CN112209333B - Preparation method of surface double-stage microstructure by using liquid drop forming method based on temperature regulation and control - Google Patents
Preparation method of surface double-stage microstructure by using liquid drop forming method based on temperature regulation and control Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00555—Achieving a desired geometry, i.e. controlling etch rates, anisotropy or selectivity
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- Microelectronics & Electronic Packaging (AREA)
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- Shaping Of Tube Ends By Bending Or Straightening (AREA)
Abstract
The invention discloses a preparation method of a two-stage microstructure on the surface of a liquid drop forming method based on temperature regulation, which comprises the steps of firstly obtaining a first polymer liquid drop array on the surface of a first substrate through a temperature gradient enhanced transfer printing method, then obtaining a second liquid drop array through condensation self-assembly on the curved surface of the first polymer liquid drop through an active refrigeration vapor condensation method, then introducing a third polymer to realize the second liquid drop morphology regulation, thus obtaining a two-stage liquid drop array, finally solidifying the first polymer liquid drop array to obtain the first polymer microstructure array, and simultaneously obtaining a curved surface second microstructure array corresponding to the second liquid drop array on the surface of the first polymer microstructure array due to the imprinting effect of the second liquid drop array, thus obtaining the two-stage microstructure array on the surface. According to the invention, the idea of additive manufacturing and subtractive manufacturing is adopted, the two-stage microstructure array is prepared based on a temperature regulation and control two-stage droplet forming method, and the flexible regulation and control of the morphology parameters of the two-stage microstructure is realized through the regulation of the technological parameters of the two-stage droplet forming.
Description
Technical Field
The invention relates to a preparation technology of an organic colloid surface microstructure, in particular to a preparation method of a two-stage microstructure of a liquid drop forming method surface based on temperature regulation.
Background
The surface microstructure film is widely applied to various fields such as optics, biomedicine, functional materials and the like. The current general method for preparing microstructures on the surface of colloid is an imprinting method, and the technological process of the imprinting method comprises the processes of mould manufacturing and compression molding. The manufacturing of the mould can realize the preparation of the microstructure on the mould, and the compression molding process is to transfer the mould pattern to the surface of the polymer colloid, but the mould is complex to process, has higher cost and depends on expensive precise equipment. In addition, for preparing the two-stage microstructure by adopting the imprinting method, the two-stage microstructure needs to be prepared on a primary microstructure curved surface die with a micrometer scale, and the processing difficulty is very high. The filling ratio and aspect ratio parameters of the microstructure are key parameters affecting the performance of the microstructure. For preparing the microstructure by adopting a mould imprinting method, the adjustment and control of the filling ratio and the aspect ratio parameters of the microstructure are mainly realized by adjusting the manufacturing process parameters of the mould.
The technology for preparing the microstructure by the liquid drop imprinting method has been widely studied in recent years because a mould manufacturing link is omitted. The method is characterized in that the prepared droplet array is stamped on the surface of the polymer to obtain a microstructure array, and the microstructure array mainly comprises a droplet printing method, a respiration pattern method and an active refrigerating droplet coagulation method according to different preparation modes of the droplet array. 1. The liquid drop printing method is to prepare a liquid drop template through direct writing or laser pulse induction, but the liquid drops are formed one by one, the production efficiency is low, high-precision and high-cost liquid drop equipment is needed, the method realizes the filling ratio adjustment by controlling the distribution of printing liquid drops, and the depth-to-width ratio adjustment is realized by changing the interaction between the liquid drops and the base material by adjusting the pre-curing degree of the base material; 2. the respiratory pattern method is to dissolve solid polymer in volatile solvent, the solvent volatilizes to take away heat so as to reduce the temperature of the solution surface, and water vapor in the air condenses on the solution surface, however, the three-phase morphology of the air-water drop-polymer is difficult to regulate and control due to the tension effect of the water drop surface, so that the aspect ratio of the microstructure cannot be effectively controlled; 3. the applicant is inspired by a respiration pattern method and proposes an active refrigeration water drop condensation method, wherein the active refrigeration water drop condensation method is to obtain a water drop array through condensation and self-assembly of actively refrigerated water drops, and although the pre-curing degree of an ultraviolet curing polymer is controlled to regulate water drop-ultraviolet curing polymer interaction, the pre-estimation degree of the ultraviolet curing polymer is not linearly controllable, so that the depth-to-width ratio regulation effect is limited. It should be noted that the droplet imprinting method described above can only produce primary microstructure arrays.
