CN104088008B - A kind of preparation method of the system and colloidal crystal for preparing colloidal crystal - Google Patents

A kind of preparation method of the system and colloidal crystal for preparing colloidal crystal Download PDF

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Publication number
CN104088008B
CN104088008B CN201410310067.5A CN201410310067A CN104088008B CN 104088008 B CN104088008 B CN 104088008B CN 201410310067 A CN201410310067 A CN 201410310067A CN 104088008 B CN104088008 B CN 104088008B
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colloidal crystal
metal
sample
sample groove
mobile module
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CN104088008A (en
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孟祥东
鲁铭
胡悦
李海波
于兆亮
曲晓慧
华杰
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Jilin Normal University
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Jilin Normal University
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Abstract

The present invention provides the preparation method of a kind of system and colloidal crystal for preparing colloidal crystal, belongs to colloidal crystal preparation method field.This system includes: microsphere injections system, infrared wavelength thermal source, metal framework, sample groove, metal platform, thread spindle, metal mobile module, polyfluortetraethylene plate and driving motor, motor is driven to be arranged on the left end of metal framework, thread spindle is connected with driving motor, metal mobile module is enclosed within thread spindle, metal mobile module is connected with metal platform, sample groove is arranged on metal platform, polyfluortetraethylene plate is fixed on the upper end of metal framework and contacts with sample groove, described driving motor rotates and drives thread spindle to drive metal mobile module to move to the right.The present invention also provides for the preparation method of a kind of colloidal crystal, and the method can assemble the colloidal crystal template that single particle size and many particle diameters are compound in the range of relatively short period of time, and the colloidal crystal thickness obtained is controlled, large-area ordered.

Description

A kind of preparation method of the system and colloidal crystal for preparing colloidal crystal
Technical field
The invention belongs to colloidal crystal preparation method field, be specifically related to a kind of for prepare colloidal crystal be System and the preparation method of colloidal crystal.
Background technology
21st century manipulates photon in photon field has become the research contents of core, and colloidal crystal is because of it Special periodic structure, can prepare photonic crystal with inverse opal structure as template, for optical function material Structure design and performance optimization provides superior measure.
The existing method preparing colloidal crystal conventional is vertical deposition method, the method in 1996 by Nagayama K proposes at first, and this method is to carry out self assembly on substrate, is dipped vertically into by substrate the most simply In colloid solution containing mono-dispersion microballoon, at substrate and solution surface formation meniscus, when the solvent evaporates, Meniscus declines, and microsphere, under capillary force effect, is periodic arrangement structure in substrate surface self assembly, is formed Colloidal crystal (DIMITROV A S, NAGAYAMA K.Continuous Convective, Assembling of Fine Particles into Two-DimensionalArrays on Solid Surfaces[J].Langmuir,1996, 12(5):1303-1311.).The advantage of vertical deposition method is: 1. the colloidal crystal degree of order of As-deposited state is higher;2. By the concentration of colloid solution, the controlled glue body crystal number of plies;And then the regulation and control number of plies.
Although the colloidal crystal quality utilizing the method self-assembled growth is preferable, but there is also problems with: 1. The self-assembled growth cycle is longer;Need 3-4 days time;2. growth area is limited, contains the vessel of colloid solution Diameter determines the width of growth substrate;3. self-assembled growth condition is harsh, and growth course is to temperature and humidity etc. Environment sensitive;4. more than particle diameter composite colloid crystal is difficult to prepare.
Summary of the invention
The invention aims to solve the preparation method cycle length of existing colloidal crystal, growth area is subject to The preparation of limit, many particle diameters composite colloid crystal difficulty and the problem of growth conditions harshness, and provide a kind of for preparing The system of colloidal crystal and the preparation method of colloidal crystal.
