CN111633881A - Preparation method of grating structure color functional surface based on injection molding - Google Patents
Preparation method of grating structure color functional surface based on injection molding Download PDFInfo
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- CN111633881A CN111633881A CN202010473727.7A CN202010473727A CN111633881A CN 111633881 A CN111633881 A CN 111633881A CN 202010473727 A CN202010473727 A CN 202010473727A CN 111633881 A CN111633881 A CN 111633881A
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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
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/38—Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
- B29C33/3842—Manufacturing moulds, e.g. shaping the mould surface by machining
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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
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/42—Moulds or cores; Details thereof or accessories therefor characterised by the shape of the moulding surface, e.g. ribs or grooves
-
- 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
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/76—Cores
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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
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
-
- 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
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/78—Measuring, controlling or regulating of temperature
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/10—Moulds; Masks; Masterforms
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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
- B29L2011/00—Optical elements, e.g. lenses, prisms
Abstract
The invention discloses a preparation method of a grating structure color functional surface based on injection molding, which adopts an ultraviolet lithography machine and an etching machine to prepare a silicon female die of a grating structure; conducting conductive treatment on the silicon female die, depositing a gold film conductive layer on the surface of the silicon female die, then placing the silicon female die in electroforming solution as a cathode to be connected with a pulse power supply cathode, taking a conductive nickel plate as an anode to be connected with a power supply anode, starting an electroforming process, ultrasonically cleaning by using absolute ethyl alcohol and distilled water, and drying to obtain a nickel die core with a grating structure on the surface; and mounting the nickel mold core on an injection mold, and mounting the injection mold on an injection molding machine for injection molding to obtain the grating structure color functional surface. The method has the advantages of short forming period, high production efficiency and potential of batch manufacturing.
Description
Technical Field
The invention belongs to the technical field of structural color processes, and relates to a preparation method of a grating structural color functional surface based on injection molding.
Background
Some animals and plants in nature have fine micro-nano structures on the surfaces, and bright and colorful colors, called structural colors, can be generated when the animals and plants are illuminated. The structural color has vivid color, is not easy to fade and has iridescent effect, more importantly, the surface of the structural color product does not need processes such as spraying, surface decoration and the like, and the structural color product has environmental protection property, and shows great research value and wide application prospect in the fields of color development, anti-counterfeiting, decoration and the like. From nature, scientists continuously utilize modern microstructure forming methods to prepare different bionic microstructures for realizing artificial reproduction of structural colors. The current common structural color preparation methods comprise a biological template method, a nano-imprinting method, a femtosecond laser and the like, although the methods successfully prepare the structural color surface, the defects of uncontrollable preparation process and large-area manufacture are existed, and the application of the structural color is limited.
Injection molding, as a template replication technique, has some mechanistic similarities to some of the above-described manufacturing methods. In addition, the injection molding technology has the advantages of low manufacturing cost, short molding period, high production efficiency and mass manufacturing potential, and has been successfully applied in the fields of microfluidics, superhydrophobicity and the like aiming at the preparation of the microstructure. However, at present, no relevant report is found on the preparation of the functional surface of the micro-nano structure by the injection molding technology and the appearance of the structural color. Therefore, the research on the injection molding preparation of the structural color functional surface has certain scientific research value and application value.
Disclosure of Invention
In order to achieve the purpose, the invention provides a preparation method of a grating structure color functional surface based on injection molding, which has the advantages of short molding period, high production efficiency and high batch manufacturing potential.
