CN110256724B - Preparation method of anti-adhesion film for photocuring continuous surface forming 3D printing - Google Patents

Preparation method of anti-adhesion film for photocuring continuous surface forming 3D printing Download PDF

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CN110256724B
CN110256724B CN201910523541.5A CN201910523541A CN110256724B CN 110256724 B CN110256724 B CN 110256724B CN 201910523541 A CN201910523541 A CN 201910523541A CN 110256724 B CN110256724 B CN 110256724B
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film
liquid
photocuring
adhesion
continuous surface
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CN110256724A (en
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段玉岗
李晓刚
康小青
李玥萱
王成萌
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Xian Jiaotong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/06—Coating with compositions not containing macromolecular substances
    • C08J7/065—Low-molecular-weight organic substances, e.g. absorption of additives in the surface of the article
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36—After-treatment
    • C08J9/40—Impregnation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36—After-treatment
    • C08J9/40—Impregnation
    • C08J9/42—Impregnation with macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2345/00—Characterised by the use of homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic ring system; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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Abstract

An anti-adhesion film preparation method for photocuring continuous surface forming 3D printing. Soaking the fluoridized porous material which is transparent to ultraviolet rays in fluoridized liquid or fluorine-containing nano-scale lubricating oil, enabling the fluoridized liquid or the fluorine-containing nano-scale lubricating oil to be fully soaked in the porous material after a period of time, and then removing redundant fluoridized liquid or fluorine-containing nano-scale lubricating oil by adopting an organic solvent. The preparation method is characterized in that a layer of stable micron-sized liquid film is formed on the surface of the porous material by utilizing the chemical compatibility of the porous material and the oleophobic phase and the capillary action of the porous material, the solid-solid bonding of the formed part and the light-transmitting porous film material is converted into the solid-liquid bonding of the formed part and the liquid oil-repellent phase, the formed part and the porous material are separated, the adhesion force between the formed part and the porous material is reduced, and the printing process can be continuously carried out.

