CN111873587A - Release film base film for low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process and preparation method thereof - Google Patents
Release film base film for low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- 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
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- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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Abstract
The invention relates to a release film base film for a low-roughness MLCC (multilayer ceramic capacitor) process and a preparation method thereof, wherein the release film base film for the low-roughness MLCC process comprises a first layer, a second layer and a third layer, the third layer comprises 50 g of third layer modified polyester base material and 50 g of third layer surface modified material, and the third layer modified polyester base material comprises 1 g of first copolyester and 49 g of third layer polyester base material. The third layer of the invention comprises the third layer of surface modification material, which better solves the problem of high surface roughness of the film, and compared with the prior art which adopts micron-sized inorganic particles, the surface roughness of the product of the invention is reduced to 10 nm-20 nm.
Description
Technical Field
The invention belongs to the field of polyethylene terephthalate films and preparation thereof, and particularly relates to a release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process and a preparation method thereof.
Background
The polyester film material is applied to MLCC manufacturing and is used as a basic material of consumables of an MLCC manufacturing process. Because the polyester film has low roughness and heat resistance, the polyester film plays a supporting role in the MLCC production process. Many researchers in this field have adopted different methods to solve the roughness and processability of the polyester-based film surface.
The polyester film is usually a film material prepared by using polyester as a main raw material, preparing a thick sheet by an extrusion method, and stretching the thick sheet in a longitudinal direction and a transverse direction. At present, the polyester film adopts micron-sized inorganic filler, the surface performance is partially solved, but the surface roughness Ra of the product is still larger than 45nm, the warping is verified, the stiffness is low, and the problem that the product is easy to transfer after being coated with a release agent cannot meet the requirements of a small-size MLCC product of a subsequent user on the surface roughness, the warping degree, the stiffness, the high adhesion and the like of the polyester film.
Chinese patent CN201910394068.5 discloses a preparation method of a high-matte polyester film, which comprises the steps of mixing 60-70 parts of poly (215 terephthalate), 15-25 parts of polybutylene terephthalate, 10-15 parts of polyethylene naphthalate and 3-5 parts of copolymerized modified polyester, granulating, mixing with titanium dioxide, drying, stretching, forming, irradiating by ultraviolet rays, and coating.
The invention discloses a silver-plated reflective film and a preparation method thereof, and relates to the technical field of reflective films, in particular to a small-size silver-plated reflective film and a preparation method thereof. The invention aims to solve the problems of high surface roughness and low adhesive force between a silver coating and a polyester film layer in the existing silver-coated reflecting film, has poor effect and cannot effectively solve the roughness problem.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process and a preparation method thereof. The invention adopts polyester and self-made surface modified material as raw materials, the surface modified material is composed of nano inorganic material and polyester, the nano inorganic material not only has opening function, but also can reduce the surface roughness of the polyester film; the method adopts an online coating mode to reduce the roughness of the membrane surface, and the specific technical scheme of the invention is as follows:
a release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process comprises a first layer, a second layer and a third layer, wherein the third layer comprises the following components in parts by weight:
50-100 parts of third-layer modified polyester base material
0 to 50 parts by weight of third-layer surface modified material
The third layer of modified polyester base material comprises the following components in parts by weight:
1 to 20 parts by weight of a first copolyester
49-80 parts by weight of third-layer polyester base material
The molecular weight of the first copolyester is 20000-40000, the first copolyester is prepared by copolycondensation of dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the 2, 6-naphthalenedicarboxylic acid, the terephthalic acid, the isophthalic acid and the phthalic acid is (1-10): (50-80): (0-5): (0-5); the viscosity of the third layer modified polyester base stock is 0.60 dL/g-0.80 dL/g;
the third layer of surface modification material comprises the following components in parts by weight:
0.1 to 10 weight portions of nano inorganic material
15 to 40 parts by weight of second copolyester
The molecular weight of the second copolyester is 20000-30000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the terephthalic acid to the isophthalic acid to the phthalic acid is 60: (15-35): and 5, the viscosity of the third layer surface modifier is between 0.60dL/g and 0.75 dL/g.
As an improved technical scheme of the invention, the nano inorganic material comprises one or more of nano silicon dioxide, nano barium sulfate, nano aluminum oxide, nano magnesium oxide, nano titanium dioxide, nano kaolin and nano calcium carbonate.
As an improved technical scheme of the invention, the thickness of the first layer is between 0.5 and 5 microns; the thickness of the second layer is 8-40 μm; the thickness of the third layer is 0.5-5 μm.
As an improved technical scheme of the invention, the third layer of polyester base material comprises one of PET, APET and CPET, the intrinsic viscosity of the third layer of polyester base material is 0.60 dL/g-0.80 dL/g, the melting point of the third layer of polyester base material is 255-265 ℃, and the molecular weight of the third layer of polyester base material is 20000-30000.
As an improved technical scheme of the invention, the first layer comprises the following components in parts by weight:
50-90 parts by weight of first layer modified polyester base material
10-50 parts of first layer polyester master batch
The particle size of the first layer of polyester master batch is less than 2um, and the second layer of polyester master batch consists of one of PET, APET and CPET.
