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.