WO2021042418A1 - 一种绝缘介质胶膜及其制备方法、多层印刷线路板 - Google Patents
一种绝缘介质胶膜及其制备方法、多层印刷线路板 Download PDFInfo
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- WO2021042418A1 WO2021042418A1 PCT/CN2019/106789 CN2019106789W WO2021042418A1 WO 2021042418 A1 WO2021042418 A1 WO 2021042418A1 CN 2019106789 W CN2019106789 W CN 2019106789W WO 2021042418 A1 WO2021042418 A1 WO 2021042418A1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2463/00—Presence of epoxy resin
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/005—Presence of polyester in the release coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2475/00—Presence of polyurethane
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0296—Conductive pattern lay-out details not covered by sub groups H05K1/02 - H05K1/0295
- H05K1/0298—Multilayer circuits
Definitions
- the invention relates to the field of high-density multilayer circuit board packaging materials, in particular to an insulating medium adhesive film and a preparation method thereof, and a multilayer printed circuit board.
- High-density multilayer circuit boards are usually used as packaging substrates for portable electronic products such as mobile phones, digital cameras, laptop computers, etc.
- the improvement of multilayer circuit boards has become a research hotspot.
- High-density multilayer circuit board refers to the use of glass cloth reinforced insulating medium on an insulating substrate, a traditional double-sided board or a multi-layer board to form wires and connection holes through electroless copper plating and copper electroplating.
- Multi-layer printed circuit boards that require layers.
- the traditional multi-layer circuit board preparation process is to obtain conductive patterns by selectively removing part of the copper foil on the surface of the copper-clad laminate, which has many procedures, is difficult to control, and is costly.
- the line width/line spacing is less than 40 microns and the line quality cannot be guaranteed, and the semiconductor chip carrier generally has a line width/line spacing less than 15 microns.
- the current solution only uses the semi-additive method (SAP) or the improved semi-processed method (MSAP), which is also the most advanced manufacturing process for HDI (High Density Interconnect Multilayer Circuit Board) today.
- SAP semi-additive method
- MSAP improved semi-processed method
- the technical key of the semi-additive method is the laminated material-insulating film material, which is the ABF/GX series products of Ajinomoto, Japan. It mainly uses epoxy and curing agents and thermoplastic phenolic resins to act as the film-forming effect.
- the solvent is dried by infrared heating or hot air to obtain a viscous film.
- the phenolic resin is made of phenol chain-extended epoxy, its large number of alcoholic hydroxyl groups will be serious Affects the dielectric properties of the insulating medium, and its application in the high-frequency and high-speed field is limited.
- Chinese patent ZL201810631718.9 uses urethane acrylate resin and hydroxyethyl methacrylate light curing to act as the epoxy resin film-forming component, and uses aliphatic epoxy as the main solvent-free coating method to prepare the insulating dielectric film.
- urethane acrylate resin and hydroxyethyl methacrylate light curing to act as the epoxy resin film-forming component
- aliphatic epoxy as the main solvent-free coating method to prepare the insulating dielectric film.
- Solvent coating is not suitable for formulation design, and the technology has poor flame retardancy and large thermal expansion.
- ABF insulating dielectric
- the purpose of the present invention is to provide an insulating dielectric film, a preparation method thereof, and a multilayer printed circuit board, which aims to solve the problem of poor flexibility, high dielectric constant, and dielectric properties of the existing insulating dielectric film.
- the electric loss factor is high, and the problem of thermal expansion is prone to occur.
- An insulating medium adhesive film which includes a release film and an insulating medium layer arranged on the surface of the release film.
- the material of the insulating medium layer includes saturated polyester resin, amino resin or blocked isocyanate, epoxy resin, and curing agent. , Inorganic fillers and curing accelerators.
- the insulating dielectric film wherein the insulating dielectric layer material comprises 5-30 parts by weight of saturated polyester resin, 0.5-3 parts of amino resin or blocked isocyanate, and 45-75 parts of epoxy resin. Resin, 1-25 parts of curing agent, 1-100 parts of inorganic filler and 0.1-5 parts of curing accelerator.
- the chemical structural formula of the saturated polyester resin is: Wherein, n is 1-100, and R1 and R2 are independently selected from alkyl groups with less than 20 carbon atoms, phenyl groups, naphthyl groups, or combinations thereof.
- the amino resin is a resin formed by the condensation polymerization of melamine or benzoic melamine, formaldehyde and organic alcohol.
- the blocked isocyanate is one or more of phenol-blocked HDI, MDI, TDI, and PDI; or, the blocked isocyanate is caprolactam-blocked HDI, MDI, TDI, and One or more of PDI.
