CN102617874B - Two-dimensional colloid crystal thin film and preparation method thereof - Google Patents
Two-dimensional colloid crystal thin film and preparation method thereof Download PDFInfo
- Publication number
- CN102617874B CN102617874B CN201210048371.8A CN201210048371A CN102617874B CN 102617874 B CN102617874 B CN 102617874B CN 201210048371 A CN201210048371 A CN 201210048371A CN 102617874 B CN102617874 B CN 102617874B
- Authority
- CN
- China
- Prior art keywords
- water
- colloidal crystal
- crystal film
- dimensional colloidal
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 65
- 239000000084 colloidal system Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000010409 thin film Substances 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000839 emulsion Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 37
- 239000004793 Polystyrene Substances 0.000 claims description 29
- 229920002223 polystyrene Polymers 0.000 claims description 29
- 239000005357 flat glass Substances 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 7
- 238000007720 emulsion polymerization reaction Methods 0.000 claims description 7
- 238000012546 transfer Methods 0.000 claims description 7
- 239000004159 Potassium persulphate Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000002612 dispersion medium Substances 0.000 claims description 5
- 238000007667 floating Methods 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000019394 potassium persulphate Nutrition 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 230000009182 swimming Effects 0.000 claims description 5
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract 3
- 239000007788 liquid Substances 0.000 abstract 2
- 239000004005 microsphere Substances 0.000 abstract 2
- 239000011806 microball Substances 0.000 description 10
- 238000001338 self-assembly Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003505 polymerization initiator Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 239000011805 ball Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229920002319 Poly(methyl acrylate) Polymers 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006059 cover glass Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 238000000054 nanosphere lithography Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Landscapes
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a two-dimensional colloid crystal thin film and a preparation method thereof. The method comprises the following steps of: (1) uniformly mixing colloid microsphere emulsion and ethanol at an equal volume to obtain a mixed liquid A; (2) placing a hydrophilically treated glass sheet in a culture dish, and then adding water to the culture dish until the water surface reaches the upper surface of the glass sheet but does not immerse the upper surface; and (3) uniformly and continuously dripping the mixed liquid A to the upper surface of the glass sheet by a continuous transmission device, and after the colloid microspheres completely disperse to the water-gas interface, adding a surfactant aqueous solution to obtain the two-dimensional colloid crystal thin film. According to the invention, the continuous transmission device is utilized to realize slow, uniform and continuous dripping of the colloid emulsion, so that the two-dimensional colloid crystal with better crystal quality is obtained; and furthermore, a mechanical manner replaces the artificial manual dripping, so that the manual labor force is effectively saved, and an effective way is provided for realizing the industrial application of the colloid crystal in the field of the nano technology.
Description
Technical field
The present invention relates to a kind of two-dimensional colloidal crystal film and preparation method thereof, belong to colloidal crystal and preparing technical field thereof.
Background technology
Self-assembly, as the powerful and effective means of the one of preparing ordered nano-structure, has been confirmed to be the important component part of nano material and nanosecond science and technology.The construction unit of self-assembly is of a great variety, from molecule, macromole, colloidal particle, DNA and protein, to macro object.Wherein, colloid micro ball or nanometer ball are widely studied, because the scope of their yardstick from tens nanometers to several microns approaches with the resolving limit of tradition design technology.The development of colloid science has also promoted the synthetic of highly single dispersion colloid particle (silicon-dioxide or polymkeric substance).Monodispersed colloidal solid can be self-assembled into two dimension (2D) and three-dimensional (3D) colloidal crystal under proper condition.Because colloidal crystal has many potential important application, as photonic crystal, prepare counter opal structure as template, and as the model of research material crystallisation process, colloidal crystal causes the interest that people are increasing.In addition, researchist is devoted to the colloid micro ball array that growth has complex construction always.
Self-assembly two-dimensional colloidal crystal is the colloidal crystal individual layer that self-assembly generation ordered arrangement occurs colloid micro-nano ball on planar substrate or water air interface.In recent years, two-dimensional colloidal crystal receives much concern in the widespread use aspect the preparation of micro nano structure because of it.Combine with micro-nano processing technology by colloidal crystal self-assembling technique, two-dimensional colloidal crystal has been used as mask or template is evaporated, deposition, etching and trace etc.These preparation method of nano material are defined as " nanometer ball etching ", are also referred to as " natural etching " or " colloid etching ".Nanosphere lithography technique is a kind of generally acknowledged simple, cheap, nanofabrication technique repeatably.At present laboratory all over the world all adopt prepare in this way light, magnetic, electrochemistry and catalytic property different functional nanostructure material.
