CN114874595A - High-temperature glue-resistant PBT (polybutylene terephthalate) separation membrane for FPC (flexible printed circuit) laminating process and processing process thereof - Google Patents

High-temperature glue-resistant PBT (polybutylene terephthalate) separation membrane for FPC (flexible printed circuit) laminating process and processing process thereof Download PDF

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CN114874595A
CN114874595A CN202210584647.8A CN202210584647A CN114874595A CN 114874595 A CN114874595 A CN 114874595A CN 202210584647 A CN202210584647 A CN 202210584647A CN 114874595 A CN114874595 A CN 114874595A
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percent
pbt
temperature
separation membrane
percentage
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牛军强
陈百怀
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Jiuyu Electronic Technology Jiangsu Co ltd
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Jiuyu Electronic Technology Jiangsu Co ltd
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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
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B29C48/08—Flat, e.g. panels flexible, e.g. films
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B29C48/22—Articles comprising two or more components, e.g. co-extruded layers the components being layers with means connecting the layers, e.g. tie layers or undercuts
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/285—Feeding the extrusion material to the extruder
    • B29C48/287—Raw material pre-treatment while feeding
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • 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
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
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    • B32B27/00—Layered products comprising a layer of synthetic resin
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2007/00—Flat articles, e.g. films or sheets
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/71—Resistive to light or to UV
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/744—Non-slip, anti-slip
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/746—Slipping, anti-blocking, low friction
    • 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
    • B32B2457/00—Electrical equipment
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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
    • 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
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    • 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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    • C08J2423/02—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
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    • C08J2423/02—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
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    • C08J2423/08—Copolymers of ethene
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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    • C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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    • C08K3/20—Oxides; Hydroxides
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
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Abstract

The invention discloses a high-temperature glue-resistant PBT separation membrane for an FPC (flexible printed circuit) laminating process and a processing process thereof, wherein the high-temperature glue-resistant PBT separation membrane comprises an inner layer and two outer layers, wherein the outer layers comprise PBT, a composite antioxidant, white oil, a first modifier and polytetrafluoroethylene; the inner layer comprises PBT, compatilizer, EVA, composite antioxidant, modifier II and LDPE. According to the invention, the polytetrafluoroethylene micropowder is added to modify PBT, so that the high temperature and high lubricity of the separation membrane are improved; ABS-g-GMA modifies PBT to improve impact strength and elongation at break; the graphene oxide is grafted to the polytetrafluoroethylene under the treatment of the KH560 silane coupling agent, so that the mechanical property and the friction coefficient are improved; blending modification treatment is carried out on LDPE by nano zinc oxide and a nucleating agent NX8000K, so that the ultraviolet shielding effect and the impact strength are improved; the separation membrane has good heat resistance, excellent mold release performance, good filling performance and low pollution.

Description

High-temperature glue-resistant PBT (polybutylene terephthalate) separation membrane for FPC (flexible printed circuit) laminating process and processing process thereof
Technical Field
The invention relates to the technical field of flexible circuit boards, in particular to a high-temperature glue-resistant PBT separation membrane for an FPC (flexible printed circuit) laminating process and a processing process thereof.
Background
The FPC is also called a flexible printed circuit board, a flexible printed circuit board and a flexible printed circuit board, which is called a flexible board or FPC for short, and has the characteristics of high wiring density, thin thickness and light weight. The method is mainly used for a plurality of products such as mobile phones, PDAs, notebook computers, digital cameras, LCMs and the like; the FPC flexible printed circuit is a flexible printed circuit with excellent reliability and is made by taking polyimide or polyester film as a base material; the pressing is an important process in the production of the FPC board, and is a process for bonding one or more inner layer etched back boards and copper foils into a multi-layer board by utilizing high temperature and high pressure to enable a prepreg to be heated and melted, flow and then be converted into a solidified sheet. In the pressing process, the upper and lower parts of the circuit board are covered by the separating film to play a role in protection. The separation membrane used in the pressing process plays a critical role in the product quality. The separation membrane mainly plays roles of isolation, filling, protection and easy peeling in FPC production, and the three basic requirements of the FPC laminated separation membrane are as follows: separability, temperature resistance, ductility.
