CN112810029A - Preparation method of polycarbonate micro-nano composite structure super-hydrophobic surface - Google Patents
Preparation method of polycarbonate micro-nano composite structure super-hydrophobic surface Download PDFInfo
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- CN112810029A CN112810029A CN202011605420.4A CN202011605420A CN112810029A CN 112810029 A CN112810029 A CN 112810029A CN 202011605420 A CN202011605420 A CN 202011605420A CN 112810029 A CN112810029 A CN 112810029A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
- B29C71/0009—After-treatment of articles without altering their shape; Apparatus therefor using liquids, e.g. solvents, swelling agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
- B29C71/0063—After-treatment of articles without altering their shape; Apparatus therefor for changing crystallisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
- B29L2007/002—Panels; Plates; Sheets
Abstract
The invention discloses a preparation method of a polycarbonate micro-nano composite structure super-hydrophobic surface, which comprises the following steps: firstly, preparing a polycarbonate flat plate with a micron protruding structure on the surface, then spraying an organic solvent on the surface of the polycarbonate flat plate, carrying out induced crystallization, standing until the organic solvent is completely volatilized, cleaning and drying to obtain the polycarbonate micro-nano composite structure super-hydrophobic surface. The preparation method provided by the invention has the advantages of simple process, cheap equipment, high processing efficiency and convenience for large-area preparation, and can realize accurate regulation and control of the size and copying of the micro-nano composite multi-layer structure. The prepared polycarbonate micro-nano composite structure has long service life and good wear resistance, and can meet the requirements of severe environment and working conditions.
Description
Technical Field
The invention belongs to the technical field of micro-nano composite structures, and particularly relates to a preparation method of a polycarbonate micro-nano composite structure super-hydrophobic surface.
Background
In nature, the phenomenon of superhydrophobicity is ubiquitous and has attracted much attention from scientists, wherein the most typical phenomenon is the lotus leaf surface, and liquid drops can freely roll on the surface of the lotus leaf surface and carry away substances on the surface, and the self-cleaning property is generally called the lotus leaf effect. In recent years, superhydrophobic surfaces based on the "lotus effect" have been widely used in industry and daily life due to their special properties of self-cleaning, water-free and contamination-resistant. For example, the super-hydrophobic surface can be used in severe working environments such as self-cleaning, dust prevention, pollution prevention, petroleum pipeline transportation and the like, and has high application value. By observing the microscopic morphology of the surface of the leaf of the self-cleaning plant such as lotus leaf, the surface of the leaf is densely distributed with the protruding structures organized by micro-nano structures of various levels, and the micro-nano composite protruding structures and the wax-like substance on the surface of the leaf support the water drops on the surface of the lotus leaf, so that the super-hydrophobic effect is realized. Another important application of nanostructures is the improvement of the wetting properties of the article surface. For example, the micron-sized bristles and nano-grooves of the water strider legs, the micron-sized hemispherical structures in the compound eyes of mosquitoes, the nano-cone structures covered on the surfaces of the micron-sized hemispherical structures, the surface micro-nano structures such as 'pockmark' protrusions densely distributed on the back wings of desert beetles and the like can greatly improve the surface infiltration characteristics of the micron-sized bristles and the nano-grooves.
Research shows that the wetting property of the material surface is mainly influenced by two factors, namely the free energy of the material surface and the rough structure of the material surface. The contact angle of the solid surface and the liquid is one of the important parameters for characterizing the wetting property of the solid surface. Hydrophobic and super-hydrophobic surfaces have wide application prospects in the fields of self-cleaning, pollution resistance and the like, and preparation technologies thereof are receiving more and more attention. Methods for preparing hydrophobic and super-hydrophobic surfaces are also roughly divided into two types according to influence factors of material infiltration characteristics, wherein the hydrophobic characteristics of the surfaces are realized by surface modification or by selecting materials with low surface free energy; the other is to achieve surface hydrophobicity by structuring the surface with a rough microstructure.