Chinese patent application CN101787139A has proposed a kind of method of preparing two-dimensional colloidal crystal film on water air interface, colloid emulsion is dropped on sheet glass by the mode of manual dropping, then colloid micro ball slowly diffuses to the water surface, due to the effect of the capillary force existing between colloid micro ball and electrostatic repulsion, colloid micro ball forms two-dimensional colloidal crystal film in water air interface generation self-assembly, then by film transfer to substrate; This method is simple, fast, cost is low, but what adopt while dripping colloid emulsion in the method is the mode dripping manually, has some limitations.First, in dropping process, drip manually and exist discontinuous, inhomogeneously and unstable, and Different Individual operates the uncertain factors such as the otherness brought; Secondly, manually drip, for machinery drips, efficiency is not high, and output is lower; Finally, manually dropping need to expend a large amount of hand labor power and time cost.The application of the two-dimensional colloidal crystal that these problems have all limited water air interface self-assembled growth in actual nanometer science and technology industry.
Summary of the invention
In order to address the above problem, the invention provides a kind of two-dimensional colloidal crystal film and preparation method thereof, the concrete mode that adopts machinery to drip is alternative to be dripped manually.
The preparation method of a kind of two-dimensional colloidal crystal film provided by the present invention, comprises the steps:
(1) emulsion of colloid micro ball and ethanol are carried out to equal-volume and mix, after mixing, obtain mixed solution a;
(2) will be placed in culture dish through the sheet glass of wetting ability processing; Then arrive the upper surface of described sheet glass and do not have this upper surface to adding water to the water surface in described culture dish;
(3) with continuous transmission mechanism, described mixed solution a is evenly dripped to the upper surface at described sheet glass continuously; Diffuse to completely after water air interface until described colloid micro ball, in described water, add water phase surfactant mixture to obtain described two-dimensional colloidal crystal film.
In above-mentioned preparation method, in step (1), described colloid micro ball can be polymeric colloid microballoon or silicon dioxide colloid microballoon, and described polymeric colloid microballoon specifically can be polystyrene colloid microballoon or polymethyl acrylate colloid micro ball; The particle diameter of described colloid micro ball can be 130nm～2000nm, as 173nm or 600nm.
In above-mentioned preparation method, in step (1), utilize ultrasonic described emulsion and ethanol to be mixed; Described ultrasonic energy can be 120J～180J, and as 12J or 180J, the described ultrasonic time can be 10 minutes～and 20 minutes, as 10 minutes or 15 minutes.
In above-mentioned preparation method, in step (2), described wetting ability processing comprises the steps: described sheet glass to be placed in by concentrated sulfuric acid aqueous solution and aqueous hydrogen peroxide solution and to form mixed solution b, and after supersound process, water cleans, then drying, available nitrogen dries up; The energy of described supersound process can be 30J～60J, and as 30J or 45J, the time of described supersound process can be 5 minutes～and 10 minutes, as 5 minutes or 10 minutes.
In above-mentioned preparation method, the mass percentage concentration of described concentrated sulfuric acid aqueous solution can be 98%, and the mass percentage concentration of described aqueous hydrogen peroxide solution can be 30%～35%, as 30% or 35%; In described mixed solution b, described concentrated sulfuric acid aqueous solution and described aqueous hydrogen peroxide solution can be 7: 3 or 3: 1.
In above-mentioned preparation method, in step (3), described continuous transmission mechanism can be peristaltic pump, constant flow pump or syringe pump; The area of described sheet glass can be 0.25cm
2～2cm
2, as 0.25cm
2or 2cm
2; The volume of described mixed solution a can be 50 μ L～300 μ L, as 50 μ L or 200 μ L; The time of described diffusion can be 2 minutes～and 10 minutes, as 5 minutes or 10 minutes.
In above-mentioned preparation method, in step (3), in described water phase surfactant mixture, described tensio-active agent can be sodium lauryl sulphate and/or sodium laurylsulfonate; The mass percentage concentration of described water phase surfactant mixture can be 1%～3%, and as 1% or 2%, consumption can be 0.5mL～1mL, as 0.5mL or 1mL.
