CN108570877A - A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg - Google Patents

A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg Download PDF

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Publication number
CN108570877A
CN108570877A CN201710148573.2A CN201710148573A CN108570877A CN 108570877 A CN108570877 A CN 108570877A CN 201710148573 A CN201710148573 A CN 201710148573A CN 108570877 A CN108570877 A CN 108570877A
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aramid fiber
aramid
glass fibre
circuit board
base prepreg
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刘德礼
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Nanjing Xinlai'er Mstar Technology Ltd
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Nanjing Xinlai'er Mstar Technology Ltd
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
    • D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
    • D21H15/10—Composite fibres
    • D21H15/12—Composite fibres partly organic, partly inorganic
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/002—Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/007—Modification of pulp properties by mechanical or physical means
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F13/00—Making discontinuous sheets of paper, pulpboard or cardboard, or of wet web, for fibreboard production
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/10—Organic non-cellulose fibres
    • D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H13/26—Polyamides; Polyimides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/36—Inorganic fibres or flakes
    • D21H13/38—Inorganic fibres or flakes siliceous
    • D21H13/40—Inorganic fibres or flakes siliceous vitreous, e.g. mineral wool, glass fibres
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/10—Coatings without pigments
    • D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • D21H19/16—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising curable or polymerisable compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/06—Paper forming aids
    • D21H21/08—Dispersing agents for fibres
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
    • D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
    • D21H23/22—Addition to the formed paper
    • D21H23/32—Addition to the formed paper by contacting paper with an excess of material, e.g. from a reservoir or in a manner necessitating removal of applied excess material from the paper

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Reinforced Plastic Materials (AREA)
  • Paper (AREA)

Abstract

The invention discloses a kind of manufacturing methods of high-frequency high-speed circuit board p-aramid fiber base prepreg.This method will use para-aramid fiber,Para-aramid pulp,Glass fibre etc. efficiently combines,It is chemically bonded by coupling agent,High efficiency dispersion and the fiber surface and interface of appropriateness are partly dissolved and weld,In combination with the respective material property advantage of aramid fiber and glass fibre,So that p-aramid fiber insulating trip or paper have certain intensity and porosity,After the completion of fully absorbing glue and immersing glue process,P-aramid fiber insulating trip or paper form the complex of " zero hole " compact texture,Its p-aramid fiber insulating trip or paper is set to be cross-linked with each other reaction using common curing process,Form high performance p-aramid fiber base prepreg,By the coefficient of thermal expansion for manufacturing experimently copper-clad plate,T 288 is tested,Glass transition point,Heat decomposition temperature,Plate prying degree,Sur-face peeling intensity,Thermal shock,Wicking performance,Dielectric constant,The requirement of the board productions index whole application technology such as dielectric loss factor.The patented technology method has the characteristics that simple for process, excellent product performance, environmental-friendly and at low cost, has boundless application prospect in high-frequency high-speed field of circuit boards.

Description

A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg
Technical field
The present invention relates to a kind of p-aramid fiber base prepregs, are transmitted more particularly to applied to electronic signal high-frequency high-speed Rigidity or flexible PCB p-aramid fiber base prepreg manufacturing method；P-aramid fiber base prepreg can be applicable to resistance to The fields such as high temperature, insulation and circuit board, including aerospace, high-frequency high-speed circuit board, military defense, warship, transformer, ship The high-tech areas such as oceangoing ship, guided missile, radar.
Background technology
P-aramid fiber base prepreg as a kind of novel high insulating property special type new material, in recent years it is military, The important application of civil field gradually expands.Although China's aramid insulating paper industry obtained development faster in recent years, But most domestic enterprise still has a long way to go still in lab scale and pilot scale stage with the technical merit of developed countries, part Key technology is still external related company monopolizing.
