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

Abstract

The invention provides a system for preparing colloidal crystals and a method for preparing colloidal crystals, belonging to the field of colloidal crystal preparation methods. The system includes: a microsphere injection system, an infrared wavelength heat source, a metal frame, a sample groove, a metal platform, a threaded shaft, a metal moving module, a polytetrafluoroethylene plate, and a drive motor. The drive motor is set at the left end of the metal frame, and the threaded shaft Connected with the drive motor, the metal moving module is set on the threaded shaft, the metal moving module is connected with the metal platform, the sample groove is set on the metal platform, and the polytetrafluoroethylene plate is fixed on the upper end of the metal frame and is in contact with the sample groove. The drive motor rotates and drives the threaded shaft to drive the metal moving module to move to the right. The present invention also provides a method for preparing colloidal crystals, which can assemble colloidal crystal templates with a single particle size and multiple particle sizes in a short period of time, and the thickness of the obtained colloidal crystals is controllable and large-area orderly. .

Description

A system for preparing colloidal crystals and a method for preparing colloidal crystals

technical field

The invention belongs to the field of preparation methods of colloidal crystals, and in particular relates to a system for preparing colloidal crystals and a preparation method of colloidal crystals.

Background technique

In the 21st century, manipulating photons in the field of photons has become the core research content. Because of its special periodic structure, colloidal crystals can be used as templates to prepare photonic crystals with inverse opal structures, which provides excellent means for the structural design and performance optimization of optical functional materials. .

The existing method commonly used to prepare colloidal crystals is the vertical deposition method, which was first proposed by Nagayama K in 1996. This method is to carry out self-assembly on the substrate, that is, simply dip the substrate vertically into a substrate containing monodisperse microspheres. In the colloidal solution, a meniscus is formed on the surface of the substrate and the solution. When the solvent evaporates, the meniscus drops, and the microspheres self-assemble into a periodic arrangement structure on the surface of the substrate under the action of capillary force, forming colloidal crystals (DIMITROV A S , NAGAYAMA K. Continuous Convective, Assembling of Fine Particles into Two-Dimensional Arrays on Solid Surfaces [J]. Langmuir, 1996, 12(5): 1303-1311.). The advantages of the vertical deposition method are: 1. The colloidal crystals in the prepared state have a high degree of order; 2. The number of colloidal crystal layers can be controlled by the concentration of the colloidal solution; and then the number of layers can be adjusted.

Although the quality of colloidal crystals grown by self-assembly using this method is good, there are still the following problems: 1. The self-assembly growth cycle is long; it takes 3-4 days; 2. The growth area is limited, and the diameter of the vessel containing the colloidal solution is determined 3. The self-assembly growth conditions are harsh, and the growth process is sensitive to environments such as temperature and humidity; 4. It is difficult to prepare composite colloidal crystals with multiple particle sizes.

Contents of the invention

The purpose of the present invention is to provide a system for preparing colloidal crystals in order to solve the problems of long cycle, limited growth area, difficult preparation of multi-particle size composite colloidal crystals and harsh growth conditions in the existing colloidal crystal preparation methods. Preparation method of colloidal crystals.

The present invention firstly provides a system for preparing colloidal crystals, which system includes: microsphere injection system, infrared wavelength heat source, metal frame, sample groove, metal platform, threaded shaft, metal moving module, polytetrafluoroethylene plate and Drive motor, the drive motor is set on the left end of the metal frame, one end of the threaded shaft is connected with the drive motor, the other end is connected with the metal frame, the metal moving module is set on the threaded shaft, the metal moving module is connected with the metal platform, and the sample groove is set in On the metal platform, the polytetrafluoroethylene plate is fixed on the upper end of the metal frame and is in contact with the sample groove, and the driving motor rotates to drive the threaded shaft to drive the metal moving module to move to the right.

The system of the present invention also includes four horizontal screws, the four horizontal screws are arranged on the metal platform, and the distance between the sample groove and the polytetrafluoroethylene plate is adjusted by adjusting the four horizontal screws.

The microsphere injection system of the present invention is used for injecting microsphere solution into the sample groove.

The infrared wavelength heat source of the present invention is an infrared evaporator.

The infrared wavelength heat source of the present invention is arranged at a distance of 10-15 cm from the sample groove.

The infrared wavelength heat source of the invention is used to irradiate the meniscus formed between the polytetrafluoroethylene plate and the sample groove.