As an improved technical scheme of the invention, the first layer of modified polyester base stock is one of PET, APET and CPET, and the first layer of polyester master batch comprises one of PET, APET and CPET.
A method for preparing the release film base film for the low-roughness MLCC process comprises the following steps:
step S1: conveying raw materials of a first layer to a first extruder, wherein the components and parts by weight of the first layer are as follows:
50-90 parts by weight of first layer modified polyester base material
10-50 parts of first layer polyester master batch
The particle size of the first layer of polyester master batch is less than 2 um; conveying the second layer of raw materials to a second extruder; conveying the raw materials of a third layer to a third extruder, wherein the components and parts by weight of the third layer are as follows:
50-100 parts of third-layer modified polyester base material
0-50 parts by weight of a third layer of surface modification material;
step S2: the first extruder, the second extruder and the third extruder are melted at a temperature of 265-300 ℃, the extrusion thickness of the first extruder is set to be 0.5-5 μm, the extrusion thickness of the second extruder is set to be 8-40 μm, the extrusion thickness of the third extruder is set to be 0.5-5 μm, and the first extruder, the second extruder and the third extruder are used for co-extruding a first layer, a second layer and a third layer;
step S3: casting the first layer, the second layer and the third layer on a cold drum at 15-40 ℃, longitudinally stretching to 3.0-3.8 times, and cooling to 20-45 ℃;
step S4: preheating the first layer, the second layer and the third layer at 80-145 ℃, transversely stretching to 3.0-4.5 times, and then performing heat setting at 200-250 ℃;
step S5: and cooling the first layer, the second layer and the third layer at 30-35 ℃ and room temperature, and then rolling.
As an improved technical scheme of the invention, the longitudinal stretching is carried out on a longitudinal stretching section, the length of the longitudinal stretching section is between 3m and 5m, the temperature is between 65 ℃ and 90 ℃, the transverse stretching is carried out on a transverse stretching section, the length of the transverse stretching section is between 10m and 16m, the temperature is between 100 ℃ and 160 ℃, the heat setting is carried out on a heat setting section, and the length of the heat setting section is between 10m and 20 m.
In step S1, the modified polyester base material of the third layer comprises the following components in parts by weight:
1 to 20 parts by weight of a first copolyester
49-80 parts by weight of third-layer polyester base material
The third layer of surface modification material comprises the following components in parts by weight:
0.1 to 10 weight portions of nano inorganic material
15 to 40 parts by weight of second copolyester
The first layer of modified polyester base material is one of PET, APET and CPET, the first layer of polyester master batch comprises one of PET, APET and CPET, and the second layer of raw material is one of PET, APET and CPET.
As an improved technical scheme of the invention, the third layer of polyester base material comprises one of PET, APET and CPET; the molecular weight of the first copolyester is 20000-40000, the first copolyester is prepared by copolycondensation of dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the 2, 6-naphthalenedicarboxylic acid to the terephthalic acid to the isophthalic acid to the phthalic acid is (1-10): (50-80): (0-5): (0-5); the molecular weight of the second copolyester is 20000-30000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the terephthalic acid, the isophthalic acid and the phthalic acid is 60: (15-35): 5.
advantageous effects
(1) The third layer of the invention comprises a third layer of surface modification material, the third layer of surface modification material comprises 0.1 to 10 weight portions of nano inorganic material and 15 to 40 weight portions of second copolyester, the nano inorganic material is uniformly distributed on the surface of the film, and the problem of high roughness of the surface of the film is better solved because the particle size is small and the protruding height is small, compared with the existing method adopting micron-sized inorganic particles, the surface roughness is reduced to 10 to 20 nm;
(2) the first layer comprises 50-90 parts by weight of first layer modified polyester base stock and 10-50 parts by weight of first layer polyester master batch, the particle size of the first layer polyester master batch is below 2um, and the master batch is distributed on a non-processing surface, so that the stability of the opening performance and the good rolling operability of the product in the processing and using processes are ensured;
(3) the second layer of the invention adopts modified polyester base stock, which is mainly characterized in that the modified base stock contains a molecular chain segment with strong rigidity, thereby improving the stiffness of the film and effectively solving the problems of high warping degree and low stiffness of the film;
(4) the preparation process disclosed by the invention is simple and convenient, easy to operate, strong in practicability and low in cost.
Detailed Description
In order to make the purpose and technical solutions of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
A release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process comprises a first layer, a second layer and a third layer, wherein the third layer comprises the following components in parts by weight:
the third layer of modified polyester base material is 50 g
Third layer surface modified material 50 g
The third layer of surface modification material comprises the following components in parts by weight:
nano inorganic material 10 g
Second copolyester 40 g
In the embodiment, the third layer comprises a third layer surface modification material, the third layer surface modification material comprises a nano inorganic material and second copolyester, the nano inorganic material is uniformly distributed on the surface of the film, and the problem of high surface roughness of the film is better solved due to small particle size and small protruding height, and compared with the existing method adopting micron-sized inorganic particles, the surface roughness is reduced to 10 nm;
the molecular weight of the second copolyester is 20000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, the terephthalic acid is 60 g, the isophthalic acid is 15 g and the phthalic acid is 5 g, and the viscosity of the surface modification material of the third layer is 0.60 dL/g.