The existing related products can not meet the requirements at the same time and must be matched for use; and a part of products are also formed by uniformly coating a layer of extremely thin silica gel release agent on the surface, and silicone oil can be separated out to pollute the circuit board in use.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a high temperature glue-blocking PBT separation film for FPC bonding process and a processing process thereof.
The utility model provides a high temperature hinders and glues PBT separation membrane for FPC pressfitting technology, includes inlayer and two skin, and the inlayer sets up between two skins, the thickness ratio of skin and inlayer is: 1: 0.7-1.3, wherein the outer layer comprises the following components in percentage by weight: 86.2-87.2% of PBT, 0.7-0.9% of composite antioxidant, 0.7-0.9% of white oil, 2.8-3.2% of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 38.8-39.4% of PBT, 4.5-4.9% of compatilizer, 13.6-14.6% of EVA, 0.7-0.9% of composite antioxidant, 1.6-1.8% of modifier II and the balance of LDPE.
Further, the first modifier comprises the following components in percentage by weight: 88.4-89.4% of ABS-g-GMA, 0.5-0.9% of silane coupling agent, and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.4-30.4% of ABS-g-GMA, 19.5-20.7% of nucleating agent and the balance of nano zinc oxide.
Further, the thickness ratio of the outer layer to the inner layer is: 1: 0.7, wherein the outer layer comprises the following components in percentage by weight: 86.2 percent of PBT, 0.7 percent of composite antioxidant, 0.7 percent of white oil, 2.8 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 38.8% of PBT, 4.5% of compatilizer, 13.6% of EVA, 0.7% of composite antioxidant, 1.6% of second modifier and the balance LDPE; the first modifier comprises the following components in percentage by weight: 88.40% of ABS-g-GMA, 0.5% of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.4 percent of ABS-g-GMA, 19.5 to 20.7 percent of nucleating agent and the balance of nano zinc oxide.
Further, the thickness ratio of the outer layer to the inner layer is: 1: 1.3, wherein the outer layer comprises the following components in percentage by weight: 87.2 percent of PBT, 0.9 percent of composite antioxidant, 0.9 percent of white oil, 3.2 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 39.4 percent of PBT, 4.9 percent of compatilizer, 14.6 percent of EVA, 0.9 percent of composite antioxidant, 1.8 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 89.4 percent of ABS-g-GMA, 0.9 percent of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 30.4 percent of ABS-g-GMA, 20.7 percent of nucleating agent and the balance of nano zinc oxide.
Further, the thickness ratio of the outer layer to the inner layer is: 1: 1, wherein the outer layer comprises the following components in percentage by weight: 86.7 percent of PBT, 0.8 percent of composite antioxidant, 0.8 percent of white oil, 3.0 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 39.1 percent of PBT, 4.7 percent of compatilizer, 14.1 percent of EVA, 0.8 percent of composite antioxidant, 1.7 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 88.9 percent of ABS-g-GMA, 0.7 percent of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.9 percent of ABS-g-GMA, 20.1 percent of nucleating agent and the balance of nano zinc oxide.
Further, the compound antioxidant comprises the following components in percentage by weight: 49.40-50.40% of antioxidant 1010, and the balance antioxidant 168; the white oil is No. 5 white oil; the compatibilizer is AX 8900; the EVA is EVA 1828; the LDPE is LDPE 2426; the silane coupling agent is KH-560 silane coupling agent; the nucleating agent is NX 8000K.
A processing technology of a high-temperature glue-resistant PBT separation membrane for an FPC pressing process comprises the following specific processing steps:
the method comprises the following steps: weighing PBT, a composite antioxidant, white oil, polytetrafluoroethylene, ABS-g-GMA, a silane coupling agent and graphene oxide in the outer layer raw materials and PBT, LDPE, a compatilizer, EVA, a composite antioxidant, ABS-g-GMA, a nucleating agent and nano zinc oxide in the inner layer raw materials in parts by weight;
step two: at normal temperature and normal pressure, adding PBT, a composite antioxidant, white oil, polytetrafluoroethylene, ABS-g-GMA, a silane coupling agent and graphene oxide in the outer layer raw materials into a high-speed mixer; adding polytetrafluoroethylene powder into a high-speed stirrer lightly; stirring and mixing to obtain a mixture a;
step three: melting and blending the mixture a by a double-screw extruder, shearing and mixing by screws, then bracing, granulating and drying to obtain an outer-layer base material;
step four: at normal temperature and normal pressure, mixing PBT, LDPE, compatilizer, EVA, composite antioxidant, ABS-g-GMA, nucleating agent and nano zinc oxide in the inner layer raw materials at high speed in a high-speed mixer, and stirring for 3 times, 40 seconds each time; obtaining a mixture b;
step five: and respectively adding the outer-layer base material and the mixture b into three screws of an extrusion casting machine, adding the outer-layer base material into the B, C screw, adding the mixture b into the screw A, carrying out intramembrane compounding on molten materials extruded by the three screws through a high-temperature T-shaped die, carrying out three-layer co-extrusion molding, cooling and stretching in the casting machine, and finally adjusting the rotating speed and the tension of the screws to obtain the high-temperature adhesive-resistant PBT separation membrane for the FPC laminating process.