- the insulating dielectric film wherein the epoxy resin is selected from the group consisting of bisphenol A epoxy resin, bisphenol F epoxy resin, DCPD epoxy resin, triphenol epoxy resin, biphenyl epoxy resin, naphthol One or more of epoxy resin and phosphorus-containing epoxy resin.
- the curing agent is selected from one or more of dicyandiamide, aromatic amines, phenolic compounds, active greases, and phosphorus-containing phenolic aldehydes.
- the release film has a thickness of 10-100 ⁇ m, and the insulating dielectric layer has a thickness of 10-200 ⁇ m.
- the method for preparing the insulating medium adhesive film includes the following steps:
- the third glue solution is coated on the release film and cured to obtain the insulating medium glue film.
- a multilayer printed circuit board which includes the insulating dielectric adhesive film of the present invention.
- the insulating medium adhesive film provided by the present invention includes a release film and an insulating medium layer arranged on the surface of the release film.
- the material of the insulating medium layer includes saturated polyester resin, amino resin or blocked isocyanate, epoxy resin, Curing agent, inorganic filler and curing accelerator.
- the saturated polyester resin component is introduced into the epoxy resin composition, so that the prepared insulating dielectric adhesive film has the advantages of low dielectric constant, low dielectric loss factor, good adhesion and the like.
- FIG. 1 is a flowchart of a preferred embodiment of a method for preparing an insulating dielectric adhesive film provided by the present invention.
- the present invention provides an insulating medium adhesive film, a preparation method thereof, and a multilayer printed circuit board.
- a preparation method thereof a preparation method thereof
- a multilayer printed circuit board a multilayer printed circuit board
- the embodiment of the present invention provides an insulating dielectric adhesive film, which includes a release film and an insulating dielectric layer disposed on the surface of the release film.
- the material of the insulating dielectric layer includes saturated polyester resin, amino resin or blocked isocyanate, ring Oxygen resin, curing agent, inorganic filler and curing accelerator.
- the prior art usually uses a mixture of thermoplastic phenolic resin and epoxy resin to prepare insulating dielectric films.
- the phenolic resin is made of phenol chain-extended epoxy, it has a large number of alcoholic hydroxyl groups. The strong polarity of the alcoholic hydroxyl group will affect the dielectric properties of the insulating dielectric film.
- a saturated polyester resin component is introduced into an epoxy resin.
- the saturated polyester resin is prepared by the polymerization reaction of a polyhydric alcohol and a polybasic acid, and the saturated polyester resin only contains hydroxyl groups at the ends.
- this embodiment also introduces amino resin or blocked isocyanate into the epoxy resin.
- the amino resin or blocked isocyanate can undergo cross-linking reaction with saturated polyester resin. Remove the hydroxyl groups at both ends of the saturated polyester resin, further reduce the polarity of the saturated polyester resin, improve the dielectric properties, and increase the molecular weight of the saturated polyester resin to improve the film-forming effect.
- the insulating dielectric layer material includes 5-30 parts by weight. Polyester resin, 0.5-3 parts amino resin or blocked isocyanate, 45-75 parts epoxy resin, 1-25 parts curing agent, 1-100 parts inorganic filler and 0.1-5 parts curing accelerator,
- the insulating dielectric layer prepared according to the formula of this embodiment has excellent dielectric properties.
- the chemical structural formula of the saturated polyester resin is Wherein, n is 1-100, and R1 and R2 are independently selected from alkyl groups with less than 20 carbon atoms, phenyl groups, naphthyl groups, or combinations thereof.
- the saturated polyester resin provided in this embodiment has excellent film-forming properties, and the saturated polyester resin contains a small amount of hydroxyl groups and is relatively weak in polarity. It is compatible with epoxy resin, amino resin or blocked isocyanate, curing agent, inorganic
- the insulating dielectric layer prepared by mixing the filler and the curing accelerator has a lower dielectric constant and dielectric loss factor.
- the relative molecular weight of the saturated polyester resin is 8000-30000. If the relative molecular weight of the saturated polyester resin is less than 8000, it is not conducive to film formation. If the relative molecular weight of the saturated polyester resin is greater than 30,000, the molecular weight is too large and the solubility is too low, which is not conducive to mixing with epoxy resin to form a film .
- the amino resin is a resin formed by polycondensation of melamine or benzoic melamine, formaldehyde and organic alcohol.
- the amino resin is a polyfunctional polymer.
- As a cross-linking agent it can cross-link with the saturated polyester resin containing hydroxyl groups at the end, thereby increasing the molecular weight of the saturated polyester resin and reducing the molecular weight of the saturated polyester resin.
- the polarity of the saturated polyester resin enhances the dielectric properties of the insulating dielectric layer.
- the blocked isocyanate is one or more of phenol-blocked HDI, MDI, TDI, and PDI, but is not limited thereto.