The technical scheme adopted by the invention is that the preparation method of the grating structure color functional surface based on injection molding is carried out according to the following steps:
step S1: preparing a silicon female die with a grating structure by adopting an ultraviolet photoetching machine and an etching machine;
step S2: conducting conductive treatment on the silicon master mold in the step S1 by using a high vacuum sputtering coating instrument, depositing a gold film conductive layer on the surface of the silicon master mold, then placing the silicon master mold in electroforming solution as a cathode to be connected with a pulse power supply cathode, and connecting a conductive nickel plate as an anode to a power supply anode to start an electroforming process, wherein the initial current of electroforming is 0.08A, the electroforming time is 30min, the later current is 0.25A, and the electroforming time is 900 min; after electroforming is finished, ultrasonically cleaning the nickel mould core by using absolute ethyl alcohol and distilled water, and fully drying the nickel mould core to obtain a nickel mould core with a grating structure on the surface;
step S3, mounting the nickel mold core prepared in the step S2 on an injection mold, and then mounting the injection mold on an injection molding machine for injection molding, wherein the injection molding process parameters are as follows: melt temperature Tmelt235 ℃ and injection rate Vinj＝18cm3S, mold temperature Tmold120 ℃ and a holding pressure Ppack150MPa, dwell time tpack8s, back pressure Pback8Mpa, demolding temperature TdeAnd obtaining the grating structure color functional surface at 85 ℃.
Further, in the step S3, in the injection molding process, the injection molding material is polypropylene PP.
Further, the specific process of step S1 is: processing a mask plate with a grating structure on the surface of a glass substrate; covering a layer of positive photoresist on the surface of the silicon plate, baking the positive photoresist for a period of time, and exposing the photoresist through a mask plate by using an ultraviolet photoetching machine; carrying out development and post-baking treatment on the exposed photoresist; carrying out plasma etching on the developed silicon plate by using an etching machine; and removing the photoresist which is not subjected to exposure treatment to obtain the silicon master mold with the grating structure.
Further, a URE-2000135 type ultraviolet lithography machine and an NLD-570 type etching machine are adopted in the step S1, a LEICA EM SCD 500 type high vacuum sputtering film plating instrument is adopted to conduct electricity to the silicon female die in the step S2, an YBM-1IH type oil type die temperature machine is adopted to achieve temperature rise and fall of the injection mold in the step S3, and a SIC-3A type water cooling machine is adopted to cool the injection molding machine.
Further, in the step S2, the periodic stripes of the grating structure are 300 to 1100 nm.
Further, in step S2, the thickness of the gold film conductive layer is 15-20 nm.
The invention has the beneficial effects that: the injection molding surface material is polymer, so the injection molding surface material has the advantages of low manufacturing cost, short molding period, high production efficiency and mass manufacturing potential. The polypropylene PP has good fluidity and provides guarantee for the filling of the microstructure. The depth and width of the grating structure are in the micro-nano level, and the grating structure belongs to the micro-injection molding category. Compared with the traditional injection molding, the micro injection molding has a serious size effect, and the process parameters such as temperature, pressure, environmental conditions and the like in the molding process have important influence on the high-precision molding and copying of the microstructure. Therefore, the preparation research of the structural color functional surface can provide important reference significance for the structural color correlation research.
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 described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the grating structure color functional surface injection molding process of the present invention.
FIG. 2 is a color reflection spectrum of the grating structure of the present invention.
FIG. 3 shows a silicon master mold with a grating structure.
FIG. 4 shows a nickel mold core with a grating structure on the surface.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the grating structure color functional surface based on injection molding in the embodiment of the invention has the flow as shown in fig. 1, and is carried out according to the following steps:
step S1: preparing a silicon female die with a grating structure by adopting instruments such as an ultraviolet photoetching machine, an etching machine and the like;
the method comprises the following specific steps: processing a mask plate with a grating structure on the surface of a glass substrate; covering a layer of positive photoresist on the surface of the silicon plate, baking the positive photoresist for a period of time, and exposing the photoresist through a mask plate by using an ultraviolet photoetching machine; carrying out development and post-baking treatment on the exposed photoresist; carrying out plasma etching on the developed silicon plate by using an etching machine; and removing the photoresist which is not subjected to exposure treatment to obtain the silicon master mold with the grating structure. The silicon master structure of the grating structure is shown in fig. 3.