Drop forming has been extensively studied as an additive manufacturing approach. The method comprises the steps of firstly preparing a liquid drop array, and then solidifying the liquid drop array to obtain the microstructure array. Depending on the manner in which the droplet array is prepared, droplet printing and solvent exchange are mainly involved. 1. The droplet printing method prepares the droplet array through direct writing type and laser pulse induction type, but the method for preparing the droplets one by one has the defects of low efficiency and high cost, theoretically, the two-stage droplet array is printed on the first polymer droplet, the two-stage microstructure is stamped on the first polymer droplet by using the two-stage droplet as a mould, so that the preparation of the two-stage microstructure can be realized, but the preparation efficiency is very low, and therefore, the preparation method of the two-stage microstructure has theoretical possibility only under the condition of not considering the cost and the production efficiency. For the adjustment of the depth-to-width ratio, the spreading of liquid drops can be restrained by the high-temperature rapid curing of the thermosetting glue so as to increase the depth-to-width ratio; the adjustment of the filling ratio is mainly realized by changing the distance between the liquid drops, but the problem of liquid drop convergence exists in the liquid drop distribution with high filling ratio, and the scholars propose to solve the problem by adopting a pre-cured polymer with high viscosity. 2. The solvent exchange method utilizes the Ouzo effect to prepare droplet arrays. In this method, a solvent of high solubility (e.g., ethanol) is replaced with a solvent of low solubility (e.g., water) to precipitate and precipitate the supersaturated droplet material and thereby obtain an array of droplets. However, the method cannot obtain an orderly controllable liquid drop array, and further cannot realize the preparation of a double-stage microstructure.
Disclosure of Invention
Aiming at the problem that the conventional surface microstructure preparation technology cannot realize the preparation of a two-stage microstructure at present, the invention aims to provide a droplet forming method surface two-stage microstructure preparation method based on temperature regulation and control, and the flexible regulation and control of the morphology parameters of the two-stage microstructure can be realized.
The purpose of the invention is realized in the following way:
a preparation method of a two-stage microstructure on the surface of a liquid drop forming method based on temperature regulation and control is characterized by comprising the following steps: the method comprises the following steps:
A. preparing a first substrate, and placing the first substrate on a temperature control platform;
B. controlling the temperature of the first substrate through a temperature control platform, and transferring the first polymer in the container to the surface of the first substrate by adopting a transfer mold to obtain a first polymer droplet array;
C. preparing a vapor atmosphere control system, realizing temperature regulation of a first polymer droplet array through refrigeration action of a temperature control platform, enabling the temperature of the first polymer droplet to be lower than the ambient temperature, enabling vapor to be coagulated and nucleated on a curved surface of the first polymer droplet, enabling the vapor to self-assemble into a second droplet array on the curved surface of the first polymer droplet after coagulation for a certain time, and enabling the second droplet array to enter the interior of the first polymer droplet array due to surface tension action, wherein: the second droplet is immiscible with the first polymer;
D. preparing a second substrate, placing a third polymer on a surface of the second substrate, wherein: the third polymer is immiscible with the first polymer and the second droplet;
E. overlaying a third polymer on a second substrate on the first polymer droplet array having the second droplet array to form a stable first polymer-second droplet-third polymer three-phase interface;
F. solidifying the first polymer droplet array until the first polymer droplet array is completely solidified to obtain a first polymer microstructure array, and obtaining a curved surface second microstructure array corresponding to the second droplet array on the surface of the first polymer microstructure array due to the imprinting effect of the second droplet array;
G. and stripping the second substrate, removing the second liquid drop array and the third polymer on the surface of the first polymer microstructure array, and finally obtaining the two-stage microstructure array.
Further, the first substrate material in the step a is one of glass, silica gel, polystyrene (PS), polycarbonate (PC) or polymethyl methacrylate (PMMA) high light transmission material.
Further, the temperature setting value of the temperature control platform in the step B is T1, where T1 is smaller than the ambient temperature Ta, so that the temperature of the first substrate is lower than the temperature of the transfer mold.
Further, the transfer mold in the step B is a hard mold or a soft mold, the material of the hard mold is a silicon material or a silicon dioxide material, and the material of the soft mold is a Polydimethylsiloxane (PDMS) material.
Further, the first polymer in the step B is an ultraviolet curing polymer, and the corresponding curing mode in the step F is to realize complete curing of the first polymer by irradiation of an ultraviolet lamp, wherein the curing time is 1-30 min; or the first polymer in the step B is a heat-curing polymer, and the corresponding curing mode in the step F is to realize complete curing of the first polymer by a heating curing method, wherein the curing time is 10-300 min.