- the blocked isocyanate can also be used as a crosslinking agent to crosslink with the saturated polyester resin containing hydroxyl groups at the end, thereby increasing the molecular weight of the saturated polyester resin and reducing the saturated polyester resin Polarity enhances the dielectric properties of the insulating dielectric layer.
- the blocked isocyanate is one or more of caprolactam-blocked HDI, MDI, TDI, and PDI, but it is not limited thereto.
- the epoxy resin is selected from bisphenol A epoxy resin, bisphenol F epoxy resin, DCPD epoxy resin, triphenol epoxy resin, biphenyl epoxy resin, naphthol epoxy resin and One or more of phosphorus-containing epoxy resins, but not limited thereto.
- the epoxy resin is a phosphorus-containing epoxy resin, the phosphorus content in the phosphorus-containing epoxy resin is 2-5%, and the epoxy equivalent is 200-600 g/mol.
- the curing agent is selected from one or more of dicyandiamide, aromatic amines, phenolic compounds, active fats, and phosphorus-containing phenolic aldehydes, but is not limited thereto.
- the curing accelerator is selected from one of 2-methylimidazole, 2-ethyl-4methylimidazole, 2-phenylimidazole, DMP-30, pyridine and p-toluenesulfonic acid or Many, but not limited to this.
- the inorganic filler is selected from aluminum hydroxide, magnesium hydroxide, aluminum oxide, boron nitride, aluminum nitride, silicon carbide, zeolite, wollastonite, silicon dioxide, magnesium oxide, calcium silicate , Calcium carbonate, clay, talc and mica, but not limited thereto.
- the amount of the inorganic filler can be adjusted appropriately according to the purpose of use.
- the insulating dielectric layer material includes 25-100 parts of inorganic filler.
- the thickness of the release film is 10-100 ⁇ m, and the thickness of the insulating dielectric layer is 10-200 ⁇ m.
- a method for preparing an insulating dielectric adhesive film is also provided, wherein, as shown in FIG. 1, the method includes the following steps:
- the saturated polyester resin solution includes an organic solvent and a saturated polyester resin dispersed in the organic solvent, and the organic solvent is selected from one or two of methyl ethyl ketone and cyclohexanone.
- the third glue solution coated on the release film is cured by direct heating or hot air, so that the third glue solution forms an insulating medium layer.
- the heating temperature is set according to the boiling point of the solvent in the third glue solution, the heating temperature is set to 80-130°C, and the heating time is 5-20 min.
- a multilayer printed circuit board which includes the insulating dielectric adhesive film of the present invention.
- the insulating dielectric film and the PCB board with the inner layer circuit are bonded together under the conditions of 80-130°C and 0.1-1MPa pressure, and then pressed in a vacuum press at a pressing temperature of 150-200 °C, curing time of 30-90 minutes, pressure of 0.5-4MPa, the multilayer printed circuit board is prepared.
- DYNAPOL LH826-05A (trade name of German Degussa, saturated polyester resin), dissolve it in isophorone solvent, dissolve completely at room temperature or medium temperature, and add 1 part of HMMM (hexamethoxymethyl melamine) , Stir the standby solution for a certain period of time; then add 30 parts of NPEL-128 (difunctional epoxy resin, trade name of Nanya Plastic Industry Co., Ltd.) and 35 parts of XZ 92530 phosphorus-containing epoxy resin, stir evenly, and add the curing agent dicyandiamide 2.5 parts are dissolved in DMF solvent and added to the above glue solution, 50 parts of spherical silica are added to the above glue solution, fully stirred and dispersed, finally put in the curing accelerator 2-ethyl-4 methylimidazole and BYK450, and stir evenly stand-by.
- a 38 ⁇ m thick PET release film with a thickness of 300 ⁇ 300cm, smooth and flat surface is selected, one side of the release film is evenly coated with the above glue, and the adhesive sheet is prepared by baking in an oven at 120°C for 7 minutes.
- the two insulating films were superimposed and placed in a vacuum hot press at 170° C. and cured for 60 minutes to obtain a substrate sample.
- a 38 ⁇ m thick PET release film with a thickness of 300 ⁇ 300cm, smooth and flat surface was selected, and the release side was uniformly coated with the above-mentioned glue solution, and then baked in an oven at 120°C for 7 minutes to obtain an adhesive sheet.
- the two insulating films were superimposed and placed in a vacuum hot press at 170° C. and cured for 60 minutes to obtain a substrate sample.
- a 38 ⁇ m thick PET release film with a thickness of 300 ⁇ 300cm, smooth and flat surface was selected, and the release side was uniformly coated with the above-mentioned glue solution, and then baked in an oven at 120°C for 7 minutes to obtain an adhesive sheet.