Further, drying the PBT for 3 hours at the temperature of 110-120 ℃ before the first step to ensure that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 230-240 +/-5 ℃, the rotating speed of the screw is 260-300 r/min, and in the drying process, the drying is carried out in a dryer at 110-120 ℃ for 5 hours, so that the moisture content is ensured to be less than 0.03%; in the fourth step, the high-speed mixer stirs for 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 235-245 +/-5 ℃, the heating temperature of the screw A is 250-260 +/-5 ℃, the temperature of a flow combiner on the casting machine is 240-250 +/-5 ℃, and the temperature of the T-shaped die is controlled to be 225-235 +/-5 ℃; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 100-190 microns.
Further, drying the PBT for 3 hours at the temperature of 115 ℃ before the first step to ensure that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 235 +/-5 ℃, the rotating speed of the screw is 270r/min, and in the drying process, the drying is carried out in a dryer at 115 ℃ for 5 hours, so as to ensure that the moisture content is less than 0.03 percent; in the fourth step, the high-speed mixer stirs for 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 240 +/-5 ℃, the heating temperature of the screw A is 255 +/-5 ℃, the temperature of the flow combiner on the casting machine is 245 +/-5 ℃, and the temperature of the T-shaped die is controlled at 230 +/-5 ℃; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 150 mu m.
Further, drying the PBT for 3 hours at the temperature of 120 ℃ before the first step to ensure that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 240 +/-5 ℃, the rotating speed of the screw is 300r/min, and in the drying process, the drying is carried out in a dryer at 120 ℃ for 5 hours, so as to ensure that the moisture content is less than 0.03 percent; in the fourth step, the high-speed mixer stirs for 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 245 +/-5 ℃, the heating temperature of the screw A is 260 +/-5 ℃, the temperature of a flow combiner on the casting machine is 250 +/-5 ℃, and the temperature of the T-shaped die is controlled to be 235 +/-5 ℃; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 140 micrometers.
The invention has the technical effects and advantages that:
1. the high-temperature glue-blocking PBT separation membrane for the FPC pressing process, which is processed by adopting the raw material formula, is modified by adding the polytetrafluoroethylene micro powder, and achieves the purpose of demand by utilizing the characteristics of high temperature, high lubricity and small surface tension of the polytetrafluoroethylene; the polytetrafluoroethylene powder particles reach more than 3000 meshes; the antioxidant 1010 can effectively prevent thermal oxidation degradation of the polymer material in a long-term aging process, is also an efficient processing stabilizer, and can improve the color change resistance of the polymer material under a high-temperature processing condition; the antioxidant 168 is an indispensable heat stabilizer in resin processing, and has excellent synergistic effect when being used together with the main antioxidant 1010; ABS-g-GMA modifies PBT to improve the impact strength and the elongation at break; the graphene oxide is grafted to polytetrafluoroethylene under the treatment of a KH560 silane coupling agent, so that the mechanical property and the friction coefficient of the graphene oxide are improved; the blending modification treatment is carried out on the LDPE by the nano zinc oxide, so that the ultraviolet shielding effect is improved; the nucleating agent NX8000K is used for carrying out blending modification treatment on LDPE so as to improve the impact strength of the LDPE; characteristics/advantages: the heat resistance is good: the PBT can also be used under the condition of high temperature of 200 ℃, the melting point of the PBT is about 230 ℃, and the melting temperature of the polytetrafluoroethylene is more than 300 ℃; the method can also be used in a process procedure of 200 ℃; the mold release property is excellent: the coating can be peeled off from various materials, has small surface tension and good demoulding property on various materials such as epoxy resin glue and the like; the filling property is good: the soft inner layer material can be matched with a complex surface shape, is softened at 100 ℃, and is very easy to closely adhere to a complex concave-convex shape; low pollution: does not contain substances such as silica gel, plasticizer and the like which pollute the surface of the product; environmental adaptability: can be incinerated, thereby facilitating the subsequent treatment of customers; one material simultaneously satisfies three main properties: high temperature, separation and glue blocking;
2. in the process of processing the high-temperature glue-resistant PBT separation membrane for the FPC pressing process, the content of polytetrafluoroethylene in the separation layer is controlled, and the content is too small, so that the release force is influenced; the content is too much, and the release force is not obviously changed; the material is too high in price, and the cost is influenced by excessive addition; the glue resistance performance of the glue resistance filling layer is reduced when the PBT content in the glue resistance filling layer is excessive, the glue resistance performance of the glue resistance filling layer is increased when the PBT content in the glue resistance filling layer is too low, but the glue outlet length is too long to pollute the circuit board surface, and the cleaning frequency of operators is increased.