Description

Preparation method of anti-adhesion film for photocuring continuous surface forming 3D printing
Technical Field
The invention belongs to the technical field of 3D printing, and particularly relates to a preparation method of an anti-adhesion film for photocuring continuous surface forming 3D printing.
Background
Stereo Stereolithography (SLA) was the first developed and one of the more mature additive manufacturing technologies. Through the development of many years, the traditional light-curing rapid forming technology is transited from the SLA forming mode of 'point-to-line, line-to-surface and surface-to-body' to the existing DLP forming mode of directly from 'surface-to-body', but the forming speed and the forming precision of the DLP are limited because the bonding force between a forming part and a release film is large. In recent years, the "continuous liquid interface manufacturing technology" (CLIP) developed by Carbon3D company in the united states utilizes the principle of oxygen inhibition to enable uncured liquid resin with a certain thickness to exist between the resin and the molded part, namely a "curing blind area", thereby reducing the stripping force between the molded part and the molding window, enabling the molding speed to be rapidly improved and reaching 500 mm/h. Subsequently, the technology was improved by the institute of Chinese academy of sciences, and the speed reached 650 mm/h. But there are some limitations due to CLIP technology:
(1) the forming window of the CLIP process needs to use oxygen-permeable and ultraviolet-permeable film materials, which are expensive, and the printing process needs to continuously consume oxygen, which has high requirements on equipment;
(2) because the continuous molding is realized mainly based on the principle of oxygen inhibition, the resin needs to have the oxygen inhibition effect, so that the used materials are limited;
(3) the presence of oxygen inhibition can result in the presence of hundreds of microns of uncured resin on the surface of the part, thereby affecting part performance and accuracy.
Disclosure of Invention
The invention aims to provide a preparation method of an anti-adhesion film for photocuring continuous surface forming 3D printing, which aims to solve the problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an anti-adhesion film for photocuring continuous surface forming 3D printing comprises the following steps:
step 1, fluoridizing a base material by using a fluorosilane coupling agent, soaking the base material in a liquid oleophobic material, and soaking for 0-2400 hours under the assistance of a physical field of ultrasonic oscillation, heating or microwave treatment or adhering the oleophobic material to the base material in a film coating mode;
and 2, removing the redundant liquid oleophobic material by using an organic solvent to obtain the adhesion film material.
Further, the matrix material is a light-transmitting porous organic polymer film material, a low-density organic polymer film material or an organic polymer film material with a microstructure.
Further, the matrix material is a porous polyperfluorinated ethylene film, a polytetrafluoroethylene core-hole film, an ultralow-density polyethylene film, a medium-density polyethylene film, a linear low-density polyethylene film, a cyclic olefin copolymer film or a PDMS film.
Further, the fluorosilane coupling agent is one or more mixed fluorosilane coupling agents of per (heptadecyl) fluorodecyltrimethoxysilane, per (tridecyl) fluorooctyltrimethoxysilane, per (heptadecyl) fluorodecyltriethoxysilane or per (tridecyl) fluorodecyltriethoxysilane.
Further, the liquid oleophobic material is a light-transmitting liquid material which is insoluble in the photosensitive resin.
Further, the liquid oleophobic material is fluorinated liquid, perfluoropolyether lubricating oil or silicone oil.
Further, the coating method is a soaking method, a spin coating method, a pulling method or a spraying method.
Compared with the prior art, the invention has the following technical effects:
1) by utilizing the chemical compatibility of the porous material and the oleophobic phase and the capillary action of the porous material, the fluorinated liquid or the fluorine-containing nano-scale lubricating oil can form a stable micron-scale liquid layer on the porous material, so that a micron-scale liquid film exists between the forming window and the forming part, the adhesive force between the forming part and the forming window is reduced, the whole printing process can be continuously carried out, and the use requirement of equipment is reduced;
(2) the fluorinated liquid or the fluorine-containing nano-scale lubricating oil has certain chemical stability, so the fluorinated liquid or the fluorine-containing nano-scale lubricating oil cannot be dissolved with photosensitive resin, and the anti-adhesion film can also be suitable for a continuous surface forming process of a photocuring material of a cationic or mixed photoinitiator system;
(3) because no oxygen participates in the printing process, the oxygen inhibition effect cannot exist so as not to influence the performance and the precision of the part.
Drawings
FIG. 1 is a schematic structural view of a cross section of an anti-adhesion material for a porous film according to the present invention
FIG. 2 is a schematic structural diagram of a cross section of an anti-adhesion material of a microstructured film according to the present invention
FIG. 3 is a schematic diagram of the preparation route of the anti-sticking film material of the invention
FIG. 4 is a photograph of a cross section of the anti-adhesion material of the present invention
FIG. 5 is a schematic structural view of a photo-curing continuous surface forming 3D printing device using the anti-adhesion film material of the present invention
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
The preparation method of the anti-adhesion film for the photocuring continuous surface forming 3D printing is characterized by comprising the following steps of:
step 1, fluoridizing a base material by using a fluorosilane coupling agent, soaking the base material in a liquid oleophobic material, and soaking for 0-2400 hours under the assistance of a physical field of ultrasonic oscillation, heating or microwave treatment or adhering the oleophobic material to the base material in a film coating mode;
and 2, removing the redundant liquid oleophobic material by using an organic solvent to obtain the adhesion film material.
The matrix material is a light-transmitting porous organic polymer film material, a low-density organic polymer film material or an organic polymer film material with a microstructure.
The matrix material is a porous polyperfluorinated ethylene film, a polytetrafluoroethylene core-hole film, an ultra-low density polyethylene film, a medium density polyethylene film, a linear low density polyethylene film, a cyclic olefin copolymer film or a PDMS film.
The fluorosilane coupling agent is one or more mixed fluorosilane coupling agents of per (heptadecyl) fluorodecyltrimethoxysilane, per (tridecyl) fluorooctyltrimethoxysilane, per (heptadecyl) fluorodecyltriethoxysilane or per (tridecyl) fluorodecyltriethoxysilane.
The liquid oleophobic material is a light-transmitting liquid material that is insoluble in the photosensitive resin.
The liquid oleophobic material is fluorinated liquid, perfluoropolyether lubricating oil or silicone oil.
The coating method is a soaking method, a spin-coating method, a pulling method or a spraying method.
Aiming at the problems, the invention utilizes the chemical compatibility of the porous material and the oleophobic phase and the capillary action of the porous material to form a layer of stable micron-sized liquid film on the surface of the porous material, and converts the solid-solid bonding of the formed part and the light-transmitting porous film material into the solid-liquid bonding of the formed part and the liquid oil-repellent phase, thereby reducing the bonding force between the formed part and the light-transmitting porous film material, enabling the whole printing process to be carried out continuously, realizing continuous surface forming by using the anti-adhesion film material without an oxygen inhibition principle, and having simple preparation method
Referring to fig. 1 to 4, an anti-adhesion film material for a photocuring continuous surface forming 3D printing apparatus. The anti-sticking material comprises a substrate 1 and an oleophobic phase 2, wherein the substrate 1 is a porous organic matter polymeric membrane which can transmit ultraviolet light, the oleophobic phase 2 is fluorinated liquid or fluorine-containing nano lubricating oil, and the oleophobic phase 2 is insoluble in photosensitive resin. Soaking the substrate 1 into the oleophobic phase 2, and after a period of time, fully soaking the oleophobic phase 2 into the substrate 1, and then removing the redundant lubricating oil 2 by adopting an organic solvent. The hydrophobic phase 2 is stably locked in the substrate 1 by utilizing the capillary action of the porous material.
Since the bond between the formed part and the substrate 1 is solid-to-solid, the bond between the two is large and if separated directly, the substrate 1 and the formed part may be damaged to some extent. As shown in fig. 4, in the present invention, a liquid oleophobic layer exists between the substrate 1 and the molded part to change solid-solid bonding into solid-liquid bonding, so as to reduce the bonding force between the substrate 1 and the molded part, and the molded part can be directly pulled up with a small separation force, so that the whole printing process can be continuously performed. The hydrophobic phase 2 has certain chemical stability, so that the hydrophobic phase is not dissolved with photosensitive resin, and the anti-adhesion film material can be also suitable for a continuous surface forming process of a photocuring material of a cationic or mixed photoinitiator system. In addition, in the photocuring continuous surface forming 3D printing process, the photosensitive resin is subjected to polymerization reaction under the irradiation of ultraviolet light, heat can be released in the reaction process, and the oil-repellent phase 2 is arranged between the part and the substrate 1, so that the oil-repellent phase 2 can play a role in heat insulation, and the substrate 1 is prevented from being damaged due to too high temperature in the printing process.
The present invention will be described in further detail with reference to the following examples.
Example 1
The method comprises the steps of taking a polyperfluorinated ethylene porous film with a back glue layer as a base material 1, taking perfluoropolyether lubricating oil as an oleophobic phase 2, respectively cleaning the surface of the film with acetone and deionized water, and then drying the surface with nitrogen. The film was immersed in perfluoropolyether lubricating oil and allowed to stand for 24 hours. And then taking out the film, washing off the redundant perfluoropolyether lubricating oil by using acetone, and blow-drying the surface of the film by using nitrogen to obtain the anti-adhesion film material. As shown in figure 4, when printing, the anti-adhesion film material is pasted at the bottom of the resin tank 5, the photosensitive resin 7 is solidified under the action of UV light and is adhered on the forming plate 3, and as the liquid oil-repellent phase 2 is arranged between the forming part 6 and the base material 1, the solid-solid adhesion of the forming part 6 and the base material 1 is changed into solid-liquid adhesion, so that the adhesion force is reduced, and the whole printing process can be continuously carried out.
Example 2
Referring to fig. 2, a PDMS film with a microstructure is used as a substrate 1, perfluoropolyether lubricating oil is used as an oleophobic phase 2, and per (heptadecafluorodecyltrimethoxysilane) is used as a silane coupling agent. And respectively cleaning the surface of the PDMS film by using acetone and deionized water, blow-drying the surface by using nitrogen, and then carrying out surface treatment on the PDMS film by using oxygen plasma. Then, the PDMS film was immersed in per (heptadecafluorodecyltrimethoxysilane and allowed to stand in a vacuum atmosphere for 8 hours for fluorination treatment. Excess per (heptadecafluorodecyltrimethoxysilane on PDMS film was removed with acetone, then rinsed with deionized water and blown dry with nitrogen. Then, the PDMS film is soaked in perfluoropolyether lubricating oil by a soaking film coating method, and is placed in a vacuum environment for standing for 24 hours. And then taking out the film, washing off the redundant perfluoropolyether lubricating oil by using acetone, washing by using deionized water, and blow-drying the surface of the film by using nitrogen to obtain the anti-adhesion film material.
The above-mentioned details described with reference to the drawings are merely illustrative and not intended to limit the scope of the present invention, and various modifications or variations made by those skilled in the art without inventive efforts based on the method for preparing the anti-adhesion film provided by the present invention are still within the scope of the present invention.