The periodic stripes of the grating structure are 300-1100 nm. This range is based on the visible wavelength range beyond which no color is observed.
In this embodiment, a URE-2000135 type UV lithography machine and an NLD-570 type etching machine are used.
Step S2: and (4) conducting the silicon master mold in the step S1 by using a high vacuum sputtering coating instrument, depositing a gold film conducting layer on the surface of the silicon master mold, and effectively transferring and depositing metal ions in the later electroforming process. Then placing the silicon female die in electroforming solution as a cathode to be connected with a pulse power supply cathode, taking a conductive nickel plate as an anode to be connected with a power supply anode, and starting an electroforming process, wherein in the initial electroforming stage, the better filling property of the grating microstructure is considered, a small current of 0.08A is adopted, the electroforming time is 30min, and if the current is too large, the situation of insufficient filling of the grating microstructure is caused; on the premise of ensuring the filling performance in the later period, in order to improve the electroforming efficiency and reduce the electroforming time, the current is increased to 0.25A, and the electroforming time is 900 min. The current setting cannot be too high, and the defects of obvious edge effect, long tumor and the like are easily caused by too high current setting.
In this example, the silicon master mold was subjected to a conductive treatment using a model LEICA EM SCD 500 high vacuum sputtering apparatus.
After the electroforming is finished, the nickel mold core with the grating structure on the surface is obtained by using absolute ethyl alcohol and distilled water for ultrasonic cleaning and fully drying, and the structure is shown in figure 4.
The thickness of the gold film conducting layer is about 15-20nm, and the shape and size of the surface microstructure are not affected.
Step S3: the nickel mold core in step S2 was mounted on an injection mold, and then the mold was mounted on an injection molding machine (a microinjection molding machine model TR05EH2 of Sodick corporation, japan) to perform injection molding, injection molding process parameters: melt temperature Tmelt235 ℃ and injection rate Vinj＝18cm3S, mold temperature Tmold120 ℃ and a holding pressure Ppack150MPa, dwell time tpack8s, back pressure Pback8Mpa, demolding temperature Tde＝85℃。
Researches find that the mold temperature, the melt temperature, the injection rate and the holding pressure are important process parameters in the injection molding process of the microstructure, so 5 groups of horizontal values are respectively set for the 4 process parameters, and the optimal values are selected through experiments.
The mold temperature was selected as the series of values: 80. 90, 100, 110, 120. The higher the temperature, the better the filling of the grating microstructure cavity, but the filling property decreases after the temperature exceeds 120 ℃, so 120 ℃ is selected.
The melt temperature was selected as the series of values: 190. 205, 220, 235, 250. The higher the temperature, the better the PP melt flow, but the filling of the mould cavity increases little after 235 ℃. So 235 c was chosen.
The injection rate was selected as the series of values: 10. 14, 18, 22, 26. However, it was found in experiments that the filling of the grating structure at different injection ratesThere was almost no change. So a reference value of 18cm is selected3/s。
The dwell pressure is selected from the series of values 60, 90, 120, 150, 80. The filling performance of the grating structure is increased along with the increase of the holding pressure, but the internal pressure of the cavity of the grating structure is increased due to the excessively high holding pressure. The pressure was selected to be 150MPa because it made it difficult to remove the mold and the part was likely to warp after removal of the mold.
In this embodiment, a YBM-1IH oil type mold temperature controller is used to rapidly raise and lower the temperature of the mold, and a SIC-3A type water chiller is selected to cool the injection molding machine, thereby improving the recovery of the grating structure. And after injection is finished, a grating structure color functional surface is obtained, and specific color forming effects on different observation angles are realized.