In above-mentioned preparation method, in step (2), before adding water in described culture dish, described method also can comprise to the step that adds substrate in described culture dish; In step (3), after obtaining described two-dimensional colloidal crystal film, described method also can comprise the steps: described substrate to move to the below of described substrate, then described substrate is mentioned, by described two-dimensional colloidal crystal film transfer on described substrate.
In above-mentioned preparation method, described substrate is cover glass, silicon chip, Sapphire Substrate, III-V family material substrate, polymeric substrates or metal base; The thickness of described substrate can be chosen according to actual needs.
The present invention also provides the two-dimensional colloidal crystal of being prepared by aforesaid method film.
In preparation method provided by the invention, machinery drip utilize continuous transmission mechanism, realize colloid emulsion slowly, evenly, continuously drip, thereby obtain the better two-dimensional colloidal crystal of crystal mass; On the other hand, substitute manually and drip by the mode of mechanize, can effectively save hand labor power, meanwhile, also can make efficiency greatly improve, increase of production; These provide a kind of effective approach for realizing in the future colloidal crystal in the industry application of field of nanometer technology.
Accompanying drawing explanation
Fig. 1 is the microphotograph of the two-dimensional colloidal crystal film prepared of embodiment 1 and comparative example 1; Wherein, the microphotograph of the two-dimensional colloidal crystal film that Fig. 1 (a) is prepared for comparative example 1, the microphotograph of the two-dimensional colloidal crystal film that Fig. 1 (b) is prepared for embodiment 1.
Fig. 2 is the SEM figure of the two-dimensional colloidal crystal film prepared of embodiment 1 and comparative example 1, wherein, the microphotograph of the two-dimensional colloidal crystal film that Fig. 2 (a) is prepared for comparative example 1, the microphotograph of the two-dimensional colloidal crystal film that Fig. 2 (b) is prepared for embodiment 1.
Embodiment
The experimental technique using in following embodiment if no special instructions, is ordinary method.
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
Embodiment 1, utilize continuous transmission mechanism to drip the polystyrene colloid microballoon that particle diameter is 600nm to prepare two-dimensional colloidal crystal film in water air interface self-assembly
(1) first prepare the polystyrene colloid microballoon that particle diameter is 600nm: under nitrogen protection, using 250ml deionized water as dispersion medium, 25ml vinylbenzene (letex polymerization monomer) and 0.125g Potassium Persulphate (letex polymerization initiator) are added in the 500ml there-necked flask that mechanical stirrer and reflux condensing tube are housed, in the water-bath of 60 ℃, carry out emulsifier-free emulsion polymerization, mechanical stirring speed is 300r/min, after reaction 24h, obtaining particle diameter is the milky emulsion of the polystyrene colloid microballoon of 600nm, the standard deviation of this polystyrene colloid microspherulite diameter is less than 3%,
Added to isopyknic ethanol above-mentioned preparation in the milky emulsion that gained particle diameter is 600nm polystyrene colloid microballoon, and supersound process 15min under the condition that is 120J at ultrasonic energy, evenly mixes, and obtains mixed solution a;
(2) sheet glass (1cm × 1cm) is placed in to the mixing solutions b that concentrated sulfuric acid aqueous solution (mass percentage concentration is 98%) and aqueous hydrogen peroxide solution (mass percentage concentration is 30%) are preparation in 3: 1 by volume, supersound process 5min under the condition that is 45J at ultrasonic energy, then use washed with de-ionized water, and dry up with nitrogen, above-mentioned sheet glass is placed in to culture dish, and puts into silicon chip substrate simultaneously; In culture dish, slowly add again deionized water, make the water surface just arrive the upper surface of sheet glass and not have upper surface;
(3) utilize constant flow pump that 200 μ L mixed solution a are dripped to the upper surface at above-mentioned sheet glass with the speed of 20 μ L/min, after 10min, treat that the polystyrene colloid microballoon in above-mentioned mixed solution a diffuses to water air interface completely, in water, add the sodium dodecyl sulfate aqueous solution that 0.5 milliliter of mass percentage concentration is 2%, obtain swimming in the two-dimensional colloidal crystal film on the water surface;
(4) silicon chip substrate in above-mentioned culture dish is moved on to floating two-dimensional colloidal crystal film below, slowly mention substrate, two-dimensional colloidal crystal film obtained above can be used as a global transfer on silicon chip substrate, at room temperature dry, after moisture evaporates completely, in silicon chip substrate, obtain two-dimensional colloidal crystal film.