Further, the transferring of the first polymer droplet array on the surface of the first substrate in the step B is performed by dipping the first polymer from the container through a transfer mold on a three-dimensional moving platform in a three-dimensional position control system, and transferring the first polymer onto the surface of the first substrate, so as to obtain the first polymer droplet array, where the diameter of the obtained first polymer droplet is 5-1000 μm.
Further, the vapor atmosphere control system in the step C can realize vapor atmosphere and ensure control of the concentration of the vapor atmosphere, and the vapor atmosphere is one of water, methanol, ethanol, glycol or glycerol; or the steam atmosphere is one of water, methanol, ethanol, glycol or glycerol or a mixture of two or more substances, and the concentration control range of the specific steam atmosphere is 10% -90%.
Further, the refrigerating temperature T2 of the temperature control platform in the step C is 5-40 ℃ smaller than the ambient temperature Ta, the condensation time of the second liquid drops is 2-30 min, and the diameter of the obtained second liquid drops is 0.5-100 mu m.
Further, the second substrate material in the step D is one of glass, polymethyl methacrylate (PMMA) or acrylonitrile-butadiene-styrene (ABS).
Further, the third polymer in the step D is one of a conventional liquid polymer, an ultraviolet cured polymer or a heat cured polymer, and the third polymer does not have the same curing form as the first polymer, that is, the third polymer cannot be cured by ultraviolet irradiation when the first polymer is an ultraviolet cured material, or the third polymer cannot be cured by heating when the first polymer is a heat cured material, and the third polymer is placed on the second substrate by means of spot coating or spin coating, and the thickness of the third polymer is 6-1000 μm.
The invention adopts a temperature-controlled drop forming method to prepare the two-stage microstructure array. The size parameter of the two-stage microstructure is the key for influencing the performance of the two-stage microstructure, so the technical scheme provided by the invention realizes the effective regulation and control of the size parameter of the two-stage liquid drop array by adjusting the corresponding technological parameter:
for the first polymer drop array preparation, a transfer mold is first prepared. For transfer mold preparation, photolithography is mainly used in combination with dry etching or wet etching. Wherein the lithographic mask pattern determines a structural parameter of the transfer mold to adjust a distribution of the transfer first polymer drop array. In the transfer printing process of the first polymer liquid drops, the first substrate is refrigerated to enable the temperature of the first substrate to be lower than the temperature of a transfer printing mold, a temperature gradient is introduced between the first substrate and the transfer printing mold, the enhanced transfer printing of the first polymer liquid drops is realized based on the temperature Magrani effect under the micro-nano scale, and the volume control of the transfer printing of the first polymer liquid drops is realized as shown in fig. 1 (b), wherein fig. 1 (a) is a schematic diagram of a traditional transfer printing method. In addition, due to the temperature adjustment of the first substrate, the contact angle adjustment of the first polymer droplet array and the first substrate can be realized, so that the adjustment of the morphology of the first polymer droplet is realized.
The invention adopts an active refrigeration drop forming method to prepare a second drop array on the curved surface of the first polymer drop, and realizes the preparation of a secondary microstructure on the curved surface through the imprinting of the second drop array. The adjustment of the size and spacing of the second droplets can be achieved by varying the condensation conditions such as refrigeration temperature, condensation time and vapor concentration. For example, the lower the refrigeration temperature, the longer the condensation time and the greater the vapor concentration, the larger the diameter of the first polymer droplet respectively obtained. Initially, the second droplet is completely immersed in the first polymer droplet due to the surface tension of the second droplet, as shown in fig. 2 (a). The acting force of the second liquid drop under the micro-nano scale is mainly surface tension, and new acting force is required to be introduced to realize the cross section morphology regulation of the second liquid drop. The invention introduces a third polymer to replace an air layer, changes the previous three-phase interface of the first polymer liquid drop-the second liquid drop-the air into the three-phase interface of the first polymer liquid drop-the second liquid drop-the third polymer, and realizes the change of the appearance of the second liquid drop through the new interfacial tension effect, as shown in the figure 2 (b). Finally, the first polymer droplet array is cured and formed, and the third polymer and the second droplet array are removed, finally, a dual-stage microstructure array is obtained, as shown in fig. 2 (c).