Present invention firstly provides a kind of system for preparing colloidal crystal, this system includes: microsphere injections system System, infrared wavelength thermal source, metal framework, sample groove, metal platform, thread spindle, metal mobile module, Polyfluortetraethylene plate and driving motor, drive motor to be arranged on the left end of metal framework, the one of thread spindle Holding and be connected with driving motor, the other end is connected with metal framework, and metal mobile module is enclosed within thread spindle, Metal mobile module is connected with metal platform, and sample groove is arranged on metal platform, and polyfluortetraethylene plate is solid Being scheduled on the upper end of metal framework and contact with sample groove, described driving motor rotates and drives thread spindle Metal mobile module is driven to move to the right.
System of the present invention also includes that four horizontal screws, four described horizontal screws are arranged on metal On platform, by the distance between four horizontal screw regulation sample grooves of regulation and polyfluortetraethylene plate.
Microsphere injections system of the present invention is for injectable microsphere solution in sample groove.
Infrared wavelength thermal source of the present invention is infrared ray vaporizer.
Infrared wavelength thermal source of the present invention is arranged at distance sample groove 10-15cm.
Infrared wavelength thermal source of the present invention is for irradiating formation between polyfluortetraethylene plate and sample groove Concave meniscus.
The present invention also provides for the preparation method of a kind of colloidal crystal, and the method includes:
Step one: prepare and clean sample groove, sample groove is fixed on metal platform, making sample recessed With polyfluortetraethylene plate right-justification on the right side of groove;
Step 2: open infrared wavelength thermal source so that it is can irradiate between polyfluortetraethylene plate and sample groove The concave meniscus formed;
Step 3: by microsphere injections system injectable microsphere solution in sample groove, described injection rate For 5-20 μ l/min;
Step 4: open and drive motor, drives motor-driven thread spindle to drive metal mobile module to the right Side shifting, simultaneously injectable microsphere solution in sample groove, when sample groove left end slips away polyfluortetraethylene plate Time, close infrared ray vaporizer, microsphere injections system and drive motor, prepared by colloidal crystal;Institute The injection rate stated is 10-25 μ l/min, and the translational speed of metal mobile module is 1-5mm/min.
Microspheres solution of the present invention is polystyrene, Si02Or PMMA microsphere solution.
The particle diameter of polystyrene microsphere of the present invention is 535.4nm.
In step 4 of the present invention, injection rate is 20 μ l/min, and the translational speed of metal mobile module is 2 mm/min。
The operation principle of the present invention
The present invention provides the preparation method of a kind of system and colloidal crystal for preparing colloidal crystal, the method By monodispersed microsphere emulsion being injected in sample groove, microsphere emulsion is at hydrophobic polyfluortetraethylene plate And between the substrate of hydrophilic treated, form meniscus, by thermal light source irradiation meniscus, simultaneously mobile solid The metal platform of random sample product groove;When in microsphere emulsion, evaporation rate and the sample groove point-to-point speed of moisture reach During to dynamic equilibrium, the microsphere emulsion in meniscus is carried out from group under surface tension and capillary force act on jointly Process of assembling, the colloidal crystal film of formation rule arrangement.
Beneficial effects of the present invention
Present invention firstly provides a kind of system for preparing colloidal crystal, this system can be made fast and effectively Standby various sizes of colloidal crystal, and the colloidal crystal surfacing prepared, the degree of order is high.
The present invention also provides for the preparation method of a kind of colloidal crystal, and prior art compares, the side of the present invention Method (15-30mins) can assemble the colloid that single particle size and many particle diameters are compound in the range of relatively short period of time Crystal template, and the colloidal crystal thickness obtained is controlled, area is controlled, large-area ordered, environment to external world Require low.
Accompanying drawing explanation
Fig. 1 is that the present invention is for preparing the overall schematic of the system of colloidal crystal;
Fig. 2 is that the present invention is for preparing the partial enlarged drawing of the system of colloidal crystal;
Fig. 3 is the outside drawing of the colloidal crystal of the embodiment of the present invention 1 preparation;
Fig. 4 is the surface SEM figure of the colloidal crystal of the embodiment of the present invention 1 preparation;
Fig. 5 is the cross section SEM figure of the colloidal crystal of the embodiment of the present invention 1 preparation;
Fig. 6 is the cross section SEM figure of the colloidal crystal of the embodiment of the present invention 2 preparation;
Fig. 7 is the cross section SEM figure of the colloidal crystal of comparative example 1 preparation;
Fig. 8 is the cross section SEM figure of the colloidal crystal of comparative example 2 preparation.
