer Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/085—Funnel filters; Holders therefor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Filtering Materials (AREA)
Abstract
The present invention relates to a kind of methods that vacuum filtration prepares photo crystal thick, comprising: mono-dispersion microballoon dispersion is obtained dispersion liquid in a solvent；Clean smooth perforated substrate is placed on filter；Dispersion liquid is poured into perforated substrate, is filtered by vacuum to solvent and is drained；It removes substrate and carries out drying and processing；It repeats to filter, drying for several times, obtains certain thickness photo crystal thick.Compared with prior art, the present invention realizes preparation of the period from 100nm-1 μm of photo crystal thick by changing the partial size of mono-dispersion microballoon, passes through the concentration for adjusting mono-dispersion microballoon, dosage, speed is filtered, the preparation of the photo crystal thick of 1 μm of -1cm of thickness is realized.
Description
Technical field
The present invention relates to photonic crystal preparation fields, and the side of photo crystal thick is prepared more particularly, to a kind of vacuum filtration
Method.
Background technique
Material with optical band gap gap (Photonic Band-Gap) is also known as photonic crystal, it refers to dielectric constant (folding
Penetrate rate) periodically variable one kind material on submicron-scale.The concept of photonic crystal be earliest 1987 by
What Yablonovitch and two people of John independently proposed, be to be got by traditional crystal concept analogy: in crystal, having a size of 10-
The atom periodic arrangement of 10m can make X-ray that diffraction occur；In the photonic crystal, the periodic structure having a size of 10-7m can
So that diffraction occurs for visible light.U.S.'s Science magazine 1999 photonic crystal be classified as the following six big research hotspots it
One, predictive of the bright prospects of photonic crystal research.
The preparation of photonic crystal of opals structure mainly has self-assembly method and spray coating method at present, and wherein self-assembly method obtains
Photonic crystal order is good, but manufacturing cycle is longer, and thickness is usually no more than 10 μm, and spray coating method is suitable for the light of large area
Sub- crystal preparation, but obtained photonic crystal order is poor.
Therefore, it is necessary to a kind of completely new, simple processes, the low-cost, method that is able to achieve photo crystal thick preparation.
Chinese patent CN100410301C discloses a kind of side with preparation of ordered porous conductive polymer by suction filtration/immersion method
Method.This method immerses monomer in colloidal crystal template simultaneously with initiator by suction filtration mode to polymerize, and then removes template and obtains
To preparing 3-D ordered multiporous conducting polymer.The present invention and the main distinction of patent CN100410301C are: 1) of the invention
The mono-dispersion microballoon is silicon dioxide microsphere, is had the advantages that corrosion-resistant, resistant to high temperature；2) substrate of the present invention is with gas
The carbon paper of body diffused layer has smaller aperture, excellent electric conductivity compared with patent CN100410301C；3) present invention adopts
With multistep processes, the defect formed after drying can be effectively reduced, patent CN100410301C does not have this advantage.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of vacuum filtrations to prepare
The method of photo crystal thick is suitable for a variety of perforated substrates, simple process and low cost.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of method that vacuum filtration prepares photo crystal thick, comprising:
Mono-dispersion microballoon dispersion is obtained into dispersion liquid in a solvent；
Clean smooth perforated substrate is placed on filter；
Dispersion liquid is poured into perforated substrate, is filtered by vacuum to solvent and is drained；
It removes substrate and carries out drying and processing；
It repeats to filter, drying for several times, obtains the photo crystal thick of 1 μm of -1cm thickness.
The mono-dispersion microballoon includes silicon dioxide microsphere.
The partial size of the mono-dispersion microballoon is 100nm-1 μm.
The solvent is ethyl alcohol or deionized water.
The mass concentration of the dispersion liquid is 0.2-1.0%, and the dispersion liquid of the concentration can form uniform after filtering
Photo crystal thick advantageously reduces the generation of defect.
The perforated substrate is the carbon fiber paper with gas diffusion layers, and the aperture of perforated membrane is necessarily less than mono-dispersion microballoon
Partial size.
The flow velocity that control filters when vacuum filtration is 1-5L/h.