Compared with the prior art, the technical scheme provided by the invention has the following characteristics: the liquid drops are adopted as the mould for preparing the surface double-stage microstructure array, so that the manufacturing cost is reduced, the preparation process is simplified, the harm to human bodies and the environment caused by the use of an organic solvent in the traditional preparation process is avoided, and the problem of limited application of a single-layer surface microstructure is solved through the preparation of the surface double-stage microstructure.
According to the invention, the idea of additive manufacturing and subtractive manufacturing is adopted, the two-stage microstructure array is prepared based on a temperature regulation and control two-stage droplet forming method, and the flexible regulation and control of the morphology parameters of the two-stage microstructure is realized through the regulation of the technological parameters of the two-stage droplet forming.
Therefore, the invention has the advantages of simple process, low cost, environmental protection and the like, and the prepared surface double-stage microstructure has high light extraction efficiency and strong light scattering capability.
Drawings
Fig. 1 is a schematic diagram of a first polymer droplet transfer principle in a conventional mode and a temperature gradient enhancement mode in a two-stage microstructure preparation method, wherein fig. 1 (a) is a schematic diagram of a conventional transfer method, and fig. 1 (b) is a schematic diagram of a temperature gradient enhancement transfer method;
fig. 2 is a schematic diagram of a principle of morphology regulation of a second droplet by a third polymer in a two-stage microstructure preparation method, in which fig. 2 (a) is a schematic diagram of a second droplet completely immersed in a first polymer droplet, fig. 2 (b) is a schematic diagram of a principle of morphology change of the second droplet, and fig. 2 (c) is a schematic diagram of a two-stage microstructure prepared by the two-stage microstructure preparation method;
FIG. 3 is a schematic diagram showing droplet picking in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 4 is a schematic diagram before droplet transfer in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 5 is a schematic diagram of the droplet transfer in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
fig. 6 is a schematic front view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 7 is a schematic top view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 8 is a schematic diagram showing the condensation of water droplets in step 3 of the experimental procedure of the method for preparing a surface two-stage microstructure according to example 1 of the present invention;
FIG. 9 is a schematic diagram of experimental procedure 4 of the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 10 is a schematic diagram of experimental procedure 5 of the method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 11 is a schematic diagram of an experimental procedure 6 of a method for preparing a surface dual-stage microstructure according to embodiment 1 of the present invention;
FIG. 12 is a schematic diagram of a two-stage microstructure array obtained by the method for preparing a two-stage microstructure on a surface according to embodiment 1 of the present invention;
FIG. 13 is a schematic view of droplet pickup in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 14 is a schematic diagram before transferring droplets in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 15 is a schematic diagram of the droplet transfer in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
fig. 16 is a schematic front view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 17 is a schematic top view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 18 is a schematic diagram showing droplet condensation in step 3 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to example 2 of the present invention;
FIG. 19 is a schematic diagram of experimental procedure 4 of the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 20 is a schematic diagram of experimental procedure 5 of the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 21 is a schematic diagram of the experimental procedure 6 of the method for preparing a surface dual-stage microstructure according to embodiment 2 of the present invention;
FIG. 22 is a schematic diagram of a two-stage microstructure array obtained by the method for preparing a two-stage microstructure on a surface according to embodiment 2 of the present invention;
FIG. 23 is a schematic view of droplet pickup in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
FIG. 24 is a schematic diagram before droplet transfer in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
FIG. 25 is a schematic diagram of the droplet transfer in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
fig. 26 is a schematic front view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
FIG. 27 is a schematic top view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
FIG. 28 is a schematic drawing showing the condensation of ethylene glycol in step 3 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to example 3 of the present invention;
FIG. 29 is a schematic diagram of experimental procedure 4 of the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
fig. 30 is a schematic diagram of experimental steps 5 and6 of the method for preparing a surface dual-stage microstructure according to embodiment 3 of the present invention;
FIG. 31 is a schematic diagram of a two-stage microstructure array obtained by the method for preparing a surface two-stage microstructure according to embodiment 3 of the present invention;
FIG. 32 is a schematic drawing showing the droplet pickup in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to embodiment 4 of the present invention;
FIG. 33 is a schematic diagram before transferring droplets in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to example 4 of the present invention;
FIG. 34 is a schematic diagram of the droplet transfer in step 2 of the experimental procedure in the method for preparing a surface dual-stage microstructure according to example 4 of the present invention;
fig. 35 is a schematic front view of a transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 4 of the present invention;
FIG. 36 is a schematic top view of the transfer mold in step 2 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to embodiment 4 of the present invention;
FIG. 37 is a schematic diagram showing droplet coagulation in step 3 of the experimental procedure of the method for preparing a surface dual-stage microstructure according to example 4 of the present invention;
FIG. 38 is a schematic diagram of experimental procedure 4 of the method for preparing a surface dual-stage microstructure according to example 4 of the present invention;
FIG. 39 is a schematic diagram of experimental steps 5 and6 of the method for preparing a surface dual-stage microstructure according to embodiment 4 of the present invention;
FIG. 40 is a schematic diagram of a two-stage microstructure array obtained by the method for preparing a surface two-stage microstructure according to example 4 of the present invention.