In figure, 1, microsphere injections system, 2, infrared wavelength thermal source, 3, meniscus, 4, metal framework, 5, In order colloidal crystal film, 6, sample groove, 7, metal platform, 8, horizontal screw, 9, thread spindle, 10, Metal mobile module, 11, polyfluortetraethylene plate, 12, drive motor.
Detailed description of the invention
Present invention firstly provides a kind of system for preparing colloidal crystal, as it is shown in figure 1, this system includes: Microsphere injections system 1, infrared wavelength thermal source 2, metal framework 4, sample groove 6, metal platform 7, spiral shell Stricture of vagina axle 9, metal mobile module 10, polyfluortetraethylene plate 11 and driving motor 12, described driving is electronic Machine 12 is arranged on the left end of metal framework 4, and one end of thread spindle 9 is connected with driving motor 12, another End is connected with metal framework 4, and metal mobile module 10 is enclosed within thread spindle 9, metal mobile module 10 Upper end is screwed on metal platform 7, and metal platform 7 is used for fixing sample groove 6, sample groove 6 are arranged on metal platform 7, and polyfluortetraethylene plate 11 is fixed on the upper end of metal framework 4 recessed with sample Groove 6 contacts, described driving motor 12 rotate drive thread spindle 9 drive metal mobile module 10 to Right side is mobile, is connected, when metal mobile module 10 owing to metal mobile module 10 is fixing with metal platform 7 When moving to the right, the sample groove 6 on metal platform 7 is driven to move the most to the right.
Fig. 2 be the present invention for preparing the partial enlarged drawing of the system of colloidal crystal, system of the present invention Also include that four horizontal screws 8, four described horizontal screws 8 are arranged on metal platform 7, sample groove After 6 are fixed on metal platform 7, reach to make the purpose of sample groove 6 level by four horizontal screws 8, and And regulate connect between the notch of sample groove 6 and polyfluortetraethylene plate 11 by four horizontal screws 8 of regulation Touch, make the meniscus 3 formed between polyfluortetraethylene plate 11 and sample groove 6.
Described microsphere injections system 1 is for injectable microsphere solution in sample groove 6.Described infrared waves Long thermal source 1 is for irradiating the meniscus 3 formed between polyfluortetraethylene plate 11 and sample groove 6;Described Infrared wavelength thermal source is preferably provided at distance sample groove 10-15cm, thus can make infrared wavelength thermal source The microsphere particles liquid level that evaporation is limited in sample groove, to prevent the gathering of liquid surface, meanwhile, this Individual distance can effectively regulate evaporation rate, and with the growth of applicable thin film, infrared wavelength thermal source is the most infrared Line vaporizer.
Metal framework 4 of the present invention preferably employs aluminum alloy materials, owing to using infrared waves in the present invention Long thermal source, therefore needs the material good with heat dispersion.Described metal mobile module 10 is not particularly limited, The syringe pump transformation preferably using model to be LSP01-1A forms.
The present invention also provides for the preparation method of a kind of colloidal crystal, and the method includes:
Step one: prepare and clean sample groove 6, sample groove 6 being fixed on metal platform 7, makes sample With polyfluortetraethylene plate 11 right-justification on the right side of product groove 6;
Step 2: open infrared wavelength thermal source 2, treat that infrared wavelength thermal source 2 reaches steady statue, by infrared waves Long thermal source 2 preferably moves to distance sample groove 10-15cm and locates so that it is can irradiate polyfluortetraethylene plate 11 and The meniscus 3 formed between sample groove 6;Infrared wavelength thermal source is preferably infrared ray vaporizer;
Step 3: by microsphere injections system 1 injectable microsphere solution in sample groove 6, make microspheres solution Space on the right side of filling sample groove 6 and polyfluortetraethylene plate 11;Described injection rate is 5-20 μ l/min; Described microspheres solution injection volume is preferably 20ul, and concentration is preferably 10% (W/V);Described microsphere is molten The preferred polystyrene of liquid, Si02Or PMMA microsphere solution, more preferably polystyrene microsphere solution, described The particle diameter of polystyrene microsphere be preferably 535.4nm.