The present invention also provides a method for preparing colloidal crystals, the method comprising:

Step 1: Prepare and clean the sample groove, fix the sample groove on the metal platform, and align the right side of the sample groove with the right side of the PTFE plate;

Step 2: Turn on the infrared wavelength heat source so that it can irradiate the meniscus formed between the PTFE plate and the sample groove;

Step 3: Inject the microsphere solution into the sample groove through the microsphere injection system, and the injection rate is 5-20 μl/min;

Step 4: Turn on the drive motor, the drive motor drives the threaded shaft to drive the metal moving module to move to the right, and inject the microsphere solution into the sample groove at the same time, when the left end of the sample groove slides away from the PTFE plate, turn off the infrared evaporator 1. A microsphere injection system and a driving motor, and the preparation of colloidal crystals is completed; the injection rate is 10-25 μl/min, and the moving speed of the metal moving module is 1-5 mm/min.

The microsphere solution of the present invention is polystyrene, SiO ₂ or PMMA microsphere solution.

The particle diameter of the polystyrene microspheres described in the present invention is 535.4nm.

In step 4 of the present invention, the injection rate is 20 μl/min, and the moving speed of the metal moving module is 2 mm/min.

How the invention works

The invention provides a system for preparing colloidal crystals and a method for preparing colloidal crystals. The method injects a monodisperse microsphere emulsion into a sample groove, and the microsphere emulsion is placed on a hydrophobic polytetrafluoroethylene plate and passed through a hydrophilic A meniscus is formed between the water-treated substrates, the meniscus is irradiated by a thermal light source, and the metal platform that fixes the sample groove is moved at the same time; when the evaporation speed of the water in the microsphere emulsion and the translation speed of the sample groove reach a dynamic balance , the microsphere emulsion in the meniscus undergoes a self-assembly process under the joint action of surface tension and capillary force to form a regularly arranged colloidal crystal film.

Beneficial effects of the present invention

The present invention firstly provides a system for preparing colloidal crystals, which can rapidly and effectively prepare colloidal crystals of different sizes, and the prepared colloidal crystals have smooth surfaces and high order.

The present invention also provides a method for preparing colloidal crystals. Compared with the prior art, the method of the present invention can assemble colloidal crystal templates with a single particle size and multiple particle sizes within a shorter time frame (15-30mins) , and the thickness of the obtained colloidal crystals is controllable, the area is controllable, the large area is orderly, and the requirements for the external environment are low.

Description of drawings

Fig. 1 is the overall schematic diagram of the system for preparing colloidal crystals of the present invention;

Fig. 2 is a partial enlarged view of the system for preparing colloidal crystals in the present invention;

3 is an appearance view of colloidal crystals prepared in Example 1 of the present invention;

Fig. 4 is the surface SEM picture of the colloidal crystal prepared in Example 1 of the present invention;

Fig. 5 is the cross-sectional SEM figure of the colloidal crystal prepared in Example 1 of the present invention;

Fig. 6 is the cross-sectional SEM figure of the colloidal crystal prepared in Example 2 of the present invention;

Fig. 7 is the cross-sectional SEM figure of the colloidal crystal prepared in Comparative Example 1;

8 is a cross-sectional SEM image of the colloidal crystal prepared in Comparative Example 2.

In the figure, 1. Microsphere injection system, 2. Infrared wavelength heat source, 3. Meniscus, 4. Metal frame, 5. Ordered colloidal crystal film, 6. Sample groove, 7. Metal platform, 8. Horizontal screw , 9, threaded shaft, 10, metal mobile module, 11, polytetrafluoroethylene plate, 12, drive motor.

detailed description

The present invention first provides a system for preparing colloidal crystals, as shown in Figure 1, the system includes: microsphere injection system 1, infrared wavelength heat source 2, metal frame 4, sample groove 6, metal platform 7, threaded shaft 9. Metal moving module 10, polytetrafluoroethylene plate 11 and drive motor 12, the drive motor 12 is arranged on the left end of the metal frame 4, one end of the threaded shaft 9 is connected with the drive motor 12, and the other end is connected with the metal frame 4 , the metal moving module 10 is set on the threaded shaft 9, the upper end of the metal moving module 10 is fixed on the metal platform 7 by screws, the metal platform 7 is used to fix the sample groove 6, the sample groove 6 is arranged on the metal platform 7, and the poly The tetrafluoroethylene plate 11 is fixed on the upper end of the metal frame 4 and is in contact with the sample groove 6, and the drive motor 12 rotates and drives the threaded shaft 9 to drive the metal moving module 10 to move to the right, because the metal moving module 10 and the metal platform 7 is fixedly connected, and when the metal moving module 10 moves to the right, it drives the sample groove 6 on the metal platform 7 to also move to the right.

Fig. 2 is the partially enlarged view of the system for preparing colloidal crystals of the present invention, the system of the present invention also includes four horizontal screws 8, and the four horizontal screws 8 are arranged on the metal platform 7, and the sample groove 6 After being fixed on the metal platform 7, the purpose of making the sample groove 6 level is achieved through four horizontal screws 8, and the contact between the notch of the sample groove 6 and the polytetrafluoroethylene plate 11 is adjusted by adjusting the four horizontal screws 8 , so that the meniscus 3 is formed between the polytetrafluoroethylene plate 11 and the sample groove 6 .