Detailed Description
The invention will be further described with reference to examples and with reference to the accompanying drawings.
Example 1:
as shown in fig. 3-12, a method for preparing a two-stage microstructure on the surface of a droplet forming method based on temperature regulation and control comprises the following steps:
1. preparing a first substrate 101, wherein the first substrate 101 is made of glass sheets, and the first substrate 101 is placed on a temperature control platform 102;
2. setting the temperature of the first substrate 101 to be minus 20 ℃ through the temperature control platform 102, enabling the temperature of the first substrate 101 to be lower than the ambient temperature by 20 ℃, transferring ultraviolet curing adhesive (NORLAND 61) 105 from a container 104 to the surface of the first substrate 101 by adopting a transfer mold 103 on a three-dimensional moving platform to obtain an ultraviolet curing adhesive 105 liquid drop array, wherein the transfer mold 103 is a hard mold made of silicon materials, and obtaining the ultraviolet curing adhesive 105 liquid drop array with the liquid drop diameter of 100 mu m on the surface of the first substrate 101;
3. placing a first substrate 101 with an ultraviolet curing glue 105 drop array on a temperature control platform 102 in a water vapor atmosphere controlled by humidifying airflow 106 in a humidity control system, and realizing temperature adjustment of the ultraviolet curing glue 105 drop array through refrigeration action of the temperature control platform 102, so that the temperature of the ultraviolet curing glue 105 drop array is lower than the ambient temperature, and water vapor in the air is condensed and nucleated on the curved surface of the ultraviolet curing glue 105 drop array; after 2min of condensation time, water vapor self-assembles on the curved surface of the ultraviolet curing glue 105 liquid drop array to form a second water drop array 107 which is uniformly distributed and has the diameter of 10 mu m, and water drops enter the ultraviolet curing glue 105 liquid drop array due to the action of surface tension; wherein, the ambient temperature is controlled to be 20 ℃, the concentration of the vapor atmosphere is controlled to be 75%, and the refrigeration temperature of the temperature control platform 102 is controlled to be-20 ℃;
4. preparing a second substrate 108, wherein the second substrate 108 is a PMMA plate, spin-coating silica gel 109 on the surface of the second substrate 108 by adopting a spin-coating method, and obtaining the silica gel 109 with the thickness of 200 mu m on the second substrate 108;
5. covering the silica gel 109 on the second substrate 108 on the ultraviolet curing glue 105 drop array with the second drop array 107, wherein the silica gel 109 faces downwards, and the second drop array 107 on the curved surface of the ultraviolet curing glue 105 drop array is stamped into the silica gel 109 under the action of surface tension to form a stable silica gel-water drop-ultraviolet curing glue three-phase interface;
6. the ultraviolet lamp 110 irradiates to realize the complete solidification of the ultraviolet curing glue 105 drop array, thereby obtaining a curved surface second microstructure array corresponding to the shape of the second drop array 107 on the surface of the ultraviolet curing glue 105 drop array, wherein the ultraviolet irradiation energy is 3W/cm 2 The curing time is 15min;
7. and stripping the second substrate 108 from the surface of the first substrate 101, respectively cleaning the surface of the ultraviolet curing adhesive 105 drop array on the surface of the first substrate 101 by adopting acetone and deionized water, and removing the second drop array 107 and the silica gel 109 to finally obtain the two-stage microstructure array.
