CN107188114B - Surface microstructure preparation method based on active refrigeration liquid drop condensation - Google Patents
Surface microstructure preparation method based on active refrigeration liquid drop condensation Download PDFInfo
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- CN107188114B CN107188114B CN201710351836.XA CN201710351836A CN107188114B CN 107188114 B CN107188114 B CN 107188114B CN 201710351836 A CN201710351836 A CN 201710351836A CN 107188114 B CN107188114 B CN 107188114B
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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
- B81C1/00436—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
- B81C1/00468—Releasing structures
- B81C1/00484—Processes for releasing structures not provided for in group B81C1/00476
Abstract
The invention discloses a surface microstructure preparation method based on active refrigeration liquid drop condensation, which is characterized in that the surface temperature of a polymer placed in a certain steam environment is lower than the ambient temperature through an active refrigeration liquid drop condensation technology, so that steam in the air nucleates on the surface of the polymer, condenses and grows, self-assembles into liquid drops which are uniformly distributed, and ultraviolet curing is adopted to realize polymer curing and liquid drop evaporation, so that a uniformly distributed microstructure is obtained on the surface of the polymer. The invention only adopts single-phase polymer material, adopts active refrigeration to realize the temperature reduction of the polymer and the condensation of liquid drops, is used for replacing the traditional surface microstructure preparation technology utilizing the volatilization refrigeration of organic solvent, simplifies the preparation process, avoids the problems of toxic hazard to human bodies, environmental pollution and the like caused by the use of the organic solvent, and has the advantages of simple process, low cost, flexible and controllable microstructure size and shape, environmental protection and the like.
Description
Technical Field
The invention relates to a preparation technology of an organic colloid surface microstructure, in particular to a preparation method of a surface microstructure based on active refrigeration liquid drop condensation.
Background
The surface microstructure film is widely applied to the fields of optics, biomedicine, functional materials and the like. At present, the main surface microstructure preparation technologies mainly include methods such as photolithography and mold imprinting.
The photoetching method needs to manufacture a mask plate, depends on photoetching machine equipment, comprises the processes of gluing, exposing, developing, pre-baking, post-baking and the like, and has higher cost and complex process. The mold imprinting method generally comprises two steps, namely manufacturing the mold, and then pressing and molding the mold to form the microstructure on the surface of the colloid. The processing of the die still needs to depend on photoetching, etching and laser processing technologies, the defects of high cost, long manufacturing period and complex process cannot be solved, and the microstructure is easy to damage during demoulding. The shape and roughness of the microstructure are completely determined by the shape and quality of the die; in addition, the temperature, pressure, viscosity of the polymer fluid, etc. during molding may affect the surface quality of the microstructure, thereby affecting its physical and optical properties, etc.
The breathing pattern method utilizes water drops as an imprinting mold, the specific process is that a polymer is dissolved in a volatile organic solvent which is not soluble in water, the solvent is quickly volatilized to generate a certain temperature gradient, the surface temperature of the polymer solution is reduced, water vapor in a high-humidity environment nucleates on the surface of the solution, the water drops grow and self-assemble into an ordered array along with the continuation of the volatilization-condensation process, and when the solvent is completely volatilized, a microstructure is formed on the surface of the polymer. The physical properties of the solution are changed along with the volatilization of the solvent, and the whole process belongs to a non-isothermal and non-equilibrium process, so that the temperature control of the surface of the solution is very difficult, the effective control of the condensation process of water drops cannot be realized, and the size and the periodic distribution of the microstructures corresponding to the water drops one by one cannot be flexibly regulated. In addition, the organic solvent is usually chloroform or carbon disulfide, which is toxic to human body and pollutes environment.
Disclosure of Invention
The invention aims to provide a surface microstructure preparation method based on active refrigeration liquid drop condensation, which has the advantages of low cost, simple process and flexible and controllable appearance.
The purpose of the invention is realized as follows:
a surface microstructure preparation method based on active refrigeration liquid drop condensation is characterized in that: the method comprises the following steps:
A. preparing a substrate, and placing a polymer on the surface of the substrate to obtain a polymer film on the substrate;
B. the polymer film is arranged below an ultraviolet lamp, and the precuring of the polymer is realized through ultraviolet irradiation;
C. preparing a constant-temperature and constant-humidity environment control box with a steam atmosphere, placing a pre-solidified polymer film on a cold surface of a semiconductor refrigerator, and realizing polymer temperature regulation through the semiconductor refrigerator to ensure that the temperature of the polymer is lower than the ambient temperature, so that steam in the air is condensed and nucleated on the surface of the polymer;
D. after a certain coagulation time, the liquid drops are self-assembled on the surface of the polymer into uniformly distributed liquid drops, and the liquid drops partially enter the interior of the polymer due to the action of surface tension;
E. the complete solidification of the polymer and the evaporation of the liquid drops are realized through the irradiation of an ultraviolet lamp, so that microstructures corresponding to the liquid drops one by one are obtained on the surface of the polymer film;
F. and peeling the polymer film from the surface of the substrate to obtain the polymer film with the microstructure on the surface.