Current main aramid insulating paper is mainly manufactured by papermaking wet method papermaking process.Its primary raw material has two classes：One Class is that strand arranges the meta-aramid fibers being serrated, and China is referred to as aramid fiber 1313；One kind is strand arrangement in straight Linear para-aramid fiber, China is referred to as Fanglun l414.The aramid insulating paper high temperature resistant manufactured paper with pulp by meta-aramid fibers Performance is not so good as the aramid paper obtained by para-aramid fiber with insulation performance, therefore meta-aramid is selected to manufacture p-aramid fiber base Prepreg has the limitation much applied.However para-aramid fiber is wadded a quilt with cotton due to the stability of its structure, hydrophobicity and easily The features such as solidifying, causes the paper uniformity difference obtained by it even at paper difficulty.And the technological means that this is taken both at home and abroad at present Predominantly surface is modified, mainly face coat method, chemical modification and physical modification.At present by the way of more there are three types of： The first is handled using phosphoric acid, by etching rough surface in aramid fiber surface come so that between fiber mutually Connection generates combination to a certain extent, but phosphoric acid processing time and degree for the treatment of can not accurately control at present, and industrialization is difficult Degree is big.It is for second that fiber is handled using plasma method, it is similar with phosphoric acid facture, and generate on fiber big and small Pore space structure, but at present this method energy consumption it is too big, it is also difficult to industrialize.The third is exactly method of directly manufacturing paper with pulp, Chinese invention Patent application CN201310114147.9 discloses a kind of preparation method of printed circuit board p-aramid fiber paper base material, adopts The mode that aramid fiber manufactures paper with pulp into paper is discongested with the directly dispersion of bonus point powder, last reheating is molded.This method is due to fibre early period For dimension without passing through specially treated, the binding force between fiber is very poor, and the intensity of paper leans on later stage high temperature and pressure dissolving aramid fiber slurry entirely The dregs of rice are realized, and Fanglun slurry cake addition can influence the thermodynamic property such as coefficient of thermal expansion of aramid paper, degradation temperature etc. too much, with And the dip effect of resin, the porosity of aramid paper is too small to lead to that impregnation resin content is few and impregnation resin content is uneven, these can all cause Product is not applied for processing in next step, therefore is only used for low-grade circuit board, is not used to high-frequency circuit board.
Invention content
It is a primary object of the present invention to overcome the uneven handsheet of para-aramid fiber in the prior art, hydrophobicity, easily Flocculation, several key technology difficulty contents such as dielectric properties are weak provide a kind of simple for process, excellent product performance, environmental-friendly With the manufacturing method of low-cost novel p-aramid fiber base prepreg, high intensity, high temperature resistant, fire-retardant, heat-resisting punching are prepared It hits, the p-aramid fiber base prepreg of ultralow dielectric insulation performance, it is high to can be widely applied to electronic signal high frequency through scheduling and planning Speed transmission（1-10 GHz）The rigidity in field or the manufacture of flexible PCB.
P-aramid fiber insulating trip or paper are mainly applicable to heat safe insulating materials and filtering material at present, such as The insulating layer and some high temperature resistant filtration arts of for transformer inside and high ferro and aircraft, these p-aramid fiber insulating trips Or paper is all the technique using high temperature and pressure, directly allows Fanglun slurry cake melting crosslinked together, causes its porosity relatively low, this Invention p-aramid fiber base prepreg is applied to HF link plate substrate, it is desirable that p-aramid fiber insulating trip or paper quickly absorb high score The problem of subtree fat and control spread, the p-aramid fiber insulating trip or paper of low porosity are unfavorable for gluing, while also very big shadow The dielectric properties of p-aramid fiber insulating trip or paper are rung, therefore in order to ensure that p-aramid fiber insulating trip or paper reach impregnation requirement, it must While p-aramid fiber insulating trip or paper some strength must be assigned, also need to ensure its corresponding porosity and special reticular fibre Structure, up to standard to reach ideal spread, high temperature resistant, thermal shock resistance properties and coefficient of thermal expansion etc., the present invention is at the pre- place of early period The reason stage is partly dissolved and is welded by the fiber surface and interface of coupling agent chemical bonding, high efficiency dispersion and appropriateness, in combination with virtue The respective material property advantage of synthetic fibre fiber and glass fibre so that p-aramid fiber insulating trip or paper have certain intensity and hole Rate, after the completion of fully absorbing glue and immersing glue process, p-aramid fiber insulating trip or paper form " zero hole " compact texture and answer Zoarium makes its p-aramid fiber insulating trip or paper be cross-linked with each other reaction, it is fragrant to form high performance contraposition using common curing process Synthetic fibre base prepreg, it is curved by coefficient of thermal expansion, T-288 tests, glass transition point, heat decomposition temperature, the plate of manufacturing experimently copper-clad plate The board productions indexs such as set-back, sur-face peeling intensity, thermal shock, wicking performance, dielectric constant, dielectric loss factor all reach To application technology requirement.