Example 2:
as shown in fig. 13-22, a method for preparing a two-stage microstructure on the surface of a droplet forming method based on temperature regulation, comprising the following steps:
1. preparing a first substrate 201, wherein the first substrate 201 is made of silica gel, and the first substrate 201 is placed on a temperature control platform 202;
2. setting the temperature of the first substrate 201 to be 0 ℃ through a temperature control platform 202, enabling the temperature of the first substrate 201 to be less than 10 ℃ of the environment temperature, transferring ultraviolet curing glue (NORLAND 68) 205 from a container 204 to the surface of the first substrate 201 by adopting a transfer mold 203 on a three-dimensional moving platform, so as to obtain an ultraviolet curing glue 205 droplet array, wherein the transfer mold 203 is a soft mold made of PDMS, and the ultraviolet curing glue 205 droplet array with the droplet diameter of 50 mu m is obtained on the surface of the first substrate 201;
3. the first substrate 201 with the ultraviolet curing glue 205 drop array on the temperature control platform 202 is placed in a water-glycerol mixed vapor atmosphere controlled by a humidifying airflow 206 in a humidity control system, and the mass ratio of water to glycerol in the humidifying solution is 1:1. The temperature of the ultraviolet curing glue 205 droplet array is adjusted through the refrigeration action of the temperature control platform 202, so that the temperature of the ultraviolet curing glue 205 droplet array is lower than the ambient temperature, and water-glycerol mixed vapor in the air is coagulated and nucleated on the curved surface of the ultraviolet curing glue 205 droplet array; after 5min of condensation time, the water-glycerol mixed vapor is self-assembled on the curved surface of the ultraviolet curing glue 205 liquid drop array to form a second water-glycerol liquid drop array 207 which is uniformly distributed and has the diameter of 5 mu m, and the water-glycerol liquid drops enter the inside of the ultraviolet curing glue 205 liquid drop array due to the action of surface tension; wherein, the environment temperature is controlled to be 10 ℃, the concentration of the water-glycerol mixed vapor atmosphere is controlled to be 70%, and the refrigeration temperature of the temperature control platform 202 is controlled to be 0 ℃;
4. preparing a second substrate 208, wherein the second substrate 208 is a glass sheet, and epoxy resin 209 is spin-coated on the surface of the second substrate 208 by a spin coating method, so as to obtain the epoxy resin 209 with the thickness of 100 mu m on the second substrate 208;
5. covering the epoxy resin 209 on the second substrate 208 on the ultraviolet curing glue 205 droplet array with the second water-glycerol droplet array 207, wherein the epoxy resin 209 faces downwards, and the second water-glycerol droplet array 207 on the curved surface of the ultraviolet curing glue 205 droplet array is stamped into the epoxy resin 209 under the action of surface tension to form a stable epoxy resin-water-glycerol droplet-ultraviolet curing glue three-phase interface;
6. the ultraviolet lamp 210 irradiates to realize the complete solidification of the ultraviolet curing glue 205 drop array, thereby obtaining a curved surface second microstructure array corresponding to the shape of the second water-glycerol drop array 207 on the surface of the ultraviolet curing glue 205 drop array, wherein the ultraviolet irradiation energy is 8W/cm 2 The curing time is 5min;
7. and stripping the second substrate 208 from the surface of the first substrate 201, respectively cleaning the surface of the ultraviolet curing adhesive 205 droplet array on the surface of the first substrate 201 by adopting acetone and deionized water, and removing the second water-glycerol droplet array 207 and the epoxy resin 209 to finally obtain the two-stage microstructure array.
Example 3:
as shown in fig. 23-31, a method for preparing a two-stage microstructure on the surface of a droplet forming method based on temperature regulation, comprising the following steps:
1. preparing a first substrate 301, wherein the first substrate 301 is made of polystyrene, and the first substrate 301 is placed on a temperature control platform 302;
2. setting the temperature of a first substrate 301 to be 10 ℃ through a temperature control platform 302, enabling the temperature of the first substrate 301 to be less than the ambient temperature of 25 ℃, transferring silica gel 305 from a container 304 to the surface of the first substrate 301 by adopting a transfer mold 303 on a three-dimensional moving platform to obtain a silica gel 305 liquid drop array, wherein the transfer mold 303 is a hard mold made of silicon material, and obtaining the silica gel 305 liquid drop array with the liquid drop diameter of 10 mu m on the surface of the first substrate 301;
3. placing a first substrate 301 with a silica gel 305 liquid drop array on a temperature control platform 302 in an ethylene glycol vapor atmosphere controlled by humidifying airflow 306 in a humidity control system, and realizing the temperature adjustment of the silica gel 305 liquid drop array through the refrigeration action of the temperature control platform 302, so that the temperature of the silica gel 305 liquid drop array is lower than the ambient temperature, and thus ethylene glycol vapor in the environment is coagulated and nucleated on the curved surface of the silica gel 305 liquid drop array; after 2min of condensation time, the glycol vapor self-assembles on the curved surface of the silica gel 305 droplet array to form a second glycol droplet array 307 which is uniformly distributed and has a diameter of 1 mu m, and the glycol droplets enter the silica gel 305 droplet array due to the action of surface tension; wherein, the ambient temperature is controlled to 25 ℃, the ethylene glycol vapor atmosphere concentration is controlled to 90%, and the refrigeration temperature of the temperature control platform 302 is 10 ℃;