The polymer in the step A is ultraviolet curing glue.
Further, the method for placing the polymer on the surface of the substrate in the step a includes a spin coating method and a dot coating method, and the polymer films obtained corresponding to the surface of the substrate are respectively a planar film and a curved film with uniformly distributed thicknesses.
Further, the pre-curing energy of the polymer in step B is 0 ~ 6J/cm2The precure time was 1 ~ 30 min.
Further, the environment control box in the step C can realize control of the environment temperature and the environment humidity, the environment temperature control range is 15 ~ 85 ℃, and the environment relative humidity control range is 0 ~ 90%.
Further, the vapor atmosphere in the environmental control box in step C is one of water, methanol, or ethanol.
Further, the refrigerating temperature range of the semiconductor refrigerator in the step C is-10 ~ 15 ℃, and the droplet condensing time is 0 ~ 30 min.
Further, the UV curing energy in step E is 0 ~ 10J/cm2The curing time was 1 ~ 30 min.
The invention uses the active refrigeration technology to make the surface temperature of the polymer in a certain steam environment lower than the environment temperature, so that the steam in the air nucleates on the surface of the polymer, condenses and grows and self-assembles into uniformly distributed liquid drops, and uses ultraviolet curing to realize the polymer curing and the liquid drop evaporation, thereby obtaining a uniformly distributed microstructure on the surface of the polymer. The invention not only changes the interaction interface of the liquid drop and the polymer by selecting different polymer materials, pre-solidification degrees and vapor atmosphere so as to realize the adjustment of the microstructure appearance, but also realizes the regulation and control of the surface microstructure size and the periodic distribution by changing different refrigeration power of the semiconductor refrigerator and the condensation time of the liquid drop.
Compared with the prior art, the technical scheme provided by the invention has the characteristics that: the method only adopts a single-phase polymer material, adopts active refrigeration to realize the temperature reduction of the polymer and realize the condensation of liquid drops, is used for replacing the traditional surface microstructure preparation technology utilizing the volatilization refrigeration of an organic solvent, simplifies the preparation process, and avoids the problems of toxic hazard to human bodies, environmental pollution and the like caused by the use of the organic solvent. Therefore, the method has the advantages of simple process, low cost, flexible and controllable size and shape of the microstructure, and environmental protection.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present invention;
FIG. 2 is a SEM image of surface microstructures at different refrigeration powers according to an embodiment of the invention;
FIG. 3 is an SEM image of surface microstructures at different setting times for an embodiment of the invention;
FIG. 4 is a SEM image of a cross section of a surface microstructure according to an embodiment of the invention.
Detailed Description
The present invention is explained in more detail below by means of examples, which are only illustrative and the scope of protection of the present invention is not limited by these examples.
Example 1:
a surface microstructure preparation method based on active refrigeration liquid drop condensation comprises the following steps:
1. preparing a substrate 1, spin-coating ultraviolet curing glue NORLAND 61 on the surface of the substrate 1 by adopting a spin-coating method, and obtaining a polymer film 2 with uniformly distributed thickness on the substrate 1;
2. the polymer film 2 is placed under an ultraviolet lamp 3, and the precuring of the polymer is realized by ultraviolet irradiation, wherein the irradiation energy of the ultraviolet lamp 3 is 2J/cm2The pre-curing time is 10 min;
3. preparing a constant-temperature constant-humidity environment control box 5 with a water vapor atmosphere, placing a pre-solidified polymer film 2 on a cold surface 8 of a semiconductor refrigerator 4, realizing temperature regulation of the polymer 2 through the semiconductor refrigerator 4, and enabling the temperature of the polymer 2 to be lower than the ambient temperature, so that water vapor 6 in the air is condensed and nucleated on the surface of the polymer 2 to form water drops 7; the environment temperature is controlled to be 15 ℃, the environment relative humidity is controlled to be 75%, and the refrigerating temperature of the semiconductor refrigerator 4 is 0 ℃;
4. after a certain coagulation time, the water drops 7 are self-assembled on the surface of the polymer into water drops 9 which are uniformly distributed, and due to the surface tension effect, the water drops 9 partially enter the polymer 2, wherein the coagulation time of the water drops is 2 min;
5. complete curing of the polymer 2 and evaporation of the water droplets 9 is achieved by irradiation with an ultraviolet lamp 10, so that a microstructure is obtained on the polymer surface, wherein: the ultraviolet irradiation energy is 4J/cm2The curing time is 10 min;
6. and peeling the polymer from the surface of the substrate to obtain the polymer film 11 with the microstructure on the surface.