It filters, the number of repetition of drying is 0-5 times, can reduce photonic crystal caliper defects by the flow velocity that control filters
Formation；The defects of by repeatedly drying and filtering, on the one hand can making the crack formed after previous step is dry is filled,
On the other hand the thickness of photonic crystal is increased.
Compared with prior art, present invention process is simple, low in cost, applied widely, it can be achieved that mono-dispersion microballoon, no
The preparation of the photo crystal thick of stack pile.
Partial size by changing mono-dispersion microballoon realizes preparation of the period from 100nm-1 μm of photo crystal thick；It is logical
The concentration of mono-dispersion microballoon is overregulated, dosage filters speed, realizes the preparation of the photo crystal thick of 1 μm of -1cm of thickness.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
A kind of method that vacuum filtration method prepares photo crystal thick, comprising the following steps:
1) mono-dispersion microballoon for being 100nm-1 μm by partial size, such as silicon dioxide microsphere, polystyrene microsphere or poly- methyl
Methyl acrylate microballoon is placed in beaker, ethyl alcohol or deionized water is added as solvent, it is 0.2- that ultrasonic disperse, which obtains mass concentration,
The dispersion liquid of 1.0% dispersion liquid, the concentration can form uniform photo crystal thick after filtering, and advantageously reduce defect
Generation；
2) clean smooth perforated substrate is placed on sand core filter, the substrate that can be used is with gas diffusion layers
Carbon fiber paper.The aperture of perforated membrane is necessarily less than the partial size of mono-dispersion microballoon；
3) vacuum pump is opened, dispersion liquid is poured into, the flow velocity for controlling suction filtration is 1-5L/h, until solvent is drained；
4) substrate is removed, is placed in drying box and dries；
5) it repeats to filter, baking step 0-5 times, photonic crystal caliper defects can be reduced by the flow velocity that control filters
It is formed；The defects of by repeatedly drying and filtering, on the one hand can making the crack formed after previous step is dry is filled, separately
On the one hand the thickness for increasing photonic crystal, finally obtains the photo crystal thick of required thickness.
Above scheme bring direct technology effect is to prepare photo crystal thick, technique letter using vacuum filtration method
It is single, it is low in cost, realize the preparation of photo crystal thick.
More detailed case study on implementation below, by following case study on implementation further illustrate technical solution of the present invention with
And the technical effect that can be obtained.
Embodiment 1
With a thickness of 10 μm of silica photo crystal thicks the preparation method is as follows:
1) it takes the silica mono-dispersion microballoon that 0.1g partial size is 300nm in beaker, 50ml dehydrated alcohol, ultrasound is added
Disperse 30min, forms uniform dispersion liquid；
2) taking area is 4cm2The carbon fiber paper with gas diffusion layers, be layered on sand core filter, clamping device；
3) dispersion liquid is poured into, vacuum pump is opened, adjusting flow velocity is 1L/h；
4) after the completion of all filtering, carbon fiber paper is removed, is placed in drying box, 60 DEG C, dry 1h.
Embodiment 2
With a thickness of 1cm polystyrene photon crystal thick film the preparation method is as follows::
1) it takes the polystyrene mono-dispersion microballoon that 0.5g partial size is 500nm in beaker, 200ml deionized water is added, surpass
Sound disperses 30min, forms uniform dispersion liquid；
2) taking area is 4cm2Aperture be 0.22 μm of filter membrane, be layered on sand core filter, clamping device；
3) dispersion liquid is poured into, vacuum pump is opened, adjusting flow velocity is 2L/h；
4) after the completion of all filtering, filter membrane is removed, is placed in drying box, 60 DEG C, dry 1h.
5) suction filtration, drying steps 5 times are repeated, the polystyrene photon crystal thick film with a thickness of 1cm is obtained.
Embodiment 3
With a thickness of 100 μm of silica photo crystal thicks the preparation method is as follows::
1) it takes the silicon dioxide microsphere that 1g partial size is 100nm in beaker, 500ml deionized water, ultrasonic disperse is added
30min forms uniform dispersion liquid；
2) taking area is 4cm2Aperture be 40nm filter membrane, be layered on sand core filter, clamping device；
3) dispersion liquid is poured into, vacuum pump is opened, adjusting flow velocity is 1L/h；
4) after the completion of all filtering, filter membrane is removed, is placed in drying box, 60 DEG C, dry 1h.