The nano inorganic material comprises one or more of nano silicon dioxide.
The third layer of modified polyester base material comprises the following components in parts by weight:
first copolyester 1 g
Third layer polyester base 49 g
The molecular weight of the first copolyester is 20000, the first copolyester is prepared by copolycondensating dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid and terephthalic acid, the 2, 6-naphthalenedicarboxylic acid is 10 g, and the terephthalic acid is 500 g; the viscosity of the third layer modified polyester base stock is 0.60 dL/g;
the thickness of the first layer is 0.5 μm; the thickness of the second layer is 8 μm; the thickness of the third layer was 0.5 μm. The first layer comprises the following components in parts by weight:
first layer modified polyester base material 50 g
First layer polyester masterbatch 10 g
The particle size of first layer polyester masterbatch is 2um, the second layer comprises PET. In the embodiment, the second layer adopts the modified polyester base material, and the modified base material mainly contains a molecular chain segment with strong rigidity, so that the stiffness of the film is improved, and the problems of high warping degree and low stiffness of the film are effectively solved;
the first layer of modified polyester base stock is PET, and the first layer of polyester master batch is PET. The first layer comprises a first layer of modified polyester base material and a first layer of polyester master batch, the particle size of the first layer of polyester master batch is 2 microns, and the master batch is distributed on a non-processing surface, so that the stability of the opening performance and the good rolling operability of the product in the processing and using processes are ensured;
the third layer of polyester base material is PET, the intrinsic viscosity of the third layer of polyester base material is 0.60dL/g, the melting point of the third layer of polyester base material is 255 ℃, and the molecular weight of the third layer of polyester base material is 20000.
A method for preparing the release film base film for the low-roughness MLCC process comprises the following steps:
step S1: conveying raw materials of a first layer to a first extruder, wherein the components and parts by weight of the first layer are as follows:
first layer modified polyester base material 50 g
First layer polyester masterbatch 10 g
The particle size of the first layer of polyester master batch is 2 um; conveying the second layer of feedstock to a second extruder; conveying the raw materials of a third layer to a third extruder, wherein the components and the parts by weight of the third layer are as follows:
the third layer of modified polyester base material is 50 g
50 g of surface modification material of the third layer;
step S2: the first, second and third extruders melt at a temperature of 265 ℃, the first extruder has an extrusion thickness of 0.5 μm, the second extruder has an extrusion thickness of 8 μm, the third extruder has an extrusion thickness of 0.5 μm, and the first, second and third extruders co-extrude a first layer, a second layer and a third layer;
step S3: casting the first layer, the second layer and the third layer on a cold drum at 15 ℃, longitudinally stretching to 3.0 times, and cooling to 20 ℃;
step S4: preheating the first layer, the second layer and the third layer at 80 ℃, transversely stretching to 3.0 times, and performing heat setting at 200 ℃;
step S5: and the first layer, the second layer and the third layer are cooled at 30 ℃ and room temperature, and then are rolled.
Longitudinal stretching is drawn at longitudinal stretching section and is gone on, longitudinal stretching section's length is 3m, and the temperature is 65 ℃, transverse stretching is gone on transverse stretching section, transverse stretching section's length is 10m, the temperature is 100 ℃, heat setting is gone on heat setting section, heat setting section's length is 10 m.
In the step S1, the components and parts by weight of the third layer modified polyester base material are as follows:
first copolyester 1 g
Third layer polyester base 49 g
The third layer of surface modification material comprises the following components in parts by weight:
nano inorganic material 10 g
Second copolyester 40 g
The first layer of modified polyester base material is PET, the first layer of polyester master batch is PET, and the second layer of raw material is PET.
The third layer of polyester base material is PET; the molecular weight of the first copolyester is 20000, the first copolyester is prepared by copolycondensating dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid and terephthalic acid, the 2, 6-naphthalenedicarboxylic acid is 10 g, and the terephthalic acid is 500 g; the molecular weight of the second copolyester is 20000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is formed by mixing terephthalic acid, isophthalic acid and phthalic acid, the terephthalic acid is 60 g, the isophthalic acid is 15 g and the phthalic acid is 5 g. The preparation process disclosed by the embodiment is simple and convenient, easy to operate, high in practicability and low in cost.
Example 2
A release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process comprises a first layer, a second layer and a third layer, wherein the third layer comprises the following components in parts by weight:
the third layer modified polyester base material is 100 g
In the embodiment, the third layer comprises the third modified polyester base material, so that the problem of high surface roughness of the film is solved, and compared with the existing method adopting micron-sized inorganic particles, the surface roughness is reduced to 10 nm.