Example 2:
a surface microstructure preparation method based on active refrigeration liquid drop condensation comprises the following steps:
1. preparing a substrate 1, and spin-coating an ultraviolet curing adhesive AALOCTLTE 4305 on the surface of the substrate 1 by adopting a spin-coating method to obtain a polymer film 2 with uniformly distributed thickness on the substrate 1;
2. the polymer film 2 is placed under an ultraviolet lamp 3, and the precuring of the polymer is realized by ultraviolet irradiation, wherein the irradiation energy of the ultraviolet lamp 3 is 1J/cm2The pre-curing time is 30 min;
3. preparing a constant-temperature constant-humidity environment control box 5 with an ethanol vapor atmosphere, placing a pre-solidified polymer film 2 on a cold surface 8 of a semiconductor refrigerator 4, realizing temperature regulation of the polymer 2 through the semiconductor refrigerator 4, and enabling the temperature of the polymer 2 to be lower than the ambient temperature, so that ethanol vapor 6 in the air is condensed and nucleated on the surface of the polymer 2 into liquid drops 7; wherein the environmental temperature is controlled to be 20 ℃, the environmental relative humidity is controlled to be 60%, and the refrigerating temperature of the semiconductor refrigerator 4 is-10 ℃;
4. after a certain coagulation time, the liquid drops 7 are self-assembled on the surface of the polymer into uniformly distributed liquid drops 9, and the liquid drops 9 partially enter the polymer 2 due to the action of surface tension, wherein the coagulation time of the liquid drops is 10 min;
5. complete solidification of the polymer 2 and evaporation of the droplets 9 is achieved by irradiation with an ultraviolet lamp 10, so as to obtain a microstructure on the polymer surface, in which: the ultraviolet irradiation energy is 7J/cm2Curing for 30 min;
6. and peeling the polymer from the surface of the substrate to obtain the polymer film 11 with the microstructure on the surface.
Example 3:
a surface microstructure preparation method based on active refrigeration liquid drop condensation comprises the following steps:
1. preparing a substrate 1, and coating ultraviolet curing glue MASTERBOND UV16 on the surface of the substrate 1 by adopting a spot coating method to obtain a polymer film 2 distributed on a curved surface on the substrate 1;
2. the polymer film 2 is placed under an ultraviolet lamp 3, and the precuring of the polymer is realized by ultraviolet irradiation, wherein the irradiation energy of the ultraviolet lamp 3 is 6J/cm2The pre-curing time is 1 min;
3. preparing a constant-temperature constant-humidity environment control box 5 with a methanol vapor atmosphere, placing a pre-solidified polymer film 2 on a cold surface 8 of a semiconductor refrigerator 4, and realizing temperature regulation of the polymer 2 through the semiconductor refrigerator 4 to ensure that the temperature of the polymer 2 is lower than the ambient temperature, so that methanol vapor 6 in the air is condensed and nucleated on the surface of the polymer 2 into liquid drops 7; the environment temperature is controlled to be 35 ℃, the environment relative humidity is controlled to be 90%, and the refrigerating temperature of the semiconductor refrigerator 4 is 5 ℃;
4. after a certain coagulation time, the liquid drops 7 are self-assembled on the surface of the polymer into uniformly distributed liquid drops 9, and the liquid drops 9 partially enter the interior of the polymer 2 due to the action of surface tension, wherein the coagulation time of the liquid drops is 20 min;
5. complete solidification of the polymer 2 and evaporation of the droplets 9 is achieved by irradiation with an ultraviolet lamp 10,thereby obtaining a microstructure on the surface of the polymer, wherein: the ultraviolet irradiation energy is 10J/cm2The curing time is 1 min;
6. and peeling the polymer from the surface of the substrate to obtain the polymer film 11 with the microstructure on the surface.