Detailed Description
The following will clearly and completely describe the technical solutions 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 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.
Example 1:
the invention provides a high-temperature glue-resistant PBT separation membrane for an FPC (flexible printed circuit) laminating process, which comprises an inner layer and two outer layers, wherein the inner layer is arranged between the two outer layers, and the thickness ratio of the outer layer to the inner layer is as follows: 1: 0.7, wherein the outer layer comprises the following components in percentage by weight: 87.4 percent of PBT, 0.7 percent of composite antioxidant, 0.7 percent of white oil, 2.8 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 38.8 percent of PBT, 4.5 percent of compatilizer, 13.6 percent of EVA, 0.7 percent of composite antioxidant, 1.6 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 88.40% of ABS-g-GMA, 0.5% of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.4 percent of ABS-g-GMA, 19.5 to 20.7 percent of nucleating agent and the balance of nano zinc oxide;
the invention also provides a processing technology of the high-temperature glue-resistant PBT separation membrane for the FPC laminating technology, which comprises the following specific processing steps:
the method comprises the following steps: weighing PBT, a composite antioxidant, white oil, polytetrafluoroethylene, ABS-g-GMA, a silane coupling agent and graphene oxide in the outer layer raw materials and PBT, LDPE, a compatilizer, EVA, a composite antioxidant, ABS-g-GMA, a nucleating agent and nano zinc oxide in the inner layer raw materials in parts by weight;
step two: at normal temperature and normal pressure, adding PBT, a composite antioxidant, white oil, polytetrafluoroethylene, ABS-g-GMA, a silane coupling agent and graphene oxide in the outer layer raw materials into a high-speed mixer, and uniformly adhering white oil on the surface of the PBT; adding polytetrafluoroethylene powder into a high-speed stirrer lightly; stirring and mixing to obtain a mixture a, so that the polytetrafluoroethylene powder is uniformly adhered to the surface of the PBT;
step three: melting and blending the mixture a by a double-screw extruder, shearing and mixing by screws, then bracing, granulating and drying to obtain an outer-layer base material;
step four: at normal temperature and normal pressure, mixing PBT, LDPE, compatilizer, EVA, composite antioxidant, ABS-g-GMA, nucleating agent and nano zinc oxide in the inner layer raw materials at high speed in a high-speed mixer, and stirring for 3 times, 40 seconds each time; obtaining a mixture b;
step five: and respectively adding the outer-layer base material and the mixture b into three screws of an extrusion casting machine, adding the outer-layer base material into the B, C screw, adding the mixture b into the screw A, carrying out intramembrane compounding on molten materials extruded by the three screws through a high-temperature T-shaped die, carrying out three-layer co-extrusion molding, cooling and stretching in the casting machine, and finally adjusting the rotating speed and the tension of the screws to obtain the high-temperature adhesive-resistant PBT separation membrane for the FPC laminating process.