The third layer of modified polyester base material comprises the following components in parts by weight:
first copolyester 20 g
Third layer polyester base material 80 g
The molecular weight of the first copolyester is 40000, the dicarboxylic acids include 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, the 2, 6-naphthalenedicarboxylic acid is 10 g, the terephthalic acid is 80 g, the isophthalic acid is 5 g and the phthalic acid is 5 g; the viscosity of the third layer modified polyester base stock is 0.80 dL/g;
the thickness of the first layer is 5 μm; the thickness of the second layer is 40 μm; the thickness of the third layer is 5 μm. The first layer comprises the following components in parts by weight:
first layer modified polyester base material 90 g
First layer polyester masterbatch 50 g
The particle size of first layer polyester masterbatch is 1.5um, the second layer comprises APET. In the embodiment, the second layer adopts the modified polyester base material, and the modified base material mainly contains a molecular chain segment with strong rigidity, so that the stiffness of the film is improved, and the problems of high warping degree and low stiffness of the film are effectively solved;
the first layer of modified polyester base material is APET, and the first layer of polyester master batch is APET. The first layer comprises a first layer of modified polyester base material and a first layer of polyester master batch, the particle size of the first layer of polyester master batch is 1.5 mu m, and the master batch is distributed on a non-processing surface, so that the stability of the opening performance and the good rolling operability of the product in the processing and using processes are ensured;
the third layer of polyester base material is APET, the intrinsic viscosity of the third layer of polyester base material is 0.80dL/g, the melting point of the third layer of polyester base material is 265 ℃, and the molecular weight of the third layer of polyester base material is 30000.
A method for preparing the release film base film for the low-roughness MLCC process comprises the following steps:
step S1: conveying raw materials of a first layer to a first extruder, wherein the components and parts by weight of the first layer are as follows:
first layer modified polyester base material 90 g
First layer polyester masterbatch 50 g
The particle size of the first layer of polyester master batch is 1.5 um; conveying the second layer of raw materials to a second extruder; conveying the raw materials of a third layer to a third extruder, wherein the components and parts by weight of the third layer are as follows:
the third layer modified polyester base material is 100 g
Step S2: the first extruder, the second extruder and the third extruder are melted at a temperature of 300 ℃, the extrusion thickness of the first extruder is set to be 5 μm, the extrusion thickness of the second extruder is set to be 40 μm, the extrusion thickness of the third extruder is set to be 5 μm, and the first extruder, the second extruder and the third extruder co-extrude a first layer, a second layer and a third layer;
step S3: casting the first layer, the second layer and the third layer on a cold drum at 40 ℃, longitudinally stretching to 3.8 times, and cooling to 45 ℃;
step S4: preheating the first layer, the second layer and the third layer at 145 ℃, transversely stretching to 4.5 times, and performing heat setting at 250 ℃;
step S5: and the first layer, the second layer and the third layer are cooled at 35 ℃ and room temperature, and then are rolled.
Longitudinal stretching is drawn at longitudinal stretching section and is gone on, longitudinal stretching section's length is 5m, and the temperature is 90 ℃, transverse stretching is gone on transverse stretching section, transverse stretching section's length is 16m, the temperature is 160 ℃, heat setting is gone on heat setting section, heat setting section's length is 20 m.
In the step S1, the components and parts by weight of the third layer modified polyester base material are as follows:
first copolyester 20 g
Third layer polyester base material 80 g
The first layer of modified polyester base material is APET, the first layer of polyester master batch is APET, and the second layer of raw material is APET.
The third layer of polyester base material is APET; the molecular weight of the first copolyester is 40000, the first copolyester is prepared by copolycondensating dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalene dicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, the 2, 6-naphthalene dicarboxylic acid is 10 g, the terephthalic acid is 80 g, the isophthalic acid is 5 g and the phthalic acid is 5 g. The preparation process disclosed by the embodiment is simple and convenient, easy to operate, high in practicability and low in cost.
Example 3
A release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process comprises a first layer, a second layer and a third layer, wherein the third layer comprises the following components in parts by weight:
the third layer of modified polyester base material is 80 g
Third layer surface modified material 20 g
The third layer of surface modification material comprises the following components in parts by weight:
nano inorganic material 5 g
Second copolyester 15 g
In the embodiment, the third layer comprises a third layer surface modification material, the third layer surface modification material comprises a nano inorganic material and second copolyester, the nano inorganic material is uniformly distributed on the surface of the film, and the problem of high surface roughness of the film is better solved due to small particle size and small protruding height, and compared with the existing method adopting micron-sized inorganic particles, the surface roughness is reduced to 20 nm;
the molecular weight of the second copolyester is 30000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, the terephthalic acid is 60 g, the isophthalic acid is 35 g and the phthalic acid is 5 g, and the viscosity of the surface modification material of the third layer is 0.75 dL/g.
The nano inorganic material comprises nano magnesium oxide, nano titanium dioxide, nano kaolin and nano calcium carbonate.