The principle of the present invention is that first carrying out advanced treating to the surface of aramid fiber with acid or oxygenation pretreatment liquid makes its fibre Dimension table face is loosely organized and profit rises, and by coupling agent chemical bonding, high efficiency dispersion, after manufacturing paper with pulp into the scraps of paper, it is right that the present invention passes through Appropriate fiber surface and interface is carried out under scraps of paper implementation high-temperature and high-pressure conditions to be partly dissolved and weld certainly, by being partly dissolved and welding Process realizes adjusting and control to hole and fibrous reticular structure inside the scraps of paper, appropriate fiber surface and interface be partly dissolved with Welding, in combination with the respective material property advantage of aramid fiber and glass fibre so that p-aramid fiber insulating trip or paper have Certain intensity and porosity, after the completion of fully absorbing glue and immersing glue process, p-aramid fiber insulating trip or paper form " zero hole The complex of gap " compact texture makes its p-aramid fiber insulating trip or paper be cross-linked with each other reaction, is formed using common curing process High performance p-aramid fiber base prepreg.
Present invention discover that pure p-aramid paper is undesirable in terms of coefficient of thermal expansion, using glass fibre and it is a small amount of between Position aramid fiber, which is mixed in a certain ratio, can adjust the index, find that being not added with meta-aramid fibers equally might be used by improving later To reach effect.
The purpose of the present invention is achieved through the following technical solutions：
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：Aramid fiber, glass fibre are cut to one kind in length difference 2~5cm or 5~8cm Or the mixing of two kinds or several length fibers；
（2）The screening and cooperation of Fanglun slurry cake：Fanglun slurry cake is dispersed in water, fiber dispersion is further by pressurized screen Screening, takes the Fanglun slurry cake by 10~200 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material under the conditions of 80~120 DEG C of temperature Drying to moisture content is less than 3%；
（4）The configuration of pretreatment fluid：Any one of phosphorous acid, sodium hydroxide, ammonium hydroxide, phosphoric acid, hydrochloric acid, citric acid are dissolved Yu Shuizhong, be configured under the conditions of 10 DEG C~100 DEG C of temperature solid content account for aqueous solution mass fraction 1%~50% pretreatment it is molten Liquid；
（5）Pretreating process process：By step（3）Any one of, two kinds or more of mixture is in step（4）Middle institute The pretreatment fluid of configuration is pre-processed, and processing time is 10 seconds~90 minutes, and treatment temperature is 30~120 DEG C；
（6）Aramid fiber surface and interface is modified：By step（5）Pretreated aramid fiber, glass fibre and the pulp obtained Processing is dried, then surface and interface modification is carried out with coupling agent, treatment temperature is 20~200 DEG C, and processing time is 10 seconds ~240 minutes；
（7）Handsheet technique：It will be through step（6）Treated any one of aramid fiber, glass fibre, Fanglun slurry cake is mixed Object cleaning is closed to remove extra coupling agent, after be diluted with water the dense fiber dispersion for being 0.05~0.5% be slurried, and be added point Powder discongests 3000~100000 turns using dispersion machine or fluffer, and sheet material is manufactured paper with pulp into automatic paper machine vacuum；