4. preparing a second substrate 308, wherein the second substrate 308 is a glass plate, spin-coating ultraviolet curing glue (NORLAND 61) 309 on the surface of the second substrate 308 by adopting a spin-coating method, and obtaining ultraviolet curing glue 309 with the thickness of 30 mu m on the second substrate 308;
5. covering ultraviolet curing glue 309 on a second substrate 308 on a silica gel 305 droplet array with a second glycol droplet array 307, wherein the ultraviolet curing glue 309 faces downwards, and under the action of surface tension, the second glycol droplet array 307 on the curved surface of the silica gel 305 droplet array is stamped into the ultraviolet curing glue 309 to form a stable ultraviolet curing glue-ethylene glycol-silica gel three-phase interface;
6. the silica gel 305 liquid drop array is completely cured in a heat curing mode, so that a curved surface second microstructure array corresponding to the shape of the second glycol liquid drop array 307 is obtained on the surface of the silica gel 305 liquid drop array, wherein the curing temperature is 150 ℃, and the curing time is 90min;
7. and stripping the second substrate 308 from the surface of the first substrate 301, respectively cleaning the surface of the silica gel 305 droplet array on the surface of the first substrate 301 by adopting acetone and deionized water, and removing the second glycol droplet array 307 and the ultraviolet polymer 309 to finally obtain the double-stage microstructure array.
Example 4:
as shown in fig. 32-40, a method for preparing a surface two-stage microstructure by a droplet forming method based on temperature regulation comprises the following steps:
1. preparing a first substrate 401, wherein the first substrate 401 is a glass sheet, and placing the first substrate 401 on a temperature control platform 402;
2. setting the temperature of a first substrate 401 to be minus 25 ℃ through a temperature control platform 402, enabling the temperature of the first substrate 401 to be smaller than the ambient temperature of 25 ℃, transferring epoxy resin 405 from a container 404 to the surface of the first substrate 401 by adopting a transfer mold 403 on a three-dimensional moving platform to obtain an epoxy resin 405 liquid drop array, wherein the transfer mold 403 is a soft mold made of PDMS, and obtaining the epoxy resin 405 liquid drop array with the liquid drop diameter of 1000 mu m on the surface of the first substrate 401;
3. placing a first substrate 401 with an epoxy resin 405 drop array on a temperature control platform 402 in a water vapor atmosphere controlled by humidifying airflow 406 in a humidity control system, and realizing temperature adjustment of the epoxy resin 405 drop array through refrigeration action of the temperature control platform 402, so that the temperature of the epoxy resin 405 drop array is lower than the ambient temperature, and thus water vapor in the environment is coagulated and nucleated on a curved surface of the epoxy resin 405 drop array; after 5min of condensation time, the water vapor self-assembles on the curved surface of the epoxy resin 405 drop array to form a second drop array 407 which is uniformly distributed and has a diameter of 50 mu m, and due to the action of surface tension, the water drops enter the interior of the epoxy resin 405 drop array; wherein, the ambient temperature is controlled to 25 ℃, the concentration of the water vapor atmosphere is controlled to 75%, and the refrigeration temperature of the temperature control platform 402 is-25 ℃;
4. preparing a second substrate 408, wherein the second substrate 408 is a transparent ABS plate, spin-coating ultraviolet curing glue (NORLAND 68) 409 on the surface of the second substrate 408 by adopting a spin-coating method, and obtaining ultraviolet curing glue 409 with the thickness of 1000 mu m on the second substrate 408;
5. covering the ultraviolet curing glue 409 on the second substrate 408 on the epoxy resin 405 drop array with the second water drop array 407, wherein the ultraviolet curing glue 409 faces downwards, and the second water drop array 407 on the curved surface of the epoxy resin 405 drop array is stamped into the ultraviolet curing glue 409 under the action of surface tension to form a stable ultraviolet curing glue-water-epoxy resin three-phase interface;
6. the complete solidification of the epoxy resin 405 drop array is realized in a heat-curing mode, so that a curved surface second microstructure array corresponding to the shape of the second drop array 407 is obtained on the surface of the epoxy resin 405 drop array, wherein the solidification temperature is 200 ℃, and the solidification time is 90min;
7. and stripping the second substrate 408 from the surface of the first substrate 401, respectively cleaning the surface of the epoxy resin 405 drop array on the surface of the first substrate 41 by adopting acetone and deionized water, and removing the second drop array 407 and the ultraviolet polymer 409 to finally obtain the two-stage microstructure array.