- the two insulating films were superimposed and placed in a vacuum hot press at 170° C. and cured for 60 minutes to obtain a substrate sample.
- a 38 ⁇ m thick PET release film with a thickness of 300 ⁇ 300cm, smooth and flat surface was selected, and the release side was uniformly coated with the above-mentioned glue solution, and then baked in an oven at 120°C for 7 minutes to obtain an adhesive sheet.
- the two insulating films were superimposed and placed in a vacuum hot press to cure at 180°C for 60 minutes to obtain a substrate sample.
- DYNAPOL L411 dissolve it in isophorone solvent, add 1 part of HMMM after it is completely dissolved at room temperature or medium temperature, stir for a certain period of time, and then add 30 parts of NPEL-128 difunctional epoxy and YEP250 containing phosphorus Epoxy 35 parts, stir evenly, dissolve 225 parts of curing agent LA-705 and 3 parts of DDS in PM solvent and add to the above glue solution, add 50 parts of spherical silica to the above glue solution, fully stir and disperse, and finally put it into curing
- the accelerators are 2-ethyl-4methylimidazole, boron trifluoride ethylamine and BYK450.
- the insulating dielectric adhesive film provided by the embodiment of the present invention can reduce the dielectric constant and the dielectric loss factor under the premise of meeting the film-forming characteristics, and at the same time can meet the glass transition temperature, the thermal expansion coefficient is not significantly degraded, and the halogen The content can reach the V-0 standard in the flame retardancy test UL 94 within the scope of the JPCA halogen-free standard.
- the insulating dielectric film provided by the present invention includes a release film and an insulating dielectric layer arranged on the surface of the release film.
- the material of the insulating dielectric layer includes saturated polyester resin, amino resin or blocked isocyanate, epoxy Resin, curing agent, inorganic filler and curing accelerator.