The microphotograph of two-dimensional colloidal crystal film prepared by the present embodiment is as shown in Fig. 1 (b), and SEM schemes as shown in Fig. 2 (b).
Embodiment 2, utilize continuous transmission mechanism to drip the polystyrene colloid microballoon that particle diameter is 173nm to prepare two-dimensional colloidal crystal film in water air interface self-assembly
(1) first prepare the polystyrene colloid microballoon that particle diameter is 173nm: under nitrogen protection, using 250ml deionized water as dispersion medium, by 10ml vinylbenzene (letex polymerization monomer), (letex polymerization initiator and 0.1g sodium lauryl sulphate (emulsifying agent) add in the 500ml there-necked flask that mechanical stirrer and reflux condensing tube are housed 0.125g Potassium Persulphate, in the water-bath of 70 ℃, carry out emulsifier-free emulsion polymerization, mechanical stirring speed is 350r/min, after reaction 18h, obtaining particle diameter is the milky emulsion of the polystyrene colloid microballoon of 173nm, the standard deviation of this polystyrene colloid microspherulite diameter is less than 3%,
Added to isopyknic ethanol above-mentioned preparation in the milky emulsion that gained particle diameter is 173nm polystyrene colloid microballoon, and supersound process 10min under the condition that is 180J at ultrasonic energy, evenly mixes, and obtains mixed solution a;
(2) sheet glass (0.5cm × 0.5cm) is placed in to the mixing solutions b that concentrated sulfuric acid aqueous solution (mass percentage concentration is 98%) and aqueous hydrogen peroxide solution (mass percentage concentration is 35%) are preparation in 7: 3 by volume, supersound process 10min under the condition that is 30J at ultrasonic energy, then use washed with de-ionized water, and dry up with nitrogen, above-mentioned sheet glass is placed in to culture dish, and puts into silicon chip substrate simultaneously; In culture dish, slowly add again deionized water, make the water surface just arrive the upper surface of sheet glass and not have upper surface;
(3) utilize constant flow pump that 50 μ L mixed solution a are dripped to the upper surface at above-mentioned sheet glass with the speed of 10 μ L/min, after 5min, treat that the polystyrene colloid microballoon in above-mentioned mixed solution a diffuses to water air interface completely, in water, add the sodium dodecyl sulfate aqueous solution that 1 milliliter of mass percentage concentration is 1%, obtain swimming in the two-dimensional colloidal crystal film on the water surface;
(4) silicon chip substrate in above-mentioned culture dish is moved on to floating two-dimensional colloidal crystal film below, slowly mention substrate, two-dimensional colloidal crystal film obtained above can be used as a global transfer on Sapphire Substrate, at room temperature dry, after moisture evaporates completely, in silicon chip substrate, obtain two-dimensional colloidal crystal film.
Comparative example 1, utilization drip manually the polystyrene colloid microballoon that particle diameter is 600nm and prepare two-dimensional colloidal crystal film in water air interface self-assembly
(1) first prepare the polystyrene colloid microballoon that particle diameter is 600nm: under nitrogen protection, using 250ml deionized water as dispersion medium, 25ml vinylbenzene (letex polymerization monomer) and 0.125g Potassium Persulphate (letex polymerization initiator) are added in the 500ml there-necked flask that mechanical stirrer and reflux condensing tube are housed, in the water-bath of 60 ℃, carry out emulsifier-free emulsion polymerization, mechanical stirring speed is 300r/min, after reaction 24h, obtaining particle diameter is the milky emulsion of the polystyrene colloid microballoon of 600nm, the standard deviation of this polystyrene colloid microspherulite diameter is less than 3%,
Added to isopyknic ethanol above-mentioned preparation in the milky emulsion that gained particle diameter is 600nm polystyrene colloid microballoon, and supersound process 15min under the condition that is 120J at ultrasonic energy, evenly mixes, and obtains mixed solution a;
(2) sheet glass (1cm × 1cm) is placed in to the mixing solutions b that concentrated sulfuric acid aqueous solution (mass percentage concentration is 98%) and aqueous hydrogen peroxide solution (mass percentage concentration is 30%) are preparation in 3: 1 by volume, supersound process 5min under the condition that is 45J at ultrasonic energy, then use washed with de-ionized water, and dry up with nitrogen, above-mentioned sheet glass is placed in to culture dish, and puts into silicon chip substrate simultaneously; In culture dish, slowly add again deionized water, make the water surface just arrive the upper surface of sheet glass and not have upper surface;
(3) manually 200 μ L mixed solution a are dripped to the upper surface at above-mentioned sheet glass, after 20min, treat that the polystyrene colloid microballoon in above-mentioned mixed solution a diffuses to water air interface completely, in water, add the sodium dodecyl sulfate aqueous solution that 0.5 milliliter of mass percentage concentration is 2%, obtain swimming in the two-dimensional colloidal crystal film on the water surface;
(4) silicon chip substrate in above-mentioned culture dish is moved on to floating two-dimensional colloidal crystal film below, slowly mention substrate, two-dimensional colloidal crystal film obtained above can be used as a global transfer on silicon chip substrate, at room temperature dry, after moisture evaporates completely, in silicon chip substrate, obtain two-dimensional colloidal crystal film.