Step 4: open and drive motor 12, drives motor 12 to drive thread spindle 9 to drive metal to move mould Block 10 moves to the right, simultaneously injection solution in sample groove 6, and the concentration of described microspheres solution is 5% (W/V), meniscus 3 is formed between sample groove 6 and polyfluortetraethylene plate 11;When sample groove 6 left end Slip away polyfluortetraethylene plate 11 time, close infrared ray vaporizer 2, microsphere injections system 1 and drive motor 12, prepared by colloidal crystal;Described injection rate is 10-25 μ l/min, the shifting of metal mobile module 10 Dynamic speed is 1-5mm/min.Preferably, in described step 4, injection rate is 20 μ l/min, metal The translational speed of mobile module is 2mm/min.
The present invention strictly to control the scope of injection rate and translational speed, if injection rate and rate travel Beyond above-mentioned parameter scope, the evaporation rate of the colloid emulsion at meniscus and injection emulsion amount can not reach flat Weighing apparatus, big particle precipitation is too fast, causes colloidal film to be hardly formed ordered structure.
Preparation and the method for cleaning sample groove 6 described in step one of the present invention are preferably as follows:
1, cutting physical dimension be some pieces of the ito glass of 40*30mm as substrate, and guarantee that it conducts electricity Property;
2, by substrate with after acetone soak 24 hours, put in the beaker containing ethanol, beaker is placed in ultrasonic In oscillation cleaning machine, clean 30mins;It is then placed in, equipped with in the beaker of deionized water, being placed on ultrasonic In oscillation cleaning machine;Repeat said process 3 times;
3, choose substrate the cleanest in 2, be placed in plasma etching machine, open plasma etching machine true Empty pump, reaches vacuum state in treating plasma etching machine, is passed through pure air, regulation etching in etching machine Dynamo-electric pressure, 10mins after gas aura, closes etching machine and takes out substrate;
4, take one side thick for 0.1mm and have sticking polytetrafluoroethylene film, cut growth 40mm, wide 30mm Inwardly the Back Word figure of extension 1mm, adheres to this thin film on 3 substrates obtained, prepared by sample groove.
Below in conjunction with specific embodiment, the present invention will be further described in detail, the polyphenyl used in embodiment Ethylene microsphere is the polystyrene microsphere that Wuhan China Tech micro-section science and technology limited Company produces;The polyphenyl used Ethylene microsphere injections system is the syringe pump of LSP01-1A, uses Shanghai Bo Li Columba livia Trade Co., Ltd. to produce 1000ul microsyringe is as injecting assembly.
Embodiment 1
Step one: prepare and clean sample groove 6, sample groove 6 being fixed on metal platform 7, makes sample With polyfluortetraethylene plate 11 right-justification on the right side of product groove 6;
Step 2: open infrared ray vaporizer 2, treat that infrared ray vaporizer 2 reaches steady statue, by infrared steaming Send out device and move at distance sample groove 10-15cm so that it is polyfluortetraethylene plate 11 and sample groove can be irradiated The meniscus 3 formed between 6;
Step 3: with injection rate be 5 μ l/min inject in sample groove 6 20ul concentration be 10% poly- Phenylethylene micro ball solution, makes on the right side of polystyrene microsphere solution filling sample groove 6 and polyfluortetraethylene plate 11 Space;
Step 4: open and drive motor 12, drives motor 12 to drive thread spindle 9 to drive metal to move mould Block 10 moves to the right, injects polystyrene solution in sample groove 6 simultaneously, and described polystyrene is micro- The concentration of ball solution is 5% (W/V), forms meniscus 3 between sample groove 6 and polyfluortetraethylene plate 11; When sample groove 6 left end slips away polyfluortetraethylene plate 11, close infrared ray vaporizer 2, microsphere injections system System 1 and driving motor 12, prepared by colloidal crystal;Described injection rate is 20 μ l/min, metal The translational speed of mobile module 10 is 2mm/min.The particle diameter of the colloidal crystal that embodiment 1 obtains is 535nm.