- the saturated polyester resin component is introduced into the epoxy resin composition, so that the prepared insulating medium adhesive film has excellent flexibility, low dielectric constant, low dielectric loss factor, resistance to thermal expansion, and adhesion.
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Abstract
一种绝缘介质胶膜及其制备方法、包括该绝缘介质胶膜的多层印刷线路板,其中,所述绝缘介质胶膜包括离型膜以及设置在离型膜表面的绝缘介质层,所述绝缘介质层材料包括饱和聚酯树脂、氨基树脂或封闭型异氰酸酯、环氧树脂、固化剂、无机填料以及固化促进剂。通过在环氧树脂组合物中引入饱和聚酯树脂组份,使得制得的绝缘介质胶膜具有介电常数低、介电损耗因数低、不易发生热膨胀,以及粘结力好的优点。
Description
本发明涉及高密度多层线路板封装材料领域,尤其涉及一种绝缘介质胶膜及其制备方法、多层印刷线路板。
随着人工智能的飞速发展,电子产品也逐渐向薄型化、高密度发展。高密度多层线路板通常作为移动电话、数码相机、手提电脑等便携式电子产品的封装基板,IC(集成电路)封装基板由有芯基板向更薄的无芯基板方向的发展,也使得高密度多层线路板的改进成为研究的热点。
高密度多层线路板是指在绝缘基板上、传统双面板或多层板上,采取玻璃布增强绝缘介质在经化学镀铜和电镀铜形成导线及连接孔,如此多次叠加,累积形成所需层数的多层印制线路板。传统的多层线路板制备工艺是通过在覆铜箔层压板表面上有选择性地除去部分铜箔来获得导电图形,这种做法工序多、控制难且成本高。
对于多层线路板而言,一般线宽/线间距低于40微米就无法保证线路品质了,而半导体芯片载板普遍线宽/线间距小于15微米。目前解决的方案只有采用半加成法(SAP)或改进型半加工法(MSAP),这也是当今HDI(高密度互联多层线路板)最先进的制成工艺。半加成法的技术关键便是积层材料-绝缘薄膜材料,也就是日本味之素公司的ABF/GX系列产品,它主要采用环氧及固化剂以及热塑性酚氧树脂来担当成膜作用。在一定厚度PET承载膜上涂一定厚度胶液后,经过红外加热或热风使溶剂干燥得到粘性薄膜,但是由于酚氧树脂是由酚扩链环氧而成,其所具有的大量醇羟基会严重影响绝缘介质的介电性能,在高频高速领域应用受限。
中国专利ZL201810631718.9利用聚氨酯丙烯酸酯树脂、甲基丙烯酸羟乙酯光固化来担当环氧树脂成膜组份,采用脂肪族环氧为主体无溶剂涂胶方式来制备绝缘介质膜,然而,无溶剂涂胶方式不太适合配方设计,而且该技术的阻燃性很差,热膨胀大。
ABF(绝缘介质)薄膜材料所要求的表面低粗化度、低热膨胀率、低介质损耗及高玻璃转变温度等特性,国内目前还无法实现,因此我国的ABF薄膜材料一直依赖于进口,这就大大提高了多层线路板的成本,对我国线路板行业的健康发展极为不利。
因此,现有技术还有待于改进。
发明内容
鉴于上述现有技术的不足,本发明的目的在于提供一种绝缘介质胶膜及其制备方法、多层印刷线路板,旨在解决现有绝缘介质胶膜柔韧性差、介电常数较高、介电损耗因数高,以及易发生热膨胀的问题。
本发明的技术方案如下:
一种绝缘介质胶膜,其中,包括离型膜以及设置在离型膜表面的绝缘介质层,所述绝缘介质层材料包括饱和聚酯树脂、氨基树脂或封闭型异氰酸酯、环氧树脂、固化剂、无机填料以及固化促进剂。
所述的绝缘介质胶膜,其中,所述绝缘介质层材料按重量份计包括5-30份的饱和聚酯树脂、0.5-3份的氨基树脂或封闭型异氰酸酯、45-75份的环氧树脂、1-25份的固化剂、1-100份的无机填料以及0.1-5份的固化促进剂。
所述绝缘介质胶膜,其中,所述氨基树脂为三聚氰胺或苯代三聚氰胺与甲醛以及有机醇缩聚形成的树脂。
所述绝缘介质胶膜,其中,所述封闭型异氰酸酯为苯酚封闭的HDI、MDI、TDI以及PDI中的一种或多种;或者,所述封闭型异氰酸酯为己内酰胺封闭的HDI、MDI、TDI以及PDI中的一种或多种。
所述的绝缘介质胶膜,其中,所述环氧树脂选自双酚A环氧树脂、双酚F环氧树脂、DCPD环氧树脂、三酚环氧树脂、联苯环氧树脂、萘酚环氧树脂和含磷环氧树脂中的一种或多种。
所述绝缘介质胶膜,其中,所述固化剂选自双氰胺、芳香胺、酚类化合物、活性脂以及含磷酚醛中的一种或多种。