Claims (5)

1. The application of the anti-adhesion film in photocuring continuous surface forming 3D printing is characterized in that the preparation method of the anti-adhesion film comprises the following steps:
step 1, fluoridizing a base material by using a fluorosilane coupling agent, soaking the base material in a liquid oleophobic material, and soaking for 0-2400 hours under the assistance of a physical field of ultrasonic oscillation, heating or microwave treatment or adhering the oleophobic material to the base material in a film coating mode;
step 2, removing the redundant liquid oleophobic material by using an organic solvent to obtain an anti-adhesion thin film material;
the substrate material is a light-transmitting porous organic polymer film material, a low-density organic polymer film material or an organic polymer film material with a microstructure;
the matrix material is a porous polyperfluorinated ethylene film, a polytetrafluoroethylene core-hole film, an ultra-low density polyethylene film, a medium density polyethylene film, a linear low density polyethylene film, a cyclic olefin copolymer film or a PDMS film.
2. The use of an anti-adhesion film for photocuring continuous surface forming 3D printing according to claim 1, wherein the fluorosilane coupling agent is one or more of per (heptadecyl) fluorodecyltrimethoxysilane, per (tridecyl) fluorooctyltrimethoxysilane, per (heptadecyl) fluorodecyltriethoxysilane or per (tridecyl) fluorodecyltriethoxysilane.
3. Use of an anti-adhesion film for photocuring continuous surface modeling 3D printing according to claim 1, characterized in that the liquid oleophobic material is a light-transmissive liquid material that is insoluble in photosensitive resin.
4. Use of an anti-adhesion film for photocuring continuous surface forming 3D printing according to claim 3, wherein the liquid oleophobic material is a fluorinated liquid, perfluoropolyether lubricating oil or silicone oil.
5. The use of the anti-adhesion film for the photocuring continuous surface forming 3D printing according to claim 1, wherein the coating method is a dipping method, a spin coating method, a pulling method or a spraying method.
CN201910523541.5A 2019-06-17 2019-06-17 Preparation method of anti-adhesion film for photocuring continuous surface forming 3D printing Active CN110256724B (en)

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