Fig. 3 is the outside drawing of the colloidal crystal of the embodiment of the present invention 1 preparation, it can be seen that this Colloidal crystal entirety pattern prepared by bright employing fast-growth method, it is seen that degree of order structure occurs.
Fig. 4 is the surface SEM figure of the colloidal crystal of the embodiment of the present invention 1 preparation, it can be seen that The polystyrene microsphere queueing discipline of the present invention is neat, and the degree of order is high.
Fig. 5 is the cross section SEM figure of the colloidal crystal of the embodiment of the present invention 1 preparation, it can be seen that The polystyrene microsphere queueing discipline of the present invention is neat, and the degree of order is high;And become the arrangement of monolayer ball.
Embodiment 2
With embodiment 1 except that, injection rate is set to 15 μ l/min, remaining step and condition with real Execute example 1.
Test result indicate that, when injection rate is at 15 μ l/min, it is complete that the present invention forms orderly colloidal crystal sample Whole degree is preferable, and sample surfaces occurs that slight crack is less, less with embodiment 1 colloidal crystal sample difference, Fig. 6 Surface SEM for the colloidal crystal of the embodiment of the present invention 2 preparation schemes, it can be seen that the present invention Polystyrene microsphere queueing discipline is neat, and the degree of order is high.
Embodiment 3
With embodiment 1 except that, injection rate is set to 10 μ l/min, the shifting of metal mobile module 10 Dynamic speed is 5mm/min, and remaining step and condition are with embodiment 1.
Test result indicate that, when injection rate is set to 10 μ l/min, the translational speed of metal mobile module 10 For 5mm/min, it is preferable that the present invention forms orderly colloidal crystal sample integrity degree, and sample surfaces occurs that slight crack is less, Polystyrene microsphere queueing discipline is neat, and the degree of order is high.
Embodiment 4
With embodiment 1 except that, injection rate is set to 25 μ l/min, the shifting of metal mobile module 10 Dynamic speed is 1mm/min, and remaining step and condition are with embodiment 1.
Test result indicate that, when injection rate is set to 25 μ l/min, the translational speed of metal mobile module 10 For 1mm/min, it is preferable that the present invention forms orderly colloidal crystal sample integrity degree, and sample surfaces occurs that slight crack is less, Polystyrene microsphere queueing discipline is neat, and the degree of order is high.
Comparative example 1
With embodiment 1 except that, the translational speed of metal mobile module 10 is 7mm/min, remaining step Rapid and condition is with embodiment 1.
Test result indicate that, rate travel, at 7mm/min, forms orderly colloidal crystal sample and in contrast to embodiment 1, the sample degree of order is poor, and the obvious slight crack of colloidal crystal sample surfaces.Fig. 7 is the glue of comparative example 1 preparation The surface SEM figure of body crystal, it can be seen that when translational speed is very fast, polystyrene microsphere is arranged Arrange unordered.
Comparative example 2
With embodiment 1 except that, injection rate is set to 30 μ l/min, remaining step and condition with real Execute example 1.
Test result indicate that, injection rate is set to 30 μ l/min, forms orderly colloidal crystal sample and in contrast to reality Executing example 1, the sample degree of order is poor, and the obvious slight crack of colloidal crystal sample surfaces.Fig. 8 is prepared by comparative example 2 Colloidal crystal surface SEM figure, it can be seen that when injection rate is very fast, polystyrene is micro- Ball arrangement only partial order.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.Should refer to Go out, for those skilled in the art, under the premise without departing from the principles of the invention, also The present invention can be carried out some improvement and modification, these improve and modify and also fall into the claims in the present invention In protection domain.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses this Invention.Multiple amendment to these embodiments will be apparent from for those skilled in the art, Generic principles defined herein can without departing from the spirit or scope of the present invention, at other Embodiment realizes.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is intended to Meet the widest scope consistent with principles disclosed herein and features of novelty.