所述绝缘介质胶膜,其中,所述离型膜的厚度为10-100μm,所述绝缘介质层的厚度为10-200μm。
所述绝缘介质胶膜的制备方法,其中,包括步骤:
将氨基树脂或封闭型异氰酸酯加入饱和聚酯树脂溶液中,混合制得第一胶液;
向所述第一胶液中加入环氧树脂以及固化剂,混合制得第二胶液;
向所述第二胶液中加入无机填料和固化促进剂,混合制得第三胶液;
将所述第三胶液涂覆于离型膜上并进行固化处理,制得所述绝缘介质胶膜。
一种多层印刷线路板,其中,包括本发明所述的绝缘介质胶膜。
有益效果:本发明提供的绝缘介质胶膜包括离型膜以及设置在离型膜表面的绝缘介质层,所述绝缘介质层材料包括饱和聚酯树脂、氨基树脂或封闭型异氰酸酯、环氧树脂、固化剂、无机填料以及固化促进剂。本发明通过在环氧树脂组合物中引入饱和聚酯树脂组份,使得制得的绝缘介质胶膜具有介电常数低、介电损耗因数低以及粘结力好等优点。
图1为本发明提供的一种绝缘介质胶膜的制备方法较佳实施例的流程图。
本发明提供一种绝缘介质胶膜及其制备方法、多层印刷线路板,为使本发明的目的、技术方案及效果更加清楚、明确,以下对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
本发明实施例提供了一种绝缘介质胶膜,其包括离型膜以及设置在离型膜表面的绝缘介质层,所述绝缘介质层材料包括饱和聚酯树脂、氨基树脂或封闭型异氰酸酯、环氧树脂、固化剂、无机填料以及固化促进剂。
具体来讲,现有技术通常采用热塑型酚氧树脂与环氧树脂混合来制备绝缘介质薄膜,然而由于酚氧树脂是由酚扩链环氧而成,其具有大量的醇羟基,所述醇羟基的强极性会影响绝缘介质薄膜的介电性能。本实施例通过在环氧树脂中引入饱和聚酯树脂成分,所述饱和聚酯树脂是由多元醇和多元酸发生聚合反应制备而成,所述饱和聚酯树脂只在端部含有羟基基团,中间不含有极性的羟基基团,因此所述饱和聚酯树脂的极性较弱,其与环氧树脂混合形成的绝缘介质胶膜具有较低的介电常数和较低的介电损耗因数,因而具有较佳的介电性能;同时本实施例还在环氧树脂中引入了氨基树脂或封闭型异氰酸酯,所述氨基树脂或封闭型异氰酸酯可与饱和聚酯树脂发生交联反应,既能够去除饱和聚酯树脂两端的羟基,进一步降低饱和聚酯树脂的极性,提升介电性能,又能够增加饱和聚酯树脂的分子量,提升成膜效果。
在一些实施方式中,基于绝缘介质层的工艺性及最终的耐热、粘结以及介电性能等综合考虑,本实施例优选所述绝缘介质层材料按重量份计包括5-30份的饱和聚酯树脂、 0.5-3份的氨基树脂或封闭型异氰酸酯、45-75份的环氧树脂、1-25份的固化剂、1-100份的无机填料以及0.1-5份的固化促进剂,按本实施例配方制得的绝缘介质层具有优异的介电性能。
在一些实施方式中,所述饱和聚酯树脂的化学结构式为
其中,n为1-100,R1、R2独立地选自碳原子小于20的烷基、苯基、萘基或其组合基团。本实施例提供的饱和聚酯树脂具有优异的成膜性能,且所述饱和聚酯树脂含有少量的羟基,极性较弱,其与环氧树脂、氨基树脂或封闭型异氰酸酯、固化剂、无机填料以及固化促进剂混合制得的绝缘介质层具有较低的介电常数和介电损耗因数。
在一些优选的实施方式中,所述饱和聚酯树脂的相对分子量为8000-30000。若所述饱和聚酯树脂的相对分子量小于8000,则不利于成膜,若所述饱和聚酯树脂的相对分子量大于30000,则分子量过大导致溶解度过低,不利于与环氧树脂混合成膜。
在一些实施方式中,所述氨基树脂为三聚氰胺或苯代三聚氰胺与甲醛以及有机醇缩聚形成的树脂。在本实施例中,氨基树脂是一种多官能度的聚合物,其作为交联剂可与端部含有羟基的饱和聚酯树脂发生交联反应,从而增加饱和聚酯树脂的分子量,并降低所述饱和聚酯树脂的极性,增强绝缘介质层的介电性能。
在一些实施方式中,所述封闭型异氰酸酯为苯酚封闭的HDI、MDI、TDI以及PDI中的一种或多种,但不限于此。在本实施例中,所述封闭性异氰酸酯同样可作为交联剂与端部含有羟基的饱和聚酯树脂发生交联反应,从而增加饱和聚酯树脂的分子量,并降低所述饱和聚酯树脂的极性,增强绝缘介质层的介电性能。
在一些实施方式中,所述封闭型异氰酸酯为己内酰胺封闭的HDI、MDI、TDI以及PDI中的一种或多种,但不限于此。
在一些实施方式中,所述环氧树脂选自双酚A环氧树脂、双酚F环氧树脂、DCPD环氧树脂、三酚环氧树脂、联苯环氧树脂、萘酚环氧树脂和含磷环氧树脂中的一种或多种,但不限于此。在一些更优选的实施方式中,所述环氧树脂为含磷环氧树脂,所述含磷环氧树脂中的磷含量为2-5%,环氧当量为200-600g/mol。
在一些实施方式中,所述固化剂选自双氰胺、芳香胺、酚类化合物、活性脂以及含磷酚醛中的一种或多种,但不限于此。