（8）Paper is dried：It will be through step（7）P-aramid fiber based insulation piece obtained is dry under the conditions of 50~200 DEG C, after dry Insulating trip moisture content is less than 15%；
（9）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（8）Obtained p-aramid fiber based insulation piece is in a level pressure Densification is carried out under power, temperature condition, to obtain the fibre layered structure of certain porosity and air permeability, temperature is 20~ 300 DEG C, pressure is 1~50Mpa, and the time is 1 minute~60 minutes.Obtain p-aramid fiber based insulation piece；
（10）By step（9）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.By insulating resin and curing agent It is mixed according to proportioning, cures 1~12h, certain organic solvent and coupling agent is added, pass through vacuum high speed in above-mentioned reactive material After mixing, impregnation steps（10）The p-aramid fiber based insulation piece produced 1~60 second simultaneously takes out, and semi-solid preparation is carried out at 70~300 DEG C Processing, processing time are 1~60 minute, that is, obtain p-aramid fiber base prepreg.
Compared with prior art, the invention has the advantages that：
（1）A kind of manufacturing method of high-frequency high-speed circuit board high-performance p-aramid fiber base prepreg of the present invention has work Skill is simple, excellent product performance, it is environmental-friendly and of low cost the features such as；
（2）What a kind of high-frequency high-speed circuit board of the present invention was prepared with the manufacturing method of high-performance p-aramid fiber base prepreg Aramid insulating paper has the characteristics that high intensity, high temperature resistant, heat shock resistance, high fire-retardance and electrical insulation capability are excellent；
（3）The para-aramid fiber content that the technical method uses is significantly larger than existing technology of preparing, makes virtue by high temperature and pressure Synthetic fibre fiber surface and interface is partly dissolved and from welding, fills up pore structure, makes paper structure densification and smooth, final to be made A kind of p-aramid fiber base prepreg.
Description of the drawings：
It is aramid fiber based insulation piece material object picture on Fig. 1, is substrate of the fiber after aftershaping of manufacturing paper with pulp；
It is the aramid fiber base copper-clad plate after pressing plate under Fig. 1, is finished product of the aramid fiber insulation piece after impregnation pressing plate；
Fig. 2 is the aramid fiber base prepreg after impregnation, is semi-finished product of the aramid fiber based insulation piece by impregnation drying but also non-tabletting.
Specific implementation mode
In order to more deeply understand the present invention, with reference to embodiment, the present invention is further illustrated, needs to illustrate , the scope of protection of present invention be not limited to embodiment statement range.
In following example, coefficient of thermal expansion test uses GB/T 16535-2008 standard testings；T-288 thermal degradations It can test and use GB/T 11998-1989 testing standards；It removes inversion point test and heat decomposition temperature uses GB/T 27761- 2011 testing standards；Peel strength test is tested using GB/T 2791-1995 national standards；Thermal shock and wicking use GB/T 15727-1995 testing standards；Tensile strength test uses ISO7500-1 standard testings；Dielectric constant and dielectric loss factor are surveyed Pilot production GB/T 1693-2007 standard testings.