Drying the PBT for 3 hours at the temperature of 120 ℃ before the first step, and ensuring that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 240 +/-5 ℃, the rotating speed of the screw is 300r/min, and in the drying process, the drying is carried out in a dryer at 120 ℃ for 5 hours, so as to ensure that the moisture content is less than 0.03 percent; in the fourth step, the high-speed mixer stirs 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 245 +/-5 ℃, the heating temperature of the screw A is 260 +/-5 ℃, the temperature of a flow combiner on the casting machine is 250 +/-5 ℃, the temperature of the T-shaped die is controlled to be 235 +/-5 ℃, and the three layers of films are firmly bonded; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 140 micrometers.
Example 2:
unlike example 1, the thickness ratio of the outer layer to the inner layer was: 1: 1.3, wherein the outer layer comprises the following components in percentage by weight: 88.4 percent of PBT, 0.9 percent of composite antioxidant, 0.9 percent of white oil, 3.2 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 39.4 percent of PBT, 4.9 percent of compatilizer, 14.6 percent of EVA, 0.9 percent of composite antioxidant, 1.8 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 89.4 percent of ABS-g-GMA, 0.9 percent of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 30.4 percent of ABS-g-GMA, 20.7 percent of nucleating agent and the balance of nano zinc oxide.
Example 3:
unlike examples 1-2, the thickness ratio of the outer layer to the inner layer was: 1: 1, wherein the outer layer comprises the following components in percentage by weight: 87.9 percent of PBT, 0.8 percent of composite antioxidant, 0.8 percent of white oil, 3.0 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 39.1 percent of PBT, 4.7 percent of compatilizer, 14.1 percent of EVA, 0.8 percent of composite antioxidant, 1.7 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 88.9 percent of ABS-g-GMA, 0.7 percent of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.9 percent of ABS-g-GMA, 20.1 percent of nucleating agent and the balance of nano zinc oxide.
Comparative example 1:
the difference from example 3 is: the outer layer comprises the following components in percentage by weight: 94 percent of PBT, 5 percent of polytetrafluoroethylene, 0.5 percent of antioxidant (1010), 0.5 percent of antioxidant (168) and No. 5 white oil are additionally added according to 0.8Kg/100 Kg; the inner layer comprises the following components in percentage by weight: 50% of PBT, 14% of EVA1828, 30% of LDPE, 5% of compatilizer AX8900, 0.5% of antioxidant (1010) and 0.5% of antioxidant (168).
Comparative example 2:
in contrast to comparative example 1: the outer layer comprises the following components in percentage by weight: 92% of PBT, 7% of polytetrafluoroethylene, 0.5% of antioxidant (1010), 0.5% of antioxidant (168) and No. 5 white oil are additionally added according to 0.8Kg/100 Kg; the inner layer comprises the following components in percentage by weight: 45% of PBT, 14% of EVA1828, 35% of LDPE2426, 5% of compatilizer AX8900, 0.5% of antioxidant (1010) and 0.5% of antioxidant (168).
Comparative example 3:
different from all of comparative examples 1-2: the outer layer comprises the following components in percentage by weight: 89 percent of PBT, 10 percent of polytetrafluoroethylene, 0.5 percent of antioxidant (1010), 0.5 percent of antioxidant (168) and No. 5 white oil are additionally added according to 0.8Kg/100 Kg; the inner layer comprises the following components in percentage by weight: 35% of PBT, 14% of EVA1828, 45% of LDPE2426, 5% of compatilizer AX8900, 0.5% of antioxidant (1010) and 0.5% of antioxidant (168).
Comparative example 4:
in contrast to comparative examples 1 to 3: the outer layer comprises the following components in percentage by weight: 84 percent of PBT, 15 percent of polytetrafluoroethylene, 0.5 percent of antioxidant (1010), 0.5 percent of antioxidant (168) and No. 5 white oil are additionally added according to 0.8Kg/100 Kg; the inner layer comprises the following components in percentage by weight: 30% of PBT, 14% of EVA1828, 50% of LDPE2426, 5% of compatilizer AX8900, 0.5% of antioxidant (1010) and 0.5% of antioxidant (168).