在一些实施方式中,所述固化促进剂选自2-甲基咪唑、2-乙基-4甲基咪唑、2-苯基 咪唑、DMP-30、吡啶和对甲苯磺酸中的一种或多种,但不限于此。
在一些实施方式中,所述无机填料选自氢氧化铝、氢氧化镁、氧化铝、氮化硼、氮化铝、碳化硅、沸石、硅灰石、二氧化硅、氧化镁、硅酸钙、碳酸钙、粘土、滑石和云母中的一种或多种,但不限于此。在本实施例中,所述无机填料的量可以随使用目的作适当的剂量调整。在一种优选的实施方式中,所述绝缘介质层材料中包括25-100份的无机填料。
在一些实施方式中,所述离型膜的厚度为10-100μm,所述绝缘介质层的厚度为10-200μm。
在一些实施方式中,还提供一种绝缘介质胶膜的制备方法,其中,如图1所示,包括步骤:
S10、将氨基树脂或封闭型异氰酸酯加入饱和聚酯树脂溶液中,混合制得第一胶液;
S20、向所述第一胶液中加入环氧树脂以及固化剂,混合制得第二胶液;
S30、向所述第二胶液中加入无机填料和固化促进剂,混合制得第三胶液;
S40、将所述第三胶液涂覆于离型膜上并进行固化处理,制得所述绝缘介质胶膜。
在一些实施方式中,所述饱和聚酯树脂溶液包括有机溶剂以及分散在所述有机溶剂中的饱和聚酯树脂,所述有机溶剂选自丁酮和环己酮中的一种或两种。
在一些实施方式中,采用直接加热或热风的方式对涂覆在离型膜上的第三胶液进行固化处理,使所述第三胶液形成绝缘介质层。当采用直接加热的方式对所述第三胶液进行固化处理时,加热的温度根据第三胶液中的溶剂沸点来设置,其加热温度设置为80-130℃,加热时间为5-20min。
在一些实施方式中,还提供一种多层印刷线路板,其包括本发明所述的绝缘介质胶膜。
具体来讲,将所述绝缘介质胶膜与做好内层线路的PCB板在80-130℃,0.1-1MPa压力条件下贴合好,然后在真空压机里压制,压制温度为150-200℃,硬化时间为30-90分钟,压力为0.5~4MPa,制得所述多层印刷线路板。
下面通过实施例对本发明进行详细说明:
实施例1
取DYNAPOL LH826-05A(德国德固赛商品名,饱和聚酯树脂)20份,溶于异佛尔酮溶剂中,在常温或中温条件下完全溶解后加入HMMM(六甲氧甲基三聚氰胺)1份,搅拌一定时间备用溶液;再加入NPEL-128(二官能环氧树脂,南亚塑胶工业股份 有限公司商品名)30份、XZ 92530含磷环氧树脂35份,搅拌均匀,将固化剂双氰胺2.5份溶解于DMF溶剂后加入上述胶液中,加入球型二氧化硅50份加入上述胶液,充分搅拌分散,最后投入固化促进剂2-乙基-4甲基咪唑和BYK450若干,搅拌均匀待用。选取300×300cm、表面光洁、平整的38μm厚的PET离型膜,离型膜一面均匀涂覆上述胶液,在烘箱中120℃下烘烤7min制得粘结片。将2张绝缘膜叠加,置于真空热压机中170℃固化60分钟得到基材样品。
实施例2
取DYNAPOL L411 20份,溶于异佛尔酮溶剂中,在常温或中温条件下完全溶解后加入HMMM 1份,搅拌一定时间备用溶液;再加入NPEL-128二官能环氧30份、XZ 92530含磷环氧35份,搅拌均匀,将固化剂双氰胺2.5份溶解于DMF溶剂后加入上述胶液中,加入球型二氧化硅50份加入上述胶液,充分搅拌分散,最后投入固化促进剂2-乙基-4甲基咪唑和BYK450若干,搅拌均匀待用。选取300×300cm、表面光洁、平整的38μm厚的PET离型膜,离型一面均匀涂覆上述胶液,在烘箱中120℃下烘烤7min制得粘结片。将2张绝缘膜叠加,置于真空热压机中170℃固化60分钟得到基材样品。
实施例3
取DYNAPOL L411 20份,溶于异佛尔酮溶剂中,在常温或中温条件下完全溶解后加入Desmodur RL1265 1份,搅拌一定时间备用溶液;再加入NPEL-128二官能环氧30份、XZ 92530含磷环氧35份,搅拌均匀,将固化剂双氰胺2.5份溶解于DMF溶剂后加入上述胶液中,加入球型二氧化硅50份加入上述胶液,充分搅拌分散,最后投入固化促进剂2-乙基-4甲基咪唑若干,搅拌均匀待用。选取300×300cm、表面光洁、平整的38μm厚的PET离型膜,离型一面均匀涂覆上述胶液,在烘箱中120℃下烘烤7min制得粘结片。将2张绝缘膜叠加,置于真空热压机中170℃固化60分钟得到基材样品。
实施例4
取DYNAPOL L411 20份,溶于异佛尔酮溶剂中,在常温或中温条件下完全溶解后加入HMMM 1份,搅拌一定时间备用溶液;再加入NPEL-128二官能环氧30份、YEP250含磷环氧35份,搅拌均匀,将固化剂双氰胺1.5份、DDS 3份溶解于DMF溶剂后加入上述胶液中,加入球型二氧化硅50份加入上述胶液,充分搅拌分散,最后投入固化促进剂2-乙基-4甲基咪唑、三氟化硼乙胺和BYK450若干,搅拌均匀待用。选取300×300cm、表面光洁、平整的38μm厚的PET离型膜,离型一面均匀涂覆上述胶液,在烘箱中120℃下烘烤7min制得粘结片。将2张绝缘膜叠加,置于真空热压机中180℃固化60分钟得 到基材样品。