The microphotograph of two-dimensional colloidal crystal film prepared by this comparative example is as shown in Fig. 1 (a), and SEM schemes as shown in Fig. 2 (a).
From Fig. 1 and Fig. 2, by the comparison of embodiment 1 and comparative example 1, can find out, transmission mechanism drips the two-dimensional colloidal crystal film of preparation continuously, and owing to having avoided the disturbance of artificial dropping in self assembling process, its crystal mass is better than the artificial mode dripping.
Claims (3)
1. a preparation method for two-dimensional colloidal crystal film, preparation process is as follows:
(1) first prepare the polystyrene colloid microballoon that particle diameter is 600nm: under nitrogen protection, using 250ml deionized water as dispersion medium, 25ml styrene emulsion polymerization single polymerization monomer and 0.125g Potassium Persulphate are added in the 500ml there-necked flask that mechanical stirrer and reflux condensing tube are housed, in the water-bath of 60 ℃, carry out emulsifier-free emulsion polymerization, mechanical stirring speed is 300r/min, after reaction 24h, obtaining particle diameter is the milky emulsion of the polystyrene colloid microballoon of 600nm, and the standard deviation of this polystyrene colloid microspherulite diameter is less than 3%; Added to isopyknic ethanol above-mentioned preparation in the milky emulsion that gained particle diameter is 600nm polystyrene colloid microballoon, and supersound process 15min under the condition that is 120J at ultrasonic energy, evenly mixes, and obtains mixed solution a;
(2) sheet glass of one 1cm × 1cm being placed in to mass percentage concentration is that the aqueous hydrogen peroxide solution that 98% concentrated sulfuric acid aqueous solution and mass percentage concentration are 30% is the mixing solutions b of preparation in 3: 1 by volume, supersound process 5min under the condition that is 45J at ultrasonic energy, then use washed with de-ionized water, and dry up with nitrogen, above-mentioned sheet glass is placed in to culture dish, and puts into silicon chip substrate simultaneously; In culture dish, slowly add again deionized water, make the water surface just arrive the upper surface of sheet glass and not have upper surface;
(3) utilize constant flow pump that 200 μ L mixed solution a are dripped to the upper surface at above-mentioned sheet glass with the speed of 20 μ L/min, after 10min, treat that the polystyrene colloid microballoon in above-mentioned mixed solution a diffuses to water air interface completely, in water, add the sodium dodecyl sulfate aqueous solution that 0.5 milliliter of mass percentage concentration is 2%, obtain swimming in the two-dimensional colloidal crystal film on the water surface;
(4) silicon chip substrate in above-mentioned culture dish is moved on to floating two-dimensional colloidal crystal film below, slowly mention substrate, two-dimensional colloidal crystal film obtained above can be used as a global transfer on silicon chip substrate, at room temperature dry, after moisture evaporates completely, in silicon chip substrate, obtain two-dimensional colloidal crystal film.