The third layer of modified polyester base material comprises the following components in parts by weight:
first copolyester 15 g
Third layer polyester base 65 g
The molecular weight of the first copolyester is 30000, the first copolyester is prepared by copolycondensating dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, the 2, 6-naphthalenedicarboxylic acid is 5 g, the terephthalic acid is 60 g, the isophthalic acid is 3 g and the phthalic acid is 3 g; the viscosity of the third layer modified polyester base stock is 0.70 dL/g;
the thickness of the first layer is 3 μm; the thickness of the second layer is 20 μm; the thickness of the third layer was 3 μm. The first layer comprises the following components in parts by weight:
first layer modified polyester base material 70 g
First layer polyester masterbatch 30 g
The particle size of the first layer of polyester master batch is 1.5um, and the second layer is composed of CPET. In the embodiment, the second layer adopts the modified polyester base material, and the modified base material mainly contains a molecular chain segment with strong rigidity, so that the stiffness of the film is improved, and the problems of high warping degree and low stiffness of the film are effectively solved;
the first layer of modified polyester base material is CPET, and the first layer of polyester master batch is CPET. The first layer comprises a first layer of modified polyester base material and a first layer of polyester master batch, the particle size of the first layer of polyester master batch is 1.5 mu m, and the master batch is distributed on a non-processing surface, so that the stability of the opening performance and the good rolling operability of the product in the processing and using processes are ensured;
the third layer of polyester base material is CPET, the intrinsic viscosity of the third layer of polyester base material is 0.80dL/g, the melting point of the third layer of polyester base material is 260 ℃, and the molecular weight of the third layer of polyester base material is 25000.
A method for preparing the release film base film for the low-roughness MLCC process comprises the following steps:
step S1: conveying raw materials of a first layer to a first extruder, wherein the components and parts by weight of the first layer are as follows:
first layer modified polyester base material 70 g
First layer polyester masterbatch 30 g
The particle size of the first layer of polyester master batch is 1.5 um; conveying the second layer of raw materials to a second extruder; conveying the raw materials of a third layer to a third extruder, wherein the components and parts by weight of the third layer are as follows:
the third layer of modified polyester base material is 80 g
20 g of surface modification material of the third layer;
step S2: the first extruder, the second extruder and the third extruder are melted at a temperature of 280 ℃, the extrusion thickness of the first extruder is set to be 3 μm, the extrusion thickness of the second extruder is set to be 20 μm, the extrusion thickness of the third extruder is set to be 3 μm, and the first extruder, the second extruder and the third extruder co-extrude a first layer, a second layer and a third layer;
step S3: casting the first layer, the second layer and the third layer on a cold drum at 20 ℃, longitudinally stretching to 3.5 times, and cooling to 40 ℃;
step S4: preheating the first layer, the second layer and the third layer at 100 ℃, transversely stretching to 4.0 times, and performing heat setting at 220 ℃;
step S5: and the first layer, the second layer and the third layer are cooled at 32 ℃ and room temperature, and then are rolled.
Longitudinal stretching is drawn at longitudinal stretching section and is gone on, longitudinal stretching section's length is 4m, and the temperature is 80 ℃, transverse stretching is gone on transverse stretching section, transverse stretching section's length is 12m, the temperature is 130 ℃, heat setting is gone on heat setting section, heat setting section's length is 12 m.
In the step S1, the components and parts by weight of the third layer modified polyester base material are as follows:
first copolyester 15 g
Third layer polyester base 65 g
The third layer of surface modification material comprises the following components in parts by weight:
nano inorganic material 5 g
Second copolyester 15 g
The first layer of modified polyester base material is CPET, the first layer of polyester master batch is CPET, and the second layer of raw material is CPET.
The third layer of polyester base material is CPET; the molecular weight of the first copolyester is 30000, the dicarboxylic acids include 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, the 2, 6-naphthalenedicarboxylic acid is 5 g, the terephthalic acid is 60 g, the isophthalic acid is 3 g and the phthalic acid is 3 g; the molecular weight of the second copolyester is 25000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, the terephthalic acid is 60 g, the isophthalic acid is 35 g and the phthalic acid is 5 g. The preparation process disclosed by the embodiment is simple and convenient, easy to operate, high in practicability and low in cost.
Example 4
A release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process comprises a first layer, a second layer and a third layer, wherein the third layer comprises the following components in parts by weight:
the third layer of modified polyester base material is 80 g
Third layer surface modified material 20 g
The third layer of surface modification material comprises the following components in parts by weight:
nano inorganic material 0.1 g
Second copolyester 19.9 g
In the embodiment, the third layer comprises a third layer surface modification material, the third layer surface modification material comprises a nano inorganic material and second copolyester, the nano inorganic material is uniformly distributed on the surface of the film, and the problem of high surface roughness of the film is better solved due to small particle size and small protruding height, and compared with the existing method adopting micron-sized inorganic particles, the surface roughness is reduced to 20 nm;
the molecular weight of the second copolyester is 25000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, the terephthalic acid is 60 g, the isophthalic acid is 20 g and the phthalic acid is 5 g, and the viscosity of the surface modification material of the third layer is 0.65 dL/g.
The nano inorganic material comprises nano barium sulfate and nano aluminum oxide.