Embodiment 1
A kind of manufacturing method of high-frequency circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 7637 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 6cm, mass ratio 20%：80%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 20~100 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 60%：5%：35%；
（5）The configuration of pretreatment fluid：Phosphoric acid is dissolved in the water, being configured to solid content under the conditions of 80 DEG C of temperature accounts for aqueous solution matter Measure 10% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid is located in advance Reason, processing time are 30 minutes, and treatment temperature is 90 DEG C；
（7）Fiber surface and interface is modified：By step（6）Pretreated aramid fiber, glass fibre, the pulp obtained is done Dry processing, then carry out surface and interface stir process, treatment temperature 100 with methyltrimethoxysilane (model 6070) coupling agent DEG C, processing time is 30 minutes；
（8）Papermaking process：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.1% be slurried, and polyethylene glycol oxide is added （PEO）Dispersant, addition be aramid fiber, glass fibre, Fanglun slurry cake gross mass 2.5%.It is discongested using dispersion machine It 80000 turns, is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（8）P-aramid fiber based insulation piece obtained is dry under the conditions of 180 DEG C, insulate after dry Piece moisture content is 9.0%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is expected Temperature be 200 DEG C and pressure be 12Mpa under the conditions of the pressing time be 15 minutes under the conditions of carry out aramid fiber surface and interface be partly dissolved with Welding, to obtain fibrous reticular structure, obtains p-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 135g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.By epoxy resin and ammonium chloride It is 4 according to mass fraction:1 proportioning mixing, cures 10h, and it is 75 that mass ratio, which is added,:1 acetone organic solvent and methyl trimethoxy oxygen Base silane (6070 model) coupling agent is adjusted epoxy resin viscosity and its modified interfacial structure, is passed through in above-mentioned reactive material After vacuum mixed at high speed, impregnates p-aramid fiber based insulation piece 30 seconds and take out, semi-solid preparation processing, processing time are carried out at 120 DEG C It is 30 minutes, that is, obtains p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦2.842%；（2）T- 288 be the non-plate burstings of 9.41min；（3）Glass transition point TG is 169.2 DEG C -165.32 DEG C；（4）Heat decomposition temperature is 365.20 DEG C； （5）With the peel strength of copper foil gluing（Lb/in）For 9.5 Lb/9.7Lb；（6）Thermal shock（288℃）Cycle 10 times it is without exception； （7）Wicking（T=288℃）It is without exception for 300s；Dielectric constant（10.0GHz）It is 3.0；Dielectric dissipation factor（10.0GHz）For 0.0058。
Technical finesse by above-mentioned steps with manufacture paper with pulp, efficiently solve p-aramid fiber insulating trip or paper be difficult to efficient absorption The problem of macromolecule resin and control spread, pass through the fiber surface and interface portion of coupling agent chemical bonding, high efficiency dispersion and appropriateness Divide dissolving and welding, in combination with the respective material property advantage of aramid fiber and glass fibre so that p-aramid fiber insulating trip Or paper has certain intensity and porosity, after the completion of fully absorbing glue and immersing glue process, p-aramid fiber insulating trip or paper The complex for forming " zero hole " compact texture, makes its p-aramid fiber insulating trip or paper be cross-linked with each other using common curing process Reaction, forms high performance p-aramid fiber base prepreg；By detection, main performance index is as shown in table 1, includes mainly Coefficient of thermal expansion, T-288 tests, glass transition point, heat decomposition temperature, sur-face peeling intensity, thermal shock, wicking performance, dielectric Constant, dielectric loss factor, performance indicator are substantially better than existing commercial aramid fiber based insulation prepreg（CEM-3 semi-solid preparations Piece, Huizhou conjunction positive electron Co., Ltd, prepreg model M-528, as shown in table 1）；It can be seen that by 1 comparative analysis of table The present embodiment p-aramid fiber base prepreg is than existing commercial aramid fiber based insulation prepreg（CEM-3 prepregs, Huizhou are closed Positive electron Co., Ltd, prepreg model M-528）With significant advantage.Such as：1 p-aramid fiber base of the present embodiment half is solid Change piece hot property（Include mainly coefficient of thermal expansion, thermal