By adopting the formula and the method, the performance parameters of the finally obtained high-temperature release film are shown in the following table:
Figure 700726DEST_PATH_IMAGE002
the results of comparative tests carried out on the components of the formulation according to the invention, with unchanged process conditions and formulation amounts, are shown in the following table:
Figure DEST_PATH_IMAGE004AAAA
the outer layer is used as a separation layer of the separation membrane, and the inner layer is used as a glue-blocking filling layer of the separation membrane; from the above table, it can be seen that: the content of the polytetrafluoroethylene in the separation layer is controlled, and the content is too low, so that the release force is influenced; the content is too much, and the release force is not obviously changed; the material is too high in price, and the cost is influenced by excessive addition; the glue-blocking performance of the glue-blocking filling layer is reduced when the PBT content is excessive, the glue-blocking performance is improved when the PBT content is too low, but the glue-discharging length is too long, so that the circuit board surface is polluted, and the cleaning frequency of operators is increased.
With the formulation of example 3 and the same variables of other process conditions, comparative tests were carried out on the parameters of the production process of the invention, the results being shown in the following table:
Figure DEST_PATH_IMAGE006AA
from the above table, it can be seen that: in the process temperature, the film with the thickness of 100-190 microns has better comprehensive performance, when the thickness of the film is changed, the fracture occurrence rate and the glue outlet length of a final product can be influenced, the production requirement of an FPC (flexible printed circuit) can not be met, and when the production temperature of the product is changed, the temperature resistance of the final product is greatly influenced, particularly the temperature of a current combiner and a T-shaped mold.
The separation membrane can simultaneously meet the three requirements through selection of high-temperature-resistant materials and control of the process, effectively improves the qualification rate of the FPC flexible circuit board, reduces the cost, and simultaneously meets the requirement of clean production of the FPC flexible circuit board.
According to the invention, a formula for synthesizing the inner layer and the outer layer of the release film and the content of each substance in the formula are co-extruded by a casting machine in three layers; the outer layer is made of PBT and polytetrafluoroethylene; pressing FPC to obtain a separation layer in a separation membrane (release membrane) and adding polytetrafluoroethylene material into the separation layer; the PBT is modified by adding the polytetrafluoroethylene micro powder, and the high temperature property, high lubricity and small surface tension property of the polytetrafluoroethylene are utilized to achieve the purpose of demand; the polytetrafluoroethylene powder particles reach more than 3000 meshes; the antioxidant 1010 can effectively prevent the thermal oxidation degradation of the inner layer and the outer layer of the separation membrane in the long-term aging process, is also an efficient processing stabilizer, and can improve the color change resistance of the inner layer and the outer layer of the separation membrane under the high-temperature processing condition; the antioxidant 168 is an indispensable heat stabilizer in resin processing, and has an excellent synergistic effect when being used together with the main antioxidant 1010, so that the temperature resistance of the inner layer and the outer layer of the separation membrane is further improved; ABS-g-GMA modifies PBT, and improves the impact strength and the elongation at break of the outer layer and the inner layer; the graphene oxide is grafted to the polytetrafluoroethylene under the treatment of the KH560 silane coupling agent, so that the mechanical property and the friction coefficient of the graphene oxide are improved; blending modification treatment is carried out on LDPE by the nano zinc oxide, so that the ultraviolet shielding effect of the inner layer is improved; the nucleating agent is used for carrying out blending modification treatment on NX8000K on LDPE so as to improve the impact strength; characteristics/advantages: the heat resistance is good: the PBT can also be used under the condition of high temperature of 200 ℃, the melting point of the PBT is about 230 ℃, and the melting temperature of the polytetrafluoroethylene is more than 300 ℃; the method can also be used in a process procedure of 200 ℃; the mold release property is excellent: the coating can be peeled off from various materials, has small surface tension and good demoulding property on various materials such as epoxy resin glue and the like; the filling property is good: the soft inner layer material can be matched with a complex surface shape, is softened at 100 ℃, and is very easy to closely adhere to a complex concave-convex shape; low pollution: does not contain substances such as silica gel, plasticizer and the like which pollute the surface of the product; environmental adaptability: can be incinerated, thereby facilitating the subsequent treatment of customers; one material simultaneously satisfies three main properties: high temperature, separation and glue blocking.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A high temperature hinders and glues PBT separation membrane for FPC pressfitting technology which characterized in that: including inlayer and two skin, the inlayer sets up between two skins, the thickness ratio of skin and inlayer is: 1: 0.7-1.3, wherein the outer layer comprises the following components in percentage by weight: 86.2-87.2% of PBT, 0.7-0.9% of composite antioxidant, 0.7-0.9% of white oil, 2.8-3.2% of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 38.8-39.4% of PBT, 4.5-4.9% of compatilizer, 13.6-14.6% of EVA, 0.7-0.9% of composite antioxidant, 1.6-1.8% of modifier II and the balance of LDPE.