The main preparation method and technical defects of the existing polymer surface micro-nano composite structure and super-hydrophobic surface are as follows: (1) the nanometer coarse structure is copied on the surface of the polymer by adopting the technologies of an anodic aluminum oxide template method, a biological template method and the like, but the methods are based on a certain fixed template and are difficult to realize the accurate regulation and control of the size and the copying of the micro-nano composite multilayer structure; (2) a micro-nano structure and a super-hydrophobic surface which are regular and controllable in structure are processed on the surface of a polymer by a femtosecond laser high-energy beam processing method, but the processing efficiency of the technology is low, and the super-hydrophobic surface with a large area is difficult to process; (3) the nano-scale fiber screen spatial structure is prepared by adopting the technologies such as electrostatic spinning and the like, the large-area preparation of the super-hydrophobic surface can be realized, but the structure prepared by the technology has the advantages of limited surface life and poor wear resistance, and is difficult to meet the requirements of severe environment and working conditions.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background technology, and provide a method for preparing a micro-nano composite structure super-hydrophobic surface on a polycarbonate surface by combining a surface induced crystallization chemical modification technology and a micron convex structure injection molding technology.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a polycarbonate micro-nano composite structure super-hydrophobic surface comprises the following steps:
(1) preparing a polycarbonate flat plate with a micron convex structure on the surface by using polycarbonate as an injection molding material through an injection molding die;
(2) spraying an organic solvent on the surface of the polycarbonate flat plate obtained in the step (1) for induced crystallization;
(3) and (3) standing the polycarbonate flat plate obtained in the step (2) until the organic solvent is completely volatilized, and cleaning and drying to obtain the polycarbonate micro-nano composite structure super-hydrophobic surface.
The method for constructing the micro-nano coarse structure on the surface of the polymer can adopt chemical methods such as molecular self-assembly from bottom to top, crystal growth and the like besides top-down processing methods such as injection molding, coining, fine precision processing and the like, and the methods can often realize large-area nano structure preparation with extremely low cost. Therefore, the method effectively combines the two methods, and the micro-nano composite structure is prepared on the surface of the polymer. Firstly, processing a micron-sized array characteristic structure on the surface of a polymer workpiece such as Polycarbonate (PC) by utilizing the technical characteristics of micro-injection molding; then, by utilizing the surface modification method of the material, chemical reagents such as acetone and the like are adopted to carry out induced crystallization on the surface of the PC, and a nano-scale rough structure is formed on the surface of the workpiece through the recrystallization process of the surface induced crystallization process, so that a micro-nano composite structure is formed, and the super-hydrophobic effect is achieved. Meanwhile, the method also avoids the problems of insufficient strength and short service life existing in the process of injection molding by adopting an AAO template, a biological template and the like to a certain extent.
In the above preparation method, preferably, in the step (1), the molding process parameters for preparing the polycarbonate flat plate with the surface containing the micrometer protruding structures through the injection molding die are as follows: the injection rate is 10-26cm3And/s, the cooling time is 40-60s, the pressure maintaining pressure is 80-120MPa, and the pressure maintaining time is 3-10 s.
In the above preparation method, preferably, in the step (1), the temperature of the polycarbonate is 280 ℃ to 320 ℃, and the temperature of the injection molding mold is 80 ℃ to 160 ℃.
Preferably, in the step (1), the surface of the mold core in the injection molding mold has a cylindrical pore array structure or a square pore array structure with a pore diameter of 25 μm to 200 μm. The mould core material is obtained by processing different materials according to different aperture sizes, and when the aperture is smaller, a method of combining mask lithography and electroforming is adopted to obtain a nickel metal mould core; if the aperture is larger, a more convenient chemical etching method can be adopted to directly carry out etching processing on the stainless steel plate to obtain the corresponding metal mold core.
Preferably, in the step (2), the organic solvent is acetone, methanol or tetrahydrofuran.
Preferably, in the step (2), during the process of inducing crystallization, a water mist is sprayed on the surface of the polycarbonate flat plate containing the organic solvent by using a spray, and the volume concentration of the organic solvent is controlled to be 100-50%. The concentration of acetone on the surface of PC can be reduced to a certain extent, so that the induced crystallization rate is slowed down, and a finer structure is generated.
Preferably, in the step (3), the polycarbonate flat plate obtained after the step (2) is placed in a closed space and stands still.
PC is adopted as an injection molding material, and a PC flat plate containing a micron protruding structure is prepared. After the sample is cooled, the induced crystallization of the surface of the PC flat plate is carried out by adopting a chemical organic solvent such as acetone and the like. The PC molecule can generate a recrystallization process under the action of chemical reagents such as acetone and the like, so that micro spherulites with the size ranging from nano-scale to micron-scale are generated on the surface, the preparation of a micro-nano composite structure on the PC surface is realized, and the super-hydrophobic effect on the PC surface is achieved.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method provided by the invention has the advantages of simple process, cheap equipment, high processing efficiency and convenience for large-area preparation, and can realize accurate regulation and control of the size and copying of the micro-nano composite multi-layer structure.