The plasticizing and metering parts of the injection molding machine in the step 3 are arranged in a Z-shaped mode, so that the plasticizing and the injection of the material can be independently realized, the metering of an injection unit is accurate and can reach 0.01mm, the control precision is high, the ejection force of the injection unit can reach 1.47KN, the maximum injection pressure can reach 200MPa, and the maximum theoretical injection amount is 4.5cm3。
The material used by the injection molding structural color is polypropylene PP.
FIG. 2 is a color reflection spectrum diagram of the grating structure of the present invention, the reflection spectrum peaks are different, showing different colors. In subsequent experiments, by observing the peak change of the reflection spectrum, the influence of different process parameters on different color developments of the structural color can be researched.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (6)
1. The preparation method of the grating structure color functional surface based on injection molding is characterized by comprising the following steps of:
step S1: preparing a silicon female die with a grating structure by adopting an ultraviolet photoetching machine and an etching machine;
step S2: conducting conductive treatment on the silicon master mold in the step S1 by using a high vacuum sputtering coating instrument, depositing a gold film conductive layer on the surface of the silicon master mold, then placing the silicon master mold in electroforming solution as a cathode to be connected with a pulse power supply cathode, and connecting a conductive nickel plate as an anode to a power supply anode to start an electroforming process, wherein the initial current of electroforming is 0.08A, the electroforming time is 30min, the later current is 0.25A, and the electroforming time is 900 min; after electroforming is finished, ultrasonically cleaning the nickel mould core by using absolute ethyl alcohol and distilled water, and fully drying the nickel mould core to obtain a nickel mould core with a grating structure on the surface;
step S3, mounting the nickel mold core prepared in the step S2 on an injection mold, and then mounting the injection mold on an injection molding machine for injection molding, wherein the injection molding process parameters are as follows: melt temperature Tmelt235 ℃ and injection rate Vinj＝18cm3S, mold temperature Tmold120 ℃ and a holding pressure Ppack150MPa, dwell time tpack8s, back pressure Pback8Mpa, demolding temperature TdeAnd obtaining the grating structure color functional surface at 85 ℃.
2. The method for preparing a functional color surface with a grating structure based on injection molding according to claim 1, wherein in the step S3, the injection molding material is polypropylene PP.
3. The method for preparing a grating structure color functional surface based on injection molding according to claim 1, wherein the step S1 is specifically performed by: processing a mask plate with a grating structure on the surface of a glass substrate; covering a layer of positive photoresist on the surface of the silicon plate, baking the positive photoresist for a period of time, and exposing the photoresist through a mask plate by using an ultraviolet photoetching machine; carrying out development and post-baking treatment on the exposed photoresist; carrying out plasma etching on the developed silicon plate by using an etching machine; and removing the photoresist which is not subjected to exposure treatment to obtain the silicon master mold with the grating structure.
4. The method for preparing a grating structure color functional surface based on injection molding according to claim 1, wherein a URE-2000135 ultraviolet lithography machine and an NLD-570 etching machine are adopted in the step S1, a LEICA EM SCD 500 high vacuum sputtering coating instrument is adopted to conduct electricity to the silicon master mold in the step S2, an YBM-1IH oil type mold temperature controller is adopted to realize temperature rise and fall of the injection mold in the step S3, and a SIC-3A water cooling machine is adopted to cool the injection molding machine.
5. The method for preparing a grating structure color function surface based on injection molding according to claim 1, wherein in step S2, the periodic stripes of the grating structure are 300-1100 nm.
6. The method for preparing a color functional surface based on an injection molded grating structure of claim 1, wherein the thickness of the gold film conductive layer in step S2 is 15-20 nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114089476A (en) * | 2021-11-25 | 2022-02-25 | Oppo广东移动通信有限公司 | Optical waveguide lens, method for preparing optical waveguide lens and augmented reality equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114089476A (en) * | 2021-11-25 | 2022-02-25 | Oppo广东移动通信有限公司 | Optical waveguide lens, method for preparing optical waveguide lens and augmented reality equipment |
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Application publication date: 20200908 |