2. The high-temperature glue-resistant PBT separation membrane used for the FPC pressing process according to claim 1, characterized in that: the first modifier comprises the following components in percentage by weight: 88.4-89.4% of ABS-g-GMA, 0.5-0.9% of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.4-30.4% of ABS-g-GMA, 19.5-20.7% of nucleating agent and the balance of nano zinc oxide.
3. The high-temperature glue-resistant PBT separation membrane used for the FPC pressing process according to claim 2, characterized in that: the thickness ratio of the outer layer to the inner layer is as follows: 1: 0.7, wherein the outer layer comprises the following components in percentage by weight: 86.2 percent of PBT, 0.7 percent of composite antioxidant, 0.7 percent of white oil, 2.8 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 38.8 percent of PBT, 4.5 percent of compatilizer, 13.6 percent of EVA, 0.7 percent of composite antioxidant, 1.6 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 88.40% of ABS-g-GMA, 0.5% of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.4 percent of ABS-g-GMA, 19.5 to 20.7 percent of nucleating agent and the balance of nano zinc oxide.
4. The high-temperature glue-resistant PBT separation membrane used for the FPC pressing process according to claim 2, characterized in that: the thickness ratio of the outer layer to the inner layer is as follows: 1: 1.3, wherein the outer layer comprises the following components in percentage by weight: 87.2 percent of PBT, 0.9 percent of composite antioxidant, 0.9 percent of white oil, 3.2 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 39.4 percent of PBT, 4.9 percent of compatilizer, 14.6 percent of EVA, 0.9 percent of composite antioxidant, 1.8 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 89.4 percent of ABS-g-GMA, 0.9 percent of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 30.4 percent of ABS-g-GMA, 20.7 percent of nucleating agent and the balance of nano zinc oxide.
5. The high-temperature glue-resistant PBT separation membrane used for the FPC pressing process according to claim 2, characterized in that: the thickness ratio of the outer layer to the inner layer is as follows: 1: 1, wherein the outer layer comprises the following components in percentage by weight: 86.7 percent of PBT, 0.8 percent of composite antioxidant, 0.8 percent of white oil, 3.0 percent of modifier I and the balance of polytetrafluoroethylene; the inner layer comprises the following components in percentage by weight: 39.1 percent of PBT, 4.7 percent of compatilizer, 14.1 percent of EVA, 0.8 percent of composite antioxidant, 1.7 percent of modifier II and the balance of LDPE; the first modifier comprises the following components in percentage by weight: 88.9 percent of ABS-g-GMA, 0.7 percent of silane coupling agent and the balance of graphene oxide; the second modifier comprises the following components in percentage by weight: 29.9 percent of ABS-g-GMA, 20.1 percent of nucleating agent and the balance of nano zinc oxide.
6. The high-temperature glue-resistant PBT separation membrane used for the FPC pressing process according to claim 2, characterized in that: the composite antioxidant comprises the following components in percentage by weight: 49.40-50.40% of antioxidant 1010, and the balance antioxidant 168; the white oil is No. 5 white oil; the compatibilizer is AX 8900; the EVA is EVA 1828; the LDPE is LDPE 2426; the silane coupling agent is KH-560 silane coupling agent; the nucleating agent is NX 8000K.