shock, T-288, glass transition point, heat decomposition temperature, thermal shock and leaching Tin）Be significantly higher than existing commercial aramid fiber based insulation prepreg, show preconditioning technique that it matches and aramid fiber with Glass fibre doping can effectively realize the fabulous compatibility and structural regularity for forming each material, and thermal property is for covering copper The properties of plate or high-frequency high-speed substrate have vital influence.After the present embodiment technical finesse, semi-solid preparation The adhesion strength of sheet material and copper foil is greatly improved to 9.5 Lb/9.7Lb, and the high-frequency high-speed for developing high-quality has ten substantially Point crucial effect because aramid fiber insulation piece due to the chemical inertness of itself, is not easy to be modified, cause the binding force of itself and copper foil compared with Difference, lower peel strength frequently can lead to copper foil in subsequent etch processing and boring procedure and fall off, so as to cause circuit board Failure.For coefficient of thermal expansion and thermal shock resistance properties, the two indexs be also it is closely bound up with the modified effect of aramid fiber, due to Aramid fiber is heated to will produce thermals contraction, and copper foil, which is heated, to be expanded, therefore since the difference of coefficient of thermal expansion can be in thermal histories Opposite direction movement, generation pulls power and can directly result in plank plate bursting, thus how aramid fiber base prepreg and copper foil reach It needs to consider various modified conditions to an equilibrium system；The p-aramid fiber base prepreg that the present embodiment obtains has non- The dielectric properties of Chang Youyi, dielectric constant and dielectric loss factor under the conditions of electronic signal transmission speed is 10.0GHz Main difference well below existing commercial aramid fiber based insulation prepreg high frequency plate and low frequency plate is that frequency, also It is related to dielectric constant and dielectric loss factor, dielectric constant directly determines that circuit board can respond how high frequency, The data of the higher transmission per unit of time of frequency are more while being also not easily disturbed, and dielectric loss factor directly determines signal Decaying and integrality, dielectric loss factor are too high to causing dropout or transmission range to reduce.
1 the present embodiment p-aramid fiber base prepreg of table and traditional commodities aramid fiber based insulation prepreg performance test knot Fruit
Embodiment 2
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：Para-aramid fiber is cut to the composite fibre that length distinguishes 4cm and 7cm, mass ratio Example is 30%：70%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 40~90 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）Middle aramid fiber, glass fibre, pulp material mass ratio be 65%：0%：35%；
（5）The configuration of pretreatment fluid：By ammonia solvent in water, it is configured to solid content under the conditions of temperature 50 C and accounts for aqueous solution matter Measure 12% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid is located in advance Reason, processing time are 45 minutes, and treatment temperature is 50 DEG C；
（7）Fiber surface and interface is modified：By step（6）Processing is dried in the pretreated aramid fiber and pulp obtained, Again surface and interface stir process, treatment temperature 90 are carried out with γ-aminopropyl triethoxysilane (550 models of KH) coupling agent DEG C, processing time is 130 minutes；
（8）Handsheet technique：It will be through step（8）It treated aramid fiber and is cleaned in Fanglun slurry cake to remove extra idol Join the residues such as agent, after be diluted with water the dense fiber dispersion for mass concentration 0.2% be slurried, and nonionic polyacrylamide is added Amine（PAM）Dispersant, addition be aramid fiber, Fanglun slurry cake gross mass 1.5%.90000 turns are discongested using dispersion machine, is used Automatic paper machine vacuum is manufactured paper with pulp molding；