2. a preparation method for two-dimensional colloidal crystal film, preparation process is as follows:
(1) first prepare the polystyrene colloid microballoon that particle diameter is 173nm: under nitrogen protection, using 250ml deionized water as dispersion medium, by 10ml styrene emulsion polymerization single polymerization monomer, 0.125g Potassium Persulphate and 0.1g sodium lauryl sulphate add in the 500ml there-necked flask that mechanical stirrer and reflux condensing tube are housed, in the water-bath of 70 ℃, carry out emulsifier-free emulsion polymerization, mechanical stirring speed is 350r/min, after reaction 18h, obtaining particle diameter is the milky emulsion of the polystyrene colloid microballoon of 173nm, the standard deviation of this polystyrene colloid microspherulite diameter is less than 3%, added to isopyknic ethanol above-mentioned preparation in the milky emulsion that gained particle diameter is 173nm polystyrene colloid microballoon, and supersound process 10min under the condition that is 180J at ultrasonic energy, evenly mixes, and obtains mixed solution a,
(2) sheet glass of one 0.5cm × 0.5cm being placed in to mass percentage concentration is that the aqueous hydrogen peroxide solution that 98% concentrated sulfuric acid aqueous solution and mass percentage concentration are 35% is the mixing solutions b of preparation in 7: 3 by volume, supersound process 10min under the condition that is 30J at ultrasonic energy, then use washed with de-ionized water, and dry up with nitrogen, above-mentioned sheet glass is placed in to culture dish, and puts into silicon chip substrate simultaneously; In culture dish, slowly add again deionized water, make the water surface just arrive the upper surface of sheet glass and not have upper surface;
(3) utilize constant flow pump that 50 μ L mixed solution a are dripped to the upper surface at above-mentioned sheet glass with the speed of 10 μ L/min, after 5min, treat that the polystyrene colloid microballoon in above-mentioned mixed solution a diffuses to water air interface completely, in water, add the sodium dodecyl sulfate aqueous solution that 1 milliliter of mass percentage concentration is 1%, obtain swimming in the two-dimensional colloidal crystal film on the water surface;
(4) silicon chip substrate in above-mentioned culture dish is moved on to floating two-dimensional colloidal crystal film below, slowly mention substrate, two-dimensional colloidal crystal film obtained above can be used as a global transfer on silicon chip substrate, at room temperature dry, after moisture evaporates completely, in silicon chip substrate, obtain two-dimensional colloidal crystal film.
3. the two-dimensional colloidal crystal film that in claim 1-2, described in any one prepared by method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210048371.8A CN102617874B (en) | 2012-02-28 | 2012-02-28 | Two-dimensional colloid crystal thin film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210048371.8A CN102617874B (en) | 2012-02-28 | 2012-02-28 | Two-dimensional colloid crystal thin film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102617874A CN102617874A (en) | 2012-08-01 |
| CN102617874B true CN102617874B (en) | 2014-06-04 |
Family
ID=46558112
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210048371.8A Expired - Fee Related CN102617874B (en) | 2012-02-28 | 2012-02-28 | Two-dimensional colloid crystal thin film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102617874B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966655B (en) * | 2014-05-07 | 2016-08-10 | 哈尔滨工业大学 | A kind of preparation method of opal structural 2 D photon crystal |
| CN103951839A (en) * | 2014-05-09 | 2014-07-30 | 中国科学院宁波材料技术与工程研究所 | Large-area self-assembly preparation method of nanosphere monolayer film and device thereof |
| CN104609362A (en) * | 2014-12-26 | 2015-05-13 | 上海维凯光电新材料有限公司 | Preparation method of polymer nanometer ring |
| CN106159092B (en) * | 2015-04-13 | 2018-06-29 | 中国科学院化学研究所 | The preparation method of organic semiconductor two-dimensional molecular crystalline material and application |
| CN105951166B (en) * | 2016-04-28 | 2019-03-29 | 河南大学 | The preparation facilities of two-dimensional colloidal crystal |
| CN106370534B (en) * | 2016-08-15 | 2019-03-22 | 常州大学 | A kind of novel colloidal crystal self-assembling method |
| CN107081976B (en) * | 2017-05-26 | 2019-04-30 | 东南大学 | A kind of transfer method of self-organized colloidal crystal |
| CN107604433B (en) * | 2017-07-28 | 2020-12-01 | 华南师范大学 | Method for producing a single-layer lattice |