Claims (10)
1. A preparation method of a two-stage microstructure on the surface of a liquid drop forming method based on temperature regulation and control is characterized by comprising the following steps: the method comprises the following steps:
A. preparing a first substrate, and placing the first substrate on a temperature control platform;
B. controlling the temperature of the first substrate through a temperature control platform, and transferring the first polymer in the container to the surface of the first substrate by adopting a transfer mold to obtain a first polymer droplet array;
C. preparing a vapor atmosphere control system, realizing temperature regulation of a first polymer droplet array through refrigeration action of a temperature control platform, enabling the temperature of the first polymer droplet to be lower than the ambient temperature, enabling vapor to be coagulated and nucleated on a curved surface of the first polymer droplet, enabling the vapor to self-assemble into a second droplet array on the curved surface of the first polymer droplet after coagulation for a certain time, and enabling the second droplet array to enter the interior of the first polymer droplet array due to surface tension action, wherein: the second droplet is immiscible with the first polymer;
D. preparing a second substrate, placing a third polymer on a surface of the second substrate, wherein: the third polymer is immiscible with the first polymer and the second droplet;
E. overlaying a third polymer on a second substrate on the first polymer droplet array having the second droplet array to form a stable first polymer-second droplet-third polymer three-phase interface;
F. solidifying the first polymer droplet array until the first polymer droplet array is completely solidified to obtain a first polymer microstructure array, and obtaining a curved surface second microstructure array corresponding to the second droplet array on the surface of the first polymer microstructure array due to the imprinting effect of the second droplet array;
G. and stripping the second substrate, removing the second liquid drop array and the third polymer on the surface of the first polymer microstructure array, and finally obtaining the two-stage microstructure array.
2. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the first substrate material in the step A is one of glass, silica gel, polystyrene, polycarbonate or polymethyl methacrylate high light transmission material.
3. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the temperature setting value of the temperature control platform in the step B is T1, wherein T1 is smaller than the ambient temperature Ta, so that the temperature of the first substrate is lower than the temperature of the transfer mold.
4. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: and B, the transfer printing mold is a hard mold or a soft mold, the hard mold is made of a silicon material or a silicon dioxide material, and the soft mold is made of a polydimethylsiloxane material.
5. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the first polymer in the step B is an ultraviolet curing polymer, and the corresponding curing mode in the step F is that the first polymer is completely cured by irradiation of an ultraviolet lamp, and the curing time is 1-30 min; or the first polymer in the step B is a heat-curing polymer, and the corresponding curing mode in the step F is to realize complete curing of the first polymer by a heating curing method, wherein the curing time is 10-300 min.
6. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the mode of transferring the first polymer droplet array on the surface of the first substrate in the step B is that the first polymer is dipped from a container and transferred on the surface of the first substrate through a transfer mold on a three-dimensional moving platform in a three-dimensional position control system, so that the first polymer droplet array is obtained, and the diameter of the obtained first polymer droplet is 5-1000 mu m.
7. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the vapor atmosphere control system in the step C can realize vapor atmosphere and ensure the control of the concentration of the vapor atmosphere, wherein the vapor atmosphere is one of water, methanol, ethanol, glycol or glycerol, or one of two or more of water, methanol, ethanol, glycol or glycerol, and the concentration control range of the vapor atmosphere is 10% -90%.
8. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: and C, the refrigerating temperature T2 of the temperature control platform is 5-40 ℃ lower than the ambient temperature Ta, the condensation time of the second liquid drops is 2-30 min, and the diameter of the obtained second liquid drops is 0.5-100 mu m.
9. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the second substrate material in the step D is one of glass, polymethyl methacrylate or acrylonitrile-butadiene-styrene copolymer.
10. The method for preparing the surface double-stage microstructure by the liquid drop forming method based on temperature regulation and control according to claim 1, which is characterized in that: the third polymer in the step D is one of a conventional liquid polymer, an ultraviolet curing polymer or a thermosetting polymer, and does not have the same curing form as the first polymer, namely, the third polymer cannot be cured by ultraviolet irradiation when the first polymer is an ultraviolet curing material, or cannot be cured by heating when the first polymer is a thermosetting material, and the third polymer is placed on the second substrate by a spot coating or spin coating mode, and has a thickness of 6-1000 μm.
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