Claims (10)

1. the system being used for preparing colloidal crystal, it is characterised in that this system includes: microsphere injections system System (1), infrared wavelength thermal source (2), metal framework (4), sample groove (6), metal platform (7), Thread spindle (9), metal mobile module (10), polyfluortetraethylene plate (11) and driving motor (12), Motor (12) is driven to be arranged on the left end of metal framework (4), one end of thread spindle (9) and driving electricity Motivation (12) connects, and the other end is connected with metal framework (4), and metal mobile module (10) is enclosed within screw thread On axle (9), metal mobile module (10) is connected with metal platform (7), and sample groove (6) is arranged on On metal platform (7), polyfluortetraethylene plate (11) is fixed on upper end and the sample of metal framework (4) Groove (6) contacts, and described driving motor (12) rotates and drives thread spindle (9) to drive metal to move Dynamic model block (10) moves to the right.
A kind of system for preparing colloidal crystal the most according to claim 1, it is characterised in that institute The system stated also includes that four horizontal screws (8), four described horizontal screws (8) are arranged on metal and put down On platform (7), by four horizontal screws (8) regulation sample groove (6) of regulation and polyfluortetraethylene plate (11) Between distance.
A kind of system for preparing colloidal crystal the most according to claim 1, it is characterised in that institute The microsphere injections system (1) stated is for injectable microsphere solution in sample groove (6).
A kind of system for preparing colloidal crystal the most according to claim 1, it is characterised in that institute The infrared wavelength thermal source (2) stated is infrared ray vaporizer.
A kind of system for preparing colloidal crystal the most according to claim 1, it is characterised in that institute The infrared wavelength thermal source (2) stated is arranged at distance sample groove (6) 10-15cm.
6. according to a kind of system for preparing colloidal crystal described in claim 1,4 or 5 any one, It is characterized in that, it is recessed with sample that described infrared wavelength thermal source (2) is used for irradiating polyfluortetraethylene plate (11) The concave meniscus formed between groove (6).
7. the preparation method of a colloidal crystal, it is characterised in that the method includes:
Step one: prepare and clean sample groove (6), sample groove (6) is fixed on metal platform (7) On, make sample groove (6) right side and polyfluortetraethylene plate (11) right-justification;
Step 2: open infrared wavelength thermal source (2) so that it is polyfluortetraethylene plate (11) and sample can be irradiated The concave meniscus formed between product groove (6);
Step 3: by microsphere injections system (1) injectable microsphere solution in sample groove (6), described Injection rate be 5-20 μ l/min;
Step 4: open and drive motor (12), drives motor (12) to drive thread spindle (9) to drive Metal mobile module (10) moves to the right, and injectable microsphere solution in sample groove (6), works as sample simultaneously Product groove (6) left end slip away polyfluortetraethylene plate (11) time, close infrared wavelength thermal source (2), microsphere Injecting systems (1) and driving motor (12), prepared by colloidal crystal;Described injection rate is 10-25 μ l/min, the translational speed of metal mobile module is 1-5mm/min.
The preparation method of a kind of colloidal crystal the most according to claim 7, it is characterised in that described Microspheres solution is polystyrene, Si02Or PMMA microsphere solution.
The preparation method of a kind of colloidal crystal the most according to claim 8, it is characterised in that described The particle diameter of polystyrene microsphere is 535.4nm.
The preparation method of a kind of colloidal crystal the most according to claim 7, it is characterised in that described Step 4 in injection rate be 20 μ l/min, the translational speed of metal mobile module is 2mm/min.
CN201410310067.5A 2014-06-30 2014-06-30 A kind of preparation method of the system and colloidal crystal for preparing colloidal crystal Expired - Fee Related CN104088008B (en)

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