Example 4:
a surface microstructure preparation method based on active refrigeration liquid drop condensation comprises the following steps:
1. preparing a substrate 1, spin-coating ultraviolet curing glue NORLAND 61 on the surface of the substrate 1 by adopting a spin-coating method, and obtaining a polymer film 2 with uniformly distributed thickness on the substrate 1;
2. the polymer film 2 is placed under an ultraviolet lamp 3, and the precuring of the polymer is realized by ultraviolet irradiation, wherein the irradiation energy of the ultraviolet lamp 3 is 4J/cm2The pre-curing time is 20 min;
3. preparing a constant-temperature constant-humidity environment control box 5 with a water vapor atmosphere, placing a pre-solidified polymer film 2 on a cold surface 8 of a semiconductor refrigerator 4, realizing temperature regulation of the polymer 2 through the semiconductor refrigerator 4, and enabling the temperature of the polymer 2 to be lower than the ambient temperature, so that water vapor 6 in the air is condensed and nucleated on the surface of the polymer 2 to form water drops 7; the environment temperature is controlled to be 85 ℃, the environment relative humidity is controlled to be 10%, and the refrigerating temperature of the semiconductor refrigerator 4 is 15 ℃;
4. after a certain coagulation time, the water drops 7 are self-assembled on the surface of the polymer into water drops 9 which are uniformly distributed, and due to the surface tension effect, the water drops 9 partially enter the polymer 2, wherein the coagulation time of the water drops is 30 min;
5. complete curing of the polymer 2 and evaporation of the water droplets 9 is achieved by irradiation with an ultraviolet lamp 10, so that a microstructure is obtained on the polymer surface, wherein: the ultraviolet irradiation energy is 1J/cm2The curing time is 25 min;
6. and peeling the polymer from the surface of the substrate to obtain the polymer film 11 with the microstructure on the surface.
Fig. 2 is an SEM image of a surface microstructure obtained when the TEC refrigeration currents are 0.5a ~ 0.9.9A, respectively, fig. 3 is an SEM image of a surface microstructure obtained when the condensation time of a water droplet is 2min ~ 6min, respectively, and fig. 4 is a cross-sectional SEM image of a surface microstructure corresponding to a condensation time of 5 min.
Claims (8)
1. A preparation method of a surface microstructure based on active refrigeration liquid drop condensation is characterized by comprising the following steps:
A. preparing a substrate, and placing a polymer on the surface of the substrate to obtain a polymer film on the substrate;
B. the polymer film is arranged below an ultraviolet lamp, and the precuring of the polymer is realized through ultraviolet irradiation;
C. preparing a constant-temperature constant-humidity environment control box with a steam atmosphere, placing a pre-solidified polymer film on a cold surface of a semiconductor refrigerator, and realizing polymer temperature regulation through the semiconductor refrigerator to ensure that the temperature of the polymer is lower than the ambient temperature, so that steam in the air is condensed and nucleated on the surface of the polymer;
D. after a certain coagulation time, the liquid drops are self-assembled on the surface of the polymer into uniformly distributed liquid drops, and the liquid drops partially enter the interior of the polymer due to the action of surface tension;
E. the complete solidification of the polymer and the evaporation of the liquid drops are realized through the irradiation of an ultraviolet lamp, so that microstructures corresponding to the liquid drops one by one are obtained on the surface of the polymer film;
F. and peeling the polymer film from the surface of the substrate to obtain the polymer film with the microstructure on the surface.
2. The method for preparing the surface microstructure based on the condensation of the active refrigerant liquid drops as claimed in claim 1, wherein the polymer in the step A is an ultraviolet curing glue.
3. The method for preparing the surface microstructure based on the condensation of the active refrigerant droplets as claimed in claim 1, wherein the method for placing the polymer on the surface of the substrate in the step A comprises a spin coating method and a point coating method, and the polymer films obtained on the surface of the substrate are respectively a plane film and a curved film with uniformly distributed thicknesses.
4. The method for preparing the surface microstructure based on the condensation of the active refrigeration liquid drops as claimed in claim 1, wherein the pre-curing time of the polymer in the step B is 1-30 min.
5. The method of claim 1, wherein the environmental control chamber in step C is capable of controlling an ambient temperature and humidity, the ambient temperature is controlled within a range of 15-85 ℃ and the ambient relative humidity is controlled within a range of 10-90%.
6. The method for preparing the surface microstructure based on the condensation of the actively refrigerated liquid droplets as claimed in claim 1, wherein the vapor atmosphere in the environment control box in step C is one of water, methanol or ethanol.
7. The method for preparing the surface microstructure based on the active refrigeration liquid drop condensation as claimed in claim 1, wherein the refrigeration temperature range of the semiconductor refrigerator in step C is-10-15 ℃, and the liquid drop condensation time is 2-30 min.
8. The method for preparing the surface microstructure based on the condensation of the active refrigeration liquid drops as claimed in claim 1, wherein the ultraviolet curing time in step E is 1-30 min.
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