2. On one hand, the preparation method has wide material selection and application range, the size range of the adopted microstructure mold core is wider (25-200 mu m), a finer micron protruding structure (such as a 25 mu m hole array structure) can be obtained, the solvent selection is wide, and the preparation method can be realized on any PC surface; on the other hand, a solvent induction method is adopted, and a nano-scale rough structure is formed on the surfaces of the workpiece and the micron protruding structure through recrystallization control.
3. The polycarbonate micro-nano composite structure super-hydrophobic surface prepared by the method has the advantages that the maximum contact angle can reach 155 degrees, the hydrophobic property can be continuously improved by optimizing process conditions, the service life is long, the wear resistance is good, and the requirements of severe environments and working conditions can be met.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow diagram of a manufacturing process of the present invention;
FIG. 2 is a microscopic SEM photograph of a stainless steel plate of example 1 having a 200 μm cylindrical hole array structure on the surface;
FIG. 3 is a microscopic SEM image of the surface of a PC plate having a 200 μm cylindrical array structure on the surface in example 1;
FIG. 4 is an SEM image (magnification × 200) of the surface of the PC plate of example 1 after induced crystallization;
FIG. 5 is an SEM photograph (magnification: 10000) of the surface of the PC plate of example 1 after induced crystallization;
FIG. 6 is a graph showing the hydrophobic effect of the surface-induced crystallization of the PC plate of example 1;
FIG. 7 is a microscopic SEM image of a nickel metal plate with 25 μm square hole array structure on the surface in example 2;
FIG. 8 is a microscopic SEM image of the surface of a PC plate having a 25 μm pillar array structure on the surface in example 2;
FIG. 9 is an SEM photograph (1000 times) of the surface of the PC plate of example 2 after induced crystallization;
FIG. 10 is an SEM photograph (magnification of 50000) of the surface of the PC plate of example 2 after induced crystallization;
FIG. 11 is the hydrophobic effect of the surface induced crystallization of the PC plate of example 2.
Illustration of the drawings:
1. a mold core; 2. a PC tablet; 3. forming a mold; 4. a spray; 5. an induced crystallization solvent; 6. the polycarbonate micro-nano composite structure is a super-hydrophobic surface.
Detailed Description
In order to facilitate understanding of the invention, the invention will be described more fully and in detail with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the preparation method of the polycarbonate micro-nano composite structure super-hydrophobic surface disclosed by the invention comprises the following steps as shown in figure 1:
(1) taking PC Markolon 2865 as an injection molding material, taking a stainless steel plate with a cylindrical hole array structure and 200 mu m pore diameter on the surface as a mold core 1 in an injection molding mold 3 (the microstructure of the surface structure is shown in figure 2), and adopting Sodick LD05EH2 as injection molding equipment to prepare a PC flat plate 2 with a micron protruding structure on the surface; the specific molding process parameters are as follows: melt temperature 280 ℃, mold temperature 148 ℃, and injection rate 18cm3The cooling time is 40s, the pressure maintaining pressure is 80MPa, and the pressure maintaining time is 3 s; the micrometer morphology of the surface of the molded PC flat plate 2 is respectively shown in FIG. 3, and the micrometer structure of the surface of the mold core 1 is perfectly copied to the surface of the PC flat plate 2 by adopting an injection molding method.
(2) Spraying an induced crystallization solvent 5 acetone on the surface of the PC flat plate 2 obtained in the step (1) for induced crystallization; in the process of surface induced crystallization, water mist is sprayed on the surface of a flat plate containing an acetone solvent by adopting a spray 4, the concentration of acetone on the surface 2 of PC can be reduced to a certain extent, and the volume concentration of an organic solvent is controlled to be 100-50%, so that the induced crystallization rate is slowed down, and a finer structure is generated, as shown in fig. 4 and 5.
(3) And (3) placing the PC plate obtained in the step (2) in a closed box until the acetone solvent and the water are completely volatilized, then cleaning the residual chemical substances on the surface of the PC plate 2 in an ultrasonic cleaning machine, and drying by blowing to obtain the polycarbonate micro-nano composite structure super-hydrophobic surface 6.
When the PC surface is not treated, the static contact angle of the surface is 88.9 degrees by using a contact angle measurement analyzer; when the method of the embodiment is adopted to prepare the PC surface containing the micro-nano composite structure, the maximum static contact angle which can be reached is 134 degrees under the parameters, and the hydrophobic effect is obviously improved, as shown in fig. 6.