| EP3778711A1 (en) * | 2019-08-13 | 2021-02-17 | Technische Universität Dresden | Method for the synthesis of a two-dimensional or quasi-two-dimensional polymer film, the two-dimensional or quasi-two-dimensional polymer film and the use |
| CN113877787B (en) * | 2021-08-18 | 2023-05-26 | 航天特种材料及工艺技术研究所 | Photonic crystal infrared stealth material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428493A (en) * | 2008-12-12 | 2009-05-13 | 清华大学 | Method for producing polymer colloid crystal film on hydrophobic substrate |
| CN101787139A (en) * | 2010-03-03 | 2010-07-28 | 清华大学 | Binary colloidal crystal film preparation method |
-
2012
- 2012-02-28 CN CN201210048371.8A patent/CN102617874B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428493A (en) * | 2008-12-12 | 2009-05-13 | 清华大学 | Method for producing polymer colloid crystal film on hydrophobic substrate |
| CN101787139A (en) * | 2010-03-03 | 2010-07-28 | 清华大学 | Binary colloidal crystal film preparation method |
Non-Patent Citations (4)
| Title |
|---|
| Flow-Controlled Vertical Deposition Method for the Fabrication of Photonic Crystals;Zuo chengzhou等;《Langmuir》;20031225;第20卷(第4期);1524-1526 * |
| Zuo chengzhou等.Flow-Controlled Vertical Deposition Method for the Fabrication of Photonic Crystals.《Langmuir》.2003,第20卷(第4期),1524-1526. |
| 二氧化硅胶体晶体制备方法进展;周倩等;《化工新型材料》;20030630;第31卷(第6期);16-18 * |
| 周倩等.二氧化硅胶体晶体制备方法进展.《化工新型材料》.2003,第31卷(第6期),16-18. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102617874A (en) | 2012-08-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102617874B (en) | Two-dimensional colloid crystal thin film and preparation method thereof | |
| CN101787139B (en) | Binary colloidal crystal film preparation method | |
| Rykaczewski et al. | Guided three-dimensional catalyst folding during metal-assisted chemical etching of silicon | |
| CN103738944B (en) | A kind of method preparing three-dimensional grapheme by nanoparticle doped | |
| TWI381994B (en) | Porous copper sulfide nano/micro hollow sphere and method for preparing the same | |
| CN101844231B (en) | Method for preparing noble metal self-organized colloidal crystal | |
| CN104445214A (en) | Mesoporous silica nano hollow sphere and preparation method thereof | |
| CN106395737B (en) | The preparation method for the micro/nano level array of structures that material surface form changes in gradient | |
| CN110128685A (en) | A kind of solution self-assembling method of large-area high-quality single layer PS microballoon film | |
| CN104860320A (en) | Method for preparing modified nanosilicon dioxide | |
| CN103611945A (en) | Method for preparing amphiphilic Janus gold nano particles in one step with liquid/liquid interface reaction | |
| CN106115613A (en) | A kind of large area monolayer compact nanometer microsphere thin film assemble method, device and the using method of device | |
| CN103933902B (en) | A kind of binary ordered colloidal crystal, metal nano array and preparation method thereof | |
| CN107376948A (en) | A kind of preparation method of two-dimentional selenizing molybdenum functional material water electrolysis hydrogen production catalyst | |
| CN109900642A (en) | A kind of submicron order miniature optical reactor and preparation method thereof | |
| CN103409802B (en) | A kind of preparation method of opal-structure polymer photonic crystal | |
| CN105601266B (en) | Gas-liquid interface method prepares silver orthophosphate sequential 2 D nano-mesh film and its method | |
| Gao et al. | Enhanced etching rate of black silicon by Cu/Ni Co-assisted chemical etching process | |
| CN104194018A (en) | Method for constructing functional ordered porous membrane by taking honeycomb-shaped porous membrane as template | |
| CN106370534A (en) | Novel self-assembling method for colloidal crystals | |
| CN101544394B (en) | Porous copper sulfide nano-micron hollow sphere and preparation method thereof | |
| CN109772183A (en) | A kind of anionic compound intercalation g-C3N4The preparation method and applications of composite membrane | |
| CN1239246C (en) | Method for preparing self-assembiling colloid crystal by vertical double base piece | |
| CN103272543B (en) | Method for preparing hollow silicon ball by self-templating method | |
| CN110548878B (en) | Preparation method of uniform and ordered platinum cubic or polyhedral nanoparticle array |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140604 Termination date: 20150228 |
|
| EXPY | Termination of patent right or utility model |