The third layer of modified polyester base material comprises the following components in parts by weight:
first copolyester 15 g
Third layer polyester base 65 g
The molecular weight of the first copolyester is 25000, the first copolyester is prepared by copolycondensation of dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, the 2, 6-naphthalenedicarboxylic acid is 5 g, the terephthalic acid is 60 g, the isophthalic acid is 3 g and the phthalic acid is 3 g; the viscosity of the third layer modified polyester base stock is 0.70 dL/g;
the thickness of the first layer is 3 μm; the thickness of the second layer is 20 μm; the thickness of the third layer was 3 μm. The first layer comprises the following components in parts by weight:
first layer modified polyester base material 70 g
First layer polyester masterbatch 30 g
The particle size of the first layer of polyester master batch is 1.5um, and the second layer is composed of CPET. In the embodiment, the second layer adopts the modified polyester base material, and the modified base material mainly contains a molecular chain segment with strong rigidity, so that the stiffness of the film is improved, and the problems of high warping degree and low stiffness of the film are effectively solved;
the first layer of modified polyester base material is CPET, and the first layer of polyester master batch is CPET. The first layer comprises a first layer of modified polyester base material and a first layer of polyester master batch, the particle size of the first layer of polyester master batch is 1.5 mu m, and the master batch is distributed on a non-processing surface, so that the stability of the opening performance and the good rolling operability of the product in the processing and using processes are ensured;
the third layer of polyester base material is CPET, the intrinsic viscosity of the third layer of polyester base material is 0.80dL/g, the melting point of the third layer of polyester base material is 260 ℃, and the molecular weight of the third layer of polyester base material is 25000.
A method for preparing the release film base film for the low-roughness MLCC process comprises the following steps:
step S1: conveying raw materials of a first layer to a first extruder, wherein the components and parts by weight of the first layer are as follows:
first layer modified polyester base material 70 g
First layer polyester masterbatch 30 g
The particle size of the first layer of polyester master batch is 1.5 um; conveying the second layer of raw materials to a second extruder; conveying the raw materials of a third layer to a third extruder, wherein the components and parts by weight of the third layer are as follows:
the third layer of modified polyester base material is 80 g
20 g of surface modification material of the third layer;
step S2: the first extruder, the second extruder and the third extruder are melted at a temperature of 280 ℃, the extrusion thickness of the first extruder is set to be 3 μm, the extrusion thickness of the second extruder is set to be 20 μm, the extrusion thickness of the third extruder is set to be 3 μm, and the first extruder, the second extruder and the third extruder co-extrude a first layer, a second layer and a third layer;
step S3: casting the first layer, the second layer and the third layer on a cold drum at 20 ℃, longitudinally stretching to 3.5 times, and cooling to 40 ℃;
step S4: preheating the first layer, the second layer and the third layer at 100 ℃, transversely stretching to 4.0 times, and performing heat setting at 220 ℃;
step S5: and the first layer, the second layer and the third layer are cooled at 32 ℃ and room temperature, and then are rolled.
Longitudinal stretching is drawn at longitudinal stretching section and is gone on, longitudinal stretching section's length is 4m, and the temperature is 80 ℃, transverse stretching is gone on transverse stretching section, transverse stretching section's length is 12m, the temperature is 130 ℃, heat setting is gone on heat setting section, heat setting section's length is 12 m.
In the step S1, the components and parts by weight of the third layer modified polyester base material are as follows:
first copolyester 15 g
Third layer polyester base 65 g
The third layer of surface modification material comprises the following components in parts by weight:
nano inorganic material 0.1 g
Second copolyester 19.9 g
The first layer of modified polyester base material is CPET, the first layer of polyester master batch is CPET, and the second layer of raw material is CPET.
The third layer of polyester base material is CPET; the molecular weight of the first copolyester is 25000, the dicarboxylic acids comprise 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, the 2, 6-naphthalenedicarboxylic acid is 5 g, the terephthalic acid is 60 g, the isophthalic acid is 3 g and the phthalic acid is 3 g; the molecular weight of the second copolyester is 25000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, the terephthalic acid is 60 g, the isophthalic acid is 20 g and the phthalic acid is 5 g. The preparation process disclosed by the embodiment is simple and convenient, easy to operate, high in practicability and low in cost.
Comparative example 1
A release film base film for an MLCC manufacturing process is of a three-layer structure, wherein a first layer is the same as a third layer.
The first layer and the third layer comprise the following components in parts by weight:
polyester base 80 g
Polyester masterbatch 20 g
The polyester base material can be FG600 and FG604 base material type film grade polyester chips provided by China petrochemical and chemical fiber GmbH, and CZ-5011 super bright polyester chips provided by Jiangsu three-alley group GmbH, and has the intrinsic viscosity of 0.62-0.68 dL/g, the melting point of 255-265 ℃ and the molecular weight of 20000-30000.
The polyester master batch consists of inorganic filler and polyester base material, wherein the particle size of the inorganic filler is 2-3.5 um, and the content is 3000-6000 ppm. The inorganic filler is one or more of silicon dioxide, barium sulfate and calcium carbonate.
The second layer adopts polyester base material.
A method for preparing the release film base film for the low-roughness MLCC process comprises the following steps.
Respectively drying the first layer raw material, the third layer raw material and the second layer raw material at 165-175 ℃ for 4-6 h, then respectively entering a single-screw extruder and a double-screw extruder for melting, mixing in a melting way, extruding through a three-layer co-extrusion die head in an A-B-A mode, wherein the extrusion temperature is 275-285 ℃, and cooling through a casting sheet roller at 20-40 ℃ to form 1.5-1.8 m casting sheets; the cast sheet is heated to 80-90 ℃ through a preheating roller and then enters a longitudinal stretching system, a unidirectional sheet is formed after being stretched at a rate of 2.8-3.8, the unidirectional sheet is heated to 100-120 ℃ through a transverse stretching preheating area and then enters a transverse stretching system, the stretching temperature is 120-135 ℃, the stretching rate is 3-4 times, the stretched film is subjected to processes of heat setting at 225-250 ℃ and cooling at 50-70 ℃ in sequence, then the stretched film can be wound into a large-shaft product through a winding machine, and the large-shaft product is cut into a specified specification through a splitting machine, so that the release film polyester base film for the MLCC process is prepared.