7. A processing technology of a high-temperature glue-resistant PBT separation membrane for an FPC pressing technology is characterized by comprising the following steps: the specific processing steps are as follows:
the method comprises the following steps: weighing PBT, a composite antioxidant, white oil, polytetrafluoroethylene, ABS-g-GMA, a silane coupling agent and graphene oxide in the outer layer raw materials and PBT, LDPE, a compatilizer, EVA, a composite antioxidant, ABS-g-GMA, a nucleating agent and nano zinc oxide in the inner layer raw materials in parts by weight;
step two: at normal temperature and normal pressure, adding PBT, a composite antioxidant, white oil, polytetrafluoroethylene, ABS-g-GMA, a silane coupling agent and graphene oxide in the outer layer raw materials into a high-speed mixer; adding polytetrafluoroethylene powder into a high-speed stirrer lightly; stirring and mixing to obtain a mixture a;
step three: melting and blending the mixture a by a double-screw extruder, shearing and mixing by screws, then bracing, granulating and drying to obtain an outer-layer base material;
step four: at normal temperature and normal pressure, mixing PBT, LDPE, compatilizer, EVA, composite antioxidant, ABS-g-GMA, nucleating agent and nano zinc oxide in the inner layer raw materials at high speed in a high-speed mixer, and stirring for 3 times, 40 seconds each time; obtaining a mixture b;
step five: and respectively adding the outer-layer base material and the mixture b into three screws of an extrusion casting machine, adding the outer-layer base material into the B, C screw, adding the mixture b into the screw A, carrying out intramembrane compounding on molten materials extruded by the three screws through a high-temperature T-shaped die, carrying out three-layer co-extrusion molding, cooling and stretching in the casting machine, and finally adjusting the rotating speed and the tension of the screws to obtain the high-temperature adhesive-resistant PBT separation membrane for the FPC laminating process.
8. The processing technology of the high-temperature glue-resistant PBT separation membrane used for the FPC pressing technology according to claim 7 is characterized in that: drying the PBT for 3 hours at the temperature of 110-120 ℃ before the first step, and ensuring that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 230-240 +/-5 ℃, the rotating speed of the screw is 260-300 r/min, and in the drying process, the drying is carried out in a dryer at the temperature of 110-120 ℃ for 5 hours, so that the moisture content is ensured to be less than 0.03%; in the fourth step, the high-speed mixer stirs for 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 235-245 +/-5 ℃, the heating temperature of the screw A is 250-260 +/-5 ℃, the temperature of a flow combiner on the casting machine is 240-250 +/-5 ℃, and the temperature of the T-shaped die is controlled to be 225-235 +/-5 ℃; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 100-190 microns.
9. The processing technology of the high-temperature glue-resistant PBT separation membrane used for the FPC pressing technology according to claim 8 is characterized in that: drying the PBT for 3 hours at the temperature of 115 ℃ before the first step to ensure that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 235 +/-5 ℃, the rotating speed of the screw is 270r/min, and in the drying process, the drying is carried out in a dryer at 115 ℃ for 5 hours, so as to ensure that the moisture content is less than 0.03 percent; in the fourth step, the high-speed mixer stirs for 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 240 +/-5 ℃, the heating temperature of the screw A is 255 +/-5 ℃, the temperature of a flow combiner on the casting machine is 245 +/-5 ℃, and the temperature of the T-shaped die is controlled to be 230 +/-5 ℃; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 150 mu m.
10. The processing technology of the high-temperature glue-resistant PBT separation membrane used for the FPC pressing technology according to claim 8 is characterized in that: drying the PBT for 3 hours at the temperature of 120 ℃ before the first step to ensure that the humidity of the PBT is less than 0.03%; in the second step, before adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by a high-speed mixer, and after adding the polytetrafluoroethylene, stirring for 3 times and 40 seconds each time by the high-speed mixer; in the third step, the temperature is controlled to be 240 +/-5 ℃, the rotating speed of the screw is 300r/min, and in the drying process, the drying is carried out in a dryer at 120 ℃ for 5 hours, so as to ensure that the moisture content is less than 0.03 percent; in the fourth step, the high-speed mixer stirs for 3 times, 40 seconds each time; in the fifth step, the heating temperature of the screw C and the screw B is 245 +/-5 ℃, the heating temperature of the screw A is 260 +/-5 ℃, the temperature of a flow combiner on the casting machine is 250 +/-5 ℃, and the temperature of the T-shaped die is controlled to be 235 +/-5 ℃; the thickness of the high-temperature glue-resistant PBT separation membrane used for the FPC laminating process is 140 micrometers.
CN202210584647.8A 2022-05-27 2022-05-27 High-temperature glue-resistant PBT (polybutylene terephthalate) separation membrane for FPC (flexible printed circuit) laminating process and processing process thereof Pending CN114874595A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115449309A (en) * 2022-09-20 2022-12-09 湖南优多新材料科技有限公司 Pyrolytic adhesive tape for FPC bearing and use method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115449309A (en) * 2022-09-20 2022-12-09 湖南优多新材料科技有限公司 Pyrolytic adhesive tape for FPC bearing and use method thereof

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