Example 2:
the preparation method of the polycarbonate micro-nano composite structure super-hydrophobic surface disclosed by the invention comprises the following steps as shown in figure 1:
(1) taking PC Markolon 2865 as an injection molding material, taking a nickel metal plate with a 25-micrometer square hole array structure on the surface, which is obtained by adopting an etching process and an electroforming process, as a mold core 1 in an injection molding mold 3 (the microstructure of the surface structure is shown in figure 7), and taking Sodick LD05EH2 as injection molding equipment to prepare a PC flat plate 2 with a micrometer protruding structure on the surface; the specific molding process parameters are as follows: melt temperature 280 ℃, mold temperature 148 ℃, and injection rate 18cm3The cooling time is 40s, the pressure maintaining pressure is 80MPa, and the pressure maintaining time is 3 s; the micrometer morphology of the surface of the molded PC flat plate 2 is respectively shown in FIG. 8, and the micrometer structure of the surface of the mold core 1 is perfectly copied to the surface of the PC flat plate 2 by adopting an injection molding method.
(2) Spraying an induced crystallization solvent 5 acetone on the surface of the PC flat plate 2 obtained in the step (1) for induced crystallization; in the process of surface induced crystallization, water mist is sprayed on the surface of a flat plate containing an acetone solvent by using a spray 4, so that the concentration of acetone on the surface 2 of PC can be reduced to a certain extent, and the volume concentration of an organic solvent is controlled to be 100-50%, thereby slowing down the induced crystallization rate and generating a finer structure, as shown in fig. 9 and 10.
(3) And (3) placing the PC panel 2 obtained in the step (2) in a closed box until the acetone solvent and the water are completely volatilized, then cleaning the residual chemical substances on the surface of the PC panel 2 in an ultrasonic cleaning machine, and drying by blowing to obtain the polycarbonate micro-nano composite structure super-hydrophobic surface 6.
When the PC surface is not treated, the static contact angle of the surface is 88.9 degrees by using a contact angle measurement analyzer; when the method of the embodiment is adopted to prepare the surface of the PC containing the micro-nano composite structure, the maximum static contact angle of the surface of the PC is 155.0 degrees under the above parameters, and the super-hydrophobic effect is achieved, as shown in fig. 11.
Claims (7)
1. A preparation method of a polycarbonate micro-nano composite structure super-hydrophobic surface is characterized by comprising the following steps:
(1) preparing a polycarbonate flat plate with a micron convex structure on the surface by using polycarbonate as an injection molding material through an injection molding die;
(2) spraying an organic solvent on the surface of the polycarbonate flat plate obtained in the step (1) for induced crystallization;
(3) and (3) standing the polycarbonate flat plate obtained in the step (2) until the organic solvent is completely volatilized, and cleaning and drying to obtain the polycarbonate micro-nano composite structure super-hydrophobic surface.
2. The method according to claim 1, wherein in the step (1), the parameters of the molding process for preparing the polycarbonate flat plate with the surface containing the micrometer protruding structures through the injection molding mold are as follows: the injection rate is 10-26cm3And/s, the cooling time is 40-60s, the pressure maintaining pressure is 80-120MPa, and the pressure maintaining time is 3-10 s.
3. The method as claimed in claim 1, wherein the temperature of the polycarbonate in the step (1) is 280-320 ℃ and the temperature of the injection mold is 80-160 ℃.
4. The production method according to claim 1, wherein in the step (1), the core surface in the injection molding die has a cylindrical hole array structure or a square hole array structure having a hole diameter of 25 μm to 200 μm.
5. The method according to claim 1, wherein in the step (2), the organic solvent is acetone, methanol or tetrahydrofuran.
6. The method according to claim 1, wherein in the step (2), during the process of inducing crystallization, the water mist is sprayed on the surface of the polycarbonate flat plate containing the organic solvent by using a spraying agent, and the volume concentration of the organic solvent is controlled to be 100-50%.
7. The production method according to any one of claims 1 to 6, wherein in the step (3), the flat polycarbonate sheet obtained after the step (2) is left to stand in a closed space.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115851048A (en) * | 2022-11-23 | 2023-03-28 | 广东腐蚀科学与技术创新研究院 | Nano cerium oxide composite aviation coating and preparation method thereof |
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Application publication date: 20210518 |