Table 1: the typical technical indexes of the release film for the low roughness MLCC process of each embodiment and comparative example are compared.
The roughness testing method comprises the following steps: the sample is made into A4(210mm multiplied by 297mm), then the sample to be tested is placed on black glass (roughness Ra is less than 2nm) to ensure that the sample to be tested is flat and clean without residual air aggregation, a Mahr roughness tester is used for testing, the average values of Ra, Rz and Rmax are taken after 10 times of parallel testing.
The friction coefficient test method comprises the following steps: preparing a sample to be tested into a slide way sample (10cm multiplied by 27cm) and a slide block sample (6.3cm multiplied by 8cm), enabling the test surface of the slide way sample to be upward, flatly paving the slide way sample on a slide way aluminum plate, and fixing the right side edge part of the slide way sample by using a clamp; fixing the slide block sample on the slide block by using an adhesive tape, wherein the test surface is contacted with the plastic surface of the slide block; the test was carried out using a GM-1 Friction coefficient tester. The replicates were tested 5 times and μ s, μ k, mean values were taken.
The warping degree test method comprises the following steps: a sample to be tested is prepared into A4 size, then the sample is tiled and put into an oven for 30min at 150 ℃, the relative humidity is 45-55 percent at the temperature of 23 +/-2 ℃, and the MD/TD is tested by a steel plate ruler (the precision is 0.1mm) or a plug gauge after the sample is tiled and put on a glass substrate for 30 min. Reference may be made to the GB/T25257-2010 detection standard.
The stiffness testing method comprises the following steps: making a sample to be tested into 70mm multiplied by 38mm, testing MD/TD by adopting a stiffness tester at an included angle of 15 degrees, testing in parallel for 5 times, and taking an average value.
The above are merely embodiments of the present invention, which are described in detail and with particularity, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the spirit of the invention, and these are within the scope of the invention.
Claims (10)
1. A release film base film for a low-roughness MLCC (multilayer ceramic chip carrier) manufacturing process comprises a first layer, a second layer and a third layer, and is characterized in that the third layer comprises the following components in parts by weight:
50-100 parts of third-layer modified polyester base material
0 to 50 parts by weight of third-layer surface modified material
The third layer of modified polyester base material comprises the following components in parts by weight:
1 to 20 parts by weight of a first copolyester
49-80 parts by weight of third-layer polyester base material
The molecular weight of the first copolyester is 20000-40000, the first copolyester is prepared by copolycondensation of dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the 2, 6-naphthalenedicarboxylic acid, the terephthalic acid, the isophthalic acid and the phthalic acid is (1-10): (50-80): (0-5): (0-5); the viscosity of the third layer modified polyester base stock is 0.60 dL/g-0.80 dL/g;
the third layer of surface modification material comprises the following components in parts by weight:
0.1 to 10 weight portions of nano inorganic material
15 to 40 parts by weight of second copolyester
The molecular weight of the second copolyester is 20000-30000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the terephthalic acid to the isophthalic acid to the phthalic acid is 60: (15-35): and 5, the viscosity of the third layer surface modifier is between 0.60dL/g and 0.75 dL/g.
2. The release film base film for the low roughness MLCC process according to claim 1, wherein the nano inorganic material comprises one or more of nano silicon dioxide, nano barium sulfate, nano aluminum oxide, nano magnesium oxide, nano titanium dioxide, nano kaolin, and nano calcium carbonate.
3. The release film-based film for the low roughness MLCC process according to claim 1, wherein the thickness of the first layer is between 0.5 μm and 5 μm; the thickness of the second layer is 8-40 μm; the thickness of the third layer is 0.5-5 μm.
4. The release film-based film for the low roughness MLCC process according to claim 1, wherein the third layer polyester base material comprises one of PET, APET and CPET, the intrinsic viscosity of the third layer polyester base material is 0.60dL/g to 0.80dL/g, the melting point of the third layer polyester base material is 255 ℃ to 265 ℃, and the molecular weight of the third layer polyester base material is 20000 to 30000.
5. The release film base film for the low roughness MLCC process according to claim 1, wherein the first layer comprises the following components in parts by weight:
50-90 parts by weight of first layer modified polyester base material
10-50 parts of first layer polyester master batch
The particle size of the first layer of polyester master batch is less than 2um, and the second layer of polyester master batch consists of one of PET, APET and CPET.
6. The release film base film for the low roughness MLCC process according to claim 5, wherein the first layer modified polyester base material is one of PET, APET and CPET, and the first layer polyester master batch comprises one of PET, APET and CPET.