The microsphere injection system 1 is used to inject the microsphere solution into the sample groove 6 . Described infrared wavelength heat source 1 is used for irradiating the meniscus 3 that forms between polytetrafluoroethylene plate 11 and sample groove 6; Described infrared wavelength heat source is preferably arranged at the place apart from sample groove 10-15cm, like this It can make the infrared wavelength heat source evaporate the microsphere particle liquid layer in the sample groove to prevent the aggregation of the liquid surface. At the same time, this distance can effectively adjust the evaporation speed to suit the growth of the film. The infrared wavelength heat source is preferably an infrared evaporator .

The metal frame 4 of the present invention is preferably made of an aluminum alloy material. Since an infrared wavelength heat source is used in the present invention, a material with good heat dissipation performance is required. The metal moving module 10 is not particularly limited, and it is preferably transformed from a syringe pump of the model LSP01-1A.

The present invention also provides a method for preparing colloidal crystals, the method comprising:

Step 1: prepare and clean the sample groove 6, fix the sample groove 6 on the metal platform 7, and align the right side of the sample groove 6 with the right side of the polytetrafluoroethylene plate 11;

Step 2: Turn on the infrared wavelength heat source 2, and wait until the infrared wavelength heat source 2 reaches a stable state, preferably move the infrared wavelength heat source 2 to a distance of 10-15 cm from the sample groove, so that it can irradiate the polytetrafluoroethylene plate 11 and the sample groove 6 The meniscus 3 formed between; the infrared wavelength heat source is preferably an infrared evaporator;

Step 3: Inject the microsphere solution into the sample groove 6 through the microsphere injection system 1, so that the microsphere solution fills the gap between the sample groove 6 and the right side of the polytetrafluoroethylene plate 11; the injection rate is 5-20 μl /min; the injection volume of the described microsphere solution is preferably 20ul, and the concentration is preferably 10% (W/V); the preferred polystyrene, _SiO2 or PMMA microsphere solution of the described microsphere solution is more preferably polyphenylene Ethylene microsphere solution, the particle diameter of the polystyrene microsphere is preferably 535.4nm.

Step 4: Turn on the driving motor 12, and the driving motor 12 drives the threaded shaft 9 to drive the metal moving module 10 to move to the right, and inject the solution into the sample groove 6 at the same time, the concentration of the microsphere solution is 5% (W/V ), the meniscus 3 is formed between the sample groove 6 and the polytetrafluoroethylene plate 11; With the motor 12, the colloidal crystals are prepared; the injection rate is 10-25 μl/min, and the moving speed of the metal moving module 10 is 1-5 mm/min. Preferably, the injection rate in step 4 is 20 μl/min, and the moving speed of the metal moving module is 2 mm/min.

The present invention will strictly control the scope of the injection rate and the moving speed. If the injection rate and the moving speed exceed the above-mentioned parameter ranges, the evaporation rate of the colloidal emulsion at the meniscus and the amount of the injected emulsion cannot reach a balance, and the large particles precipitate too quickly, resulting in colloidal Membranes are difficult to form ordered structures.

The method for preparing and cleaning the sample groove 6 described in step one of the present invention is preferably as follows:

1. Cut several pieces of ITO glass with a geometric size of 40*30mm as the substrate, and ensure its conductivity;

2. After soaking the substrate in acetone for 24 hours, put it into a beaker filled with ethanol, place the beaker in an ultrasonic vibration cleaning machine, and clean it for 30 minutes; then put it into a beaker filled with deionized water, and place it in an ultrasonic vibration In the washing machine; repeat the above process 3 times;

3. Select the relatively clean substrate in 2, place it in the plasma etching machine, turn on the vacuum pump of the plasma etching machine, and wait until the plasma etching machine reaches a vacuum state, feed pure air into the etching machine, and adjust the voltage of the etching machine 10mins after the gas glow, turn off the etching machine and take out the substrate;

4. Take a 0.1mm thick polytetrafluoroethylene film with adhesive on one side, cut it into a 40mm long, 30mm wide and 1mm inwardly extended back pattern, stick this film to the substrate obtained in 3, and the sample groove is prepared.

Below in conjunction with specific embodiment, the present invention is described in further detail, the polystyrene microsphere used in the embodiment is the polystyrene microsphere produced by Wuhan Huake Weike Technology Co., Ltd.; the polystyrene microsphere injection system used is The syringe pump of LSP01-1A uses the 1000ul micro-sampler produced by Shanghai Boli Pigeon Industry and Trade Co., Ltd. as the injection component.