实施例5
取DYNAPOL L411 20份,溶于异佛尔酮溶剂中,在常温或中温条件下完全溶解后加入HMMM 1份,搅拌一定时间备用溶液;再加入NPEL-128二官能环氧30份、YEP250含磷环氧35份,搅拌均匀,将固化剂LA-705225份、DDS 3份溶解于PM溶剂后加入上述胶液中,加入球型二氧化硅50份加入上述胶液,充分搅拌分散,最后投入固化促进剂2-乙基-4甲基咪唑、三氟化硼乙胺和BYK450若干,选取300×300cm、表面光洁、平整的38μm厚的PET离型膜,离型一面均匀涂覆上述胶液,在烘箱中120℃下烘烤7min制得粘结片。将2张绝缘膜叠加,置于真空热压机中180℃固化60分钟得到基材样品。
对比例
取YL6747H3020份,加入NPEL-128二官能环氧30份、XZ 92530含磷环氧35份,搅拌均匀,将固化剂双氰胺2.5份溶解于DMF溶剂后加入上述胶液中,加入球型二氧化硅50份加入上述胶液,充分搅拌分散,最后投入固化促进剂2-乙基-4甲基咪唑若干,搅拌均匀待用。选取300×300cm、表面光洁、平整的38μm厚的PET离型膜,离型一面均匀涂覆上述胶液,在烘箱中120℃下烘烤7min制得粘结片。将2张绝缘膜叠加,置于真空热压机中170℃固化60分钟得到基材样品。
对上述实施例1-实施例5以及对比例中制得的基材样本进行性能测试,得到结果如表1所述:
表1基材样本性能测试结果
通过上述测试结果可知,本发明实施例提供的绝缘介质胶膜在满足成膜特性前提下能够降低介电常数、以及介电损耗因数,同时可满足玻璃化温度,热膨胀系数不明显劣化,且卤素含量在JPCA无卤标准要求范围内能达到难燃性试验UL 94中的V-0的标准。
综上所述,本发明提供的绝缘介质胶膜包括离型膜以及设置在离型膜表面的绝缘介质层,所述绝缘介质层材料包括饱和聚酯树脂、氨基树脂或封闭型异氰酸酯、环氧树脂、固化剂、无机填料以及固化促进剂。本发明通过在环氧树脂组合物中引入饱和聚酯树脂组份,使得制得的绝缘介质胶膜柔韧性极好、介电常数低、介电损耗因数低、不易发生热膨胀,且粘结力好。
应当理解的是,本发明的应用不限于上述的举例,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (10)
- 一种绝缘介质胶膜,其特征在于,包括离型膜以及设置在所述离型膜表面的绝缘介质层,所述绝缘介质层材料包括饱和聚酯树脂、氨基树脂或封闭型异氰酸酯、环氧树脂、固化剂、无机填料以及固化促进剂。
- 根据权利要求1所述的绝缘介质胶膜,其特征在于,所述绝缘介质层材料按重量份计包括5-30份的饱和聚酯树脂、0.5-3份的氨基树脂或封闭型异氰酸酯、45-75份的环氧树脂、1-25份的固化剂、1-100份的无机填料以及0.1-5份的固化促进剂。
- 根据权利要求1所述的绝缘介质胶膜,其特征在于,所述氨基树脂为三聚氰胺或苯代三聚氰胺与甲醛以及有机醇缩聚形成的树脂。
- 根据权利要去1所述绝缘介质胶膜,其特征在于,所述封闭型异氰酸酯为苯酚封闭的HDI、MDI、TDI以及PDI中的一种或多种;或者,所述封闭型异氰酸酯为己内酰胺封闭的HDI、MDI、TDI以及PDI中的一种或多种。
- 根据权利要求1所述的绝缘介质胶膜,其特征在于,所述环氧树脂选自双酚A环氧树脂、双酚F环氧树脂、DCPD环氧树脂、三酚环氧树脂、联苯环氧树脂、萘酚环氧树脂和含磷环氧树脂中的一种或多种。
- 根据权利要求1所述绝缘介质胶膜,其特征在于,所述固化剂选自双氰胺、芳香胺、酚类化合物、活性脂以及含磷酚醛中的一种或多种。
- 根据权利要求1所述绝缘介质胶膜,其特征在于,所述离型膜的厚度为10-100μm,所述绝缘介质层的厚度为10-200μm。
- 一种如权利要求1-8任一所述绝缘介质胶膜的制备方法,其特征在于,包括步骤:将氨基树脂或封闭型异氰酸酯加入饱和聚酯树脂溶液中,混合制得第一胶液;向所述第一胶液中加入环氧树脂以及固化剂,混合制得第二胶液;向所述第二胶液中加入无机填料和固化促进剂,混合制得第三胶液;将所述第三胶液涂覆于离型膜上并进行固化处理,制得所述绝缘介质胶膜。
- 一种多层印刷线路板,其特征在于,包括权利要求1-8任一所述的绝缘介质胶膜。
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