5) suction filtration, drying steps 2 times are repeated, the silica photo crystal thick with a thickness of 100 μm is obtained.
Embodiment 4
With a thickness of 300 μm of polymethyl methacrylate photo crystal thicks the preparation method is as follows::
1) it takes the polymethyl methacrylate mono-dispersion microballoon that 1g partial size is 1 μm in beaker, 100ml deionization is added
Water, ultrasonic disperse 60min form uniform dispersion liquid；
2) taking area is 8cm2Aperture be 0.5 μm of filter membrane, be layered on sand core filter, clamping device；
3) dispersion liquid is poured into, vacuum pump is opened, adjusting flow velocity is 5L/h；
4) after the completion of all filtering, filter membrane is removed, is placed in drying box, 60 DEG C, dry 2h.
5) suction filtration, drying steps 4 times are repeated, the polymethyl methacrylate photo crystal thick with a thickness of 300 μm is obtained.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (9)
1. a kind of method that vacuum filtration prepares photo crystal thick, which is characterized in that this method comprises:
Mono-dispersion microballoon dispersion is obtained into dispersion liquid in a solvent；
Clean smooth perforated substrate is placed on filter；
Dispersion liquid is poured into perforated substrate, is filtered by vacuum to solvent and is drained；
It removes substrate and carries out drying and processing；
It repeats to filter, drying for several times, obtains certain thickness photo crystal thick.
2. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that the list
Dispersion microsphere includes silicon dioxide microsphere.
3. the method that a kind of vacuum filtration according to claim 1 or 2 prepares photo crystal thick, which is characterized in that institute
The partial size for stating mono-dispersion microballoon is 100nm-1 μm.
4. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that described molten
Agent is ethyl alcohol or deionized water.
5. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that described point
The mass concentration of dispersion liquid is 0.2-1.0%.
6. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that described more
Hole substrate is the carbon fiber paper with gas diffusion layers.
7. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that vacuum is taken out
The flow velocity that control filters when filter is 1-5L/h.
8. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that it filters,
The number of repetition of drying is 0-5 times.
9. the method that a kind of vacuum filtration according to claim 1 prepares photo crystal thick, which is characterized in that the light
Sub- crystal thick film with a thickness of 1 μm of -1cm.
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Cited By (4)
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|---|---|---|---|---|
| CN110983424A (en) * | 2019-11-19 | 2020-04-10 | 上海交通大学 | Method for preparing large-area crack-free thick film photonic crystal on porous substrate |
| CN111082147A (en) * | 2019-12-09 | 2020-04-28 | 上海交通大学 | Preparation method of photonic crystal lithium-sulfur battery based on large-area thick film controllable texture |
| CN114420995A (en) * | 2022-01-07 | 2022-04-29 | 上海交通大学 | Selenium-enriched lithium selenium battery based on three-dimensional ordered porous carbon optical crystal and preparation method thereof |
| CN114839702A (en) * | 2022-04-27 | 2022-08-02 | 中国科学院力学研究所 | Method and system for rapidly preparing photonic crystal through low-pressure auxiliary evaporation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110983424A (en) * | 2019-11-19 | 2020-04-10 | 上海交通大学 | Method for preparing large-area crack-free thick film photonic crystal on porous substrate |
| CN111082147A (en) * | 2019-12-09 | 2020-04-28 | 上海交通大学 | Preparation method of photonic crystal lithium-sulfur battery based on large-area thick film controllable texture |
| CN111082147B (en) * | 2019-12-09 | 2023-09-12 | 上海交通大学 | Preparation method of photonic crystal lithium sulfur battery based on large-area thick film controllable texture |
| CN114420995A (en) * | 2022-01-07 | 2022-04-29 | 上海交通大学 | Selenium-enriched lithium selenium battery based on three-dimensional ordered porous carbon optical crystal and preparation method thereof |
| CN114839702A (en) * | 2022-04-27 | 2022-08-02 | 中国科学院力学研究所 | Method and system for rapidly preparing photonic crystal through low-pressure auxiliary evaporation |
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