Example 1

Step 1: prepare and clean the sample groove 6, fix the sample groove 6 on the metal platform 7, and align the right side of the sample groove 6 with the right side of the polytetrafluoroethylene plate 11;

Step 2: Turn on the infrared evaporator 2, and when the infrared evaporator 2 reaches a stable state, move the infrared evaporator to a distance of 10-15 cm from the sample groove, so that it can irradiate between the PTFE plate 11 and the sample groove 6 The meniscus 3 formed;

Step 3: Inject 20 ul of polystyrene microsphere solution with a concentration of 10% into the sample groove 6 at an injection rate of 5 μl/min, so that the polystyrene microsphere solution fills the sample groove 6 and the polytetrafluoroethylene plate 11 side gaps;

Step 4: Turn on the driving motor 12, and the driving motor 12 drives the threaded shaft 9 to drive the metal moving module 10 to move to the right, and at the same time inject polystyrene solution into the sample groove 6, and the concentration of the polystyrene microsphere solution is 5% (W/V), the meniscus 3 is formed between the sample groove 6 and the polytetrafluoroethylene plate 11; when the left end of the sample groove 6 slides away from the polytetrafluoroethylene plate 11, close the infrared evaporator 2 and The ball injection system 1 and the driving motor 12 complete the preparation of colloidal crystals; the injection rate is 20 μl/min, and the moving speed of the metal moving module 10 is 2 mm/min. The particle size of the colloidal crystals obtained in Example 1 was 535 nm.

Fig. 3 is an appearance diagram of the colloidal crystal prepared in Example 1 of the present invention. It can be seen from the figure that the overall appearance of the colloidal crystal prepared by the rapid growth method in the present invention shows that the ordered structure appears.

Fig. 4 is a SEM image of the surface of the colloidal crystal prepared in Example 1 of the present invention. It can be seen from the figure that the polystyrene microspheres of the present invention are regularly arranged and have a high degree of order.

Figure 5 is a cross-sectional SEM image of the colloidal crystal prepared in Example 1 of the present invention. It can be seen from the figure that the polystyrene microspheres of the present invention are arranged regularly and orderly, and are arranged in a single layer of balls.

Example 2

The difference from Example 1 is that the injection rate is set to 15 μl/min, and the rest of the steps and conditions are the same as in Example 1.

The experimental results show that when the injection rate is 15 μl/min, the integrity of the ordered colloidal crystal sample formed by the present invention is better, and there are fewer cracks on the surface of the sample, which is less different from the colloidal crystal sample in Example 1. Figure 6 is the embodiment of the present invention. The SEM image of the surface of the colloidal crystal prepared in Example 2, as can be seen from the figure, the polystyrene microspheres of the present invention are regularly arranged and have a high degree of order.

Example 3

The difference from Example 1 is that the injection rate is set at 10 μl/min, the moving speed of the metal moving module 10 is 5 mm/min, and other steps and conditions are the same as in Example 1.

The experimental results show that when the injection rate is set to 10 μl/min and the moving speed of the metal moving module 10 is 5mm/min, the integrity of the ordered colloidal crystal sample formed by the present invention is better, there are fewer cracks on the sample surface, and the polystyrene microspheres The arrangement is regular and neat, with a high degree of order.

Example 4

The difference from Example 1 is that the injection rate is set at 25 μl/min, the moving speed of the metal moving module 10 is 1 mm/min, and other steps and conditions are the same as in Example 1.

The experimental results show that when the injection rate is set to 25 μl/min and the moving speed of the metal moving module 10 is 1mm/min, the integrity of the ordered colloidal crystal sample formed by the present invention is better, there are fewer cracks on the sample surface, and the polystyrene microspheres The arrangement is regular and neat, with a high degree of order.

Comparative example 1

The difference from Embodiment 1 is that the moving speed of the metal moving module 10 is 7 mm/min, and other steps and conditions are the same as Embodiment 1.

The experimental results show that when the moving rate is 7mm/min, the ordered colloidal crystal sample is formed. Compared with Example 1, the order degree of the sample is poor, and the surface of the colloidal crystal sample has obvious cracks. Fig. 7 is the SEM image of the surface of the colloidal crystal prepared in Comparative Example 1. It can be seen from the figure that when the moving speed is fast, the arrangement of the polystyrene microspheres is disordered.

Comparative example 2

The difference from Example 1 is that the injection rate is set to 30 μl/min, and the rest of the steps and conditions are the same as in Example 1.

The experimental results show that when the injection rate is set to 30 μl/min, the ordered colloidal crystal sample is formed. Compared with Example 1, the order of the sample is poor, and the surface of the colloidal crystal sample has obvious cracks. Figure 8 is the SEM image of the surface of the colloidal crystal prepared in Comparative Example 2. It can be seen from the figure that when the injection rate is fast, the arrangement of polystyrene microspheres is only partially ordered.

The descriptions of the above embodiments are only used to help understand the method and core idea of the present invention. It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, some improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.

The above description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

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.