7. A method for preparing the release film base film for the low roughness MLCC process as claimed in any one of claims 1 to 6, which comprises the following steps:
step S1: conveying raw materials of a first layer to a first extruder, wherein the components and parts by weight of the first layer are as follows:
50-90 parts by weight of first layer modified polyester base material
10-50 parts of first layer polyester master batch
The particle size of the first layer of polyester master batch is less than 2 um; conveying the second layer of raw materials to a second extruder; conveying the raw materials of a third layer to a third extruder, wherein the components and parts by weight of the third layer are as follows:
50-100 parts of third-layer modified polyester base material
0-50 parts by weight of a third layer of surface modification material;
step S2: the first extruder, the second extruder and the third extruder are melted at a temperature of 265-300 ℃, the extrusion thickness of the first extruder is set to be 0.5-5 μm, the extrusion thickness of the second extruder is set to be 8-40 μm, the extrusion thickness of the third extruder is set to be 0.5-5 μm, and the first extruder, the second extruder and the third extruder are used for co-extruding a first layer, a second layer and a third layer;
step S3: casting the first layer, the second layer and the third layer on a cold drum at 15-40 ℃, longitudinally stretching to 3.0-3.8 times, and cooling to 20-45 ℃;
step S4: preheating the first layer, the second layer and the third layer at 80-145 ℃, transversely stretching to 3.0-4.5 times, and then performing heat setting at 200-250 ℃;
step S5: and cooling the first layer, the second layer and the third layer at 30-35 ℃ and room temperature, and then rolling.
8. The process according to claim 7, characterized in that the longitudinal stretching is carried out in a longitudinal stretching section having a length of between 3m and 5m and a temperature of between 65 ℃ and 90 ℃, the transverse stretching is carried out in a transverse stretching section having a length of between 10m and 16m and a temperature of between 100 ℃ and 160 ℃, the heat setting is carried out in a heat setting section having a length of between 10m and 20 m.
9. The method of claim 7, wherein in the step S1, the composition and weight parts of the third layer modified polyester base material are as follows:
1 to 20 parts by weight of a first copolyester
49-80 parts by weight of third-layer polyester base material
The third layer of surface modification material comprises the following components in parts by weight:
0.1 to 10 weight portions of nano inorganic material
15 to 40 parts by weight of second copolyester
The first layer of modified polyester base material is one of PET, APET and CPET, the first layer of polyester master batch comprises one of PET, APET and CPET, and the second layer of raw material is one of PET, APET and CPET.
10. The method of claim 9, wherein the third layer of polyester substrate comprises one of PET, APET, CPET; the molecular weight of the first copolyester is 20000-40000, the first copolyester is prepared by copolycondensation of dicarboxylic acid and ethylene glycol, the dicarboxylic acid comprises 2, 6-naphthalenedicarboxylic acid, terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the 2, 6-naphthalenedicarboxylic acid, the terephthalic acid, the isophthalic acid and the phthalic acid is (1-10): (50-80): (0-5): (0-5); the molecular weight of the second copolyester is 20000-30000, the second copolyester is prepared by copolycondensation of phthalic acid and ethylene glycol, the phthalic acid is prepared by mixing terephthalic acid, isophthalic acid and phthalic acid, and the weight ratio of the terephthalic acid to the isophthalic acid to the phthalic acid is 60: (15-35): 5.
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| CN113172854A (en) * | 2021-05-18 | 2021-07-27 | 山东胜通光学材料科技有限公司 | Preparation method of MLCC polyester base film for 5G communication |
| CN113524848A (en) * | 2021-07-19 | 2021-10-22 | 江苏裕兴薄膜科技股份有限公司 | Low-roughness release film base film and preparation method thereof |
| CN114407468A (en) * | 2021-12-28 | 2022-04-29 | 常州钟恒新材料股份有限公司 | MLCC release film base film and preparation method thereof |
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| CN107915960A (en) * | 2017-11-17 | 2018-04-17 | 江苏东材新材料有限责任公司 | A kind of ultra low surface roughness polyester base film/compound substrate membranes and preparation method thereof |
| CN109159514A (en) * | 2018-09-04 | 2019-01-08 | 安徽国风塑业股份有限公司 | A kind of high compound fastness carbon ribbon biaxially oriented polyester film and preparation method thereof |
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| CN107915960A (en) * | 2017-11-17 | 2018-04-17 | 江苏东材新材料有限责任公司 | A kind of ultra low surface roughness polyester base film/compound substrate membranes and preparation method thereof |
| CN109159514A (en) * | 2018-09-04 | 2019-01-08 | 安徽国风塑业股份有限公司 | A kind of high compound fastness carbon ribbon biaxially oriented polyester film and preparation method thereof |
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| CN113172854A (en) * | 2021-05-18 | 2021-07-27 | 山东胜通光学材料科技有限公司 | Preparation method of MLCC polyester base film for 5G communication |
| CN113524848A (en) * | 2021-07-19 | 2021-10-22 | 江苏裕兴薄膜科技股份有限公司 | Low-roughness release film base film and preparation method thereof |
| CN114407468A (en) * | 2021-12-28 | 2022-04-29 | 常州钟恒新材料股份有限公司 | MLCC release film base film and preparation method thereof |
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