（9）The scraps of paper are dried：It will be through step（8）P-aramid fiber based insulation piece obtained is dry under the conditions of 190 DEG C, insulate after dry Piece moisture content is 10%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is expected Temperature is 210 DEG C, pressure 15Mpa, and the time is to carry out densification under the conditions of 12 minutes, to obtain fibre layered structure. Obtain p-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 100g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.By polyimide resin and 4, 4 '-diaminodiphenylsulfones (DDS) are 4 according to mass fraction:1 proportioning mixing, cures 2h, and it is 75 that mass ratio, which is added,:1 acetone Organic solvent and methyltrimethoxysilane (6070 model) coupling agent are adjusted epoxy resin viscosity and its modified interface is tied Structure, after above-mentioned reactive material is by vacuum mixed at high speed, dipping p-aramid fiber based insulation piece 40 seconds simultaneously takes out, 230 DEG C into The processing of row semi-solid preparation, processing time are 15 minutes, that is, obtain p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦3.242%；（2）T- 288 be the non-plate burstings of 8.4min；（3）Glass transition point TG is 165.2 DEG C -167.4 DEG C；（4）Heat decomposition temperature is 365.20 DEG C； （5）With the peel strength of copper foil gluing（Lb/in）For 8.5 Lb/9.1Lb；（6）Thermal shock（288℃）Cycle 11 times it is without exception； （7）Wicking（T=288℃）It is without exception for 350s；Dielectric constant（10.0GHz）It is 3.6；Dielectric dissipation factor（10.0GHz）For 0.0068。
Embodiment 3
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 1506 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 7cm, mass ratio 25%：75%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 20~100 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 50%：10%：40%；
（5）The configuration of pretreatment fluid：Phosphoric acid is dissolved in the water, being configured to solid content under the conditions of 80 DEG C of temperature accounts for aqueous solution matter Measure 25% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid is located in advance Reason, processing time are 45 minutes, and treatment temperature is 50 DEG C；
（7）Aramid fiber surface and interface is modified：By step（6）Pretreated aramid fiber, glass fibre and the pulp obtained It is dried processing, then with γ-aminopropyl triethoxysilane (550 models of KH) coupling agent and its alcohol mixeding liquid（Quality Than being 1:100）Surface and interface stir process is carried out, treatment temperature is 90 DEG C, and processing time is 130 minutes；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.2% be slurried, and nonionic polypropylene is added Amide（PAM）Dispersant, addition be aramid fiber, glass fibre and Fanglun slurry cake gross mass 1.5%.It is dredged using dispersion machine 90000 turns of solution is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（8）P-aramid fiber based insulation piece obtained is dry under the conditions of 190 DEG C, insulate after dry Piece moisture content is 10%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is expected Temperature is 190 DEG C, pressure 16Mpa, and the time is to carry out densification under the conditions of 15 minutes, to obtain fibre layered structure, Obtain p-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 75g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.By polyphenylene oxide resin and triolefin Base isocyanuric acid ester is 4 according to mass fraction:1 proportioning mixing, cures 2h, and it is 75 that mass ratio, which is added,:1 acetone organic solvent and Methyltrimethoxysilane (550 models of KH) coupling agent is adjusted epoxy resin viscosity and its modified interfacial structure, above-mentioned It after reactive material is by vacuum mixed at high speed, impregnates p-aramid fiber based insulation piece 40 seconds and takes out, carried out at semi-solid preparation at 230 DEG C Reason, processing time are 30 minutes, that is, obtain p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦2.952%；（2）T- 288 be the non-plate burstings of 9.6min；（3）Glass transition point TG is 164.2 DEG C -165.4 DEG C；（4）Heat decomposition temperature is 369.20 DEG C； （5）With the peel strength of copper foil gluing（Lb/in）For 8.8 Lb/9.6Lb；（6）Thermal shock（288℃）Cycle 10 times it is without exception； （7）Wicking（T=288℃）It is without exception for 355s；Dielectric constant（10.0GHz）It is 3.1；Dielectric dissipation factor（10.0GHz）For 0.0055。
Embodiment 4
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 1506 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 7cm, mass ratio 20%：80%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 10~90 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 40%：20%：40%；
（5）The configuration of pretreatment fluid：By dissolving with hydrochloric acid in water, it is configured to solid content under the conditions of temperature 60 C and accounts for aqueous solution matter Measure 45% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid is located in advance Reason, processing time are 45 minutes, and treatment temperature is 120 DEG C；
（7）Aramid fiber surface and interface is modified：By step（6）Pretreated aramid fiber, glass fibre and the pulp obtained Processing is dried, then uses N-2-（Aminoethyl）- 3- aminopropyl trimethoxysilanes (KH792 models) coupling agent and its ethyl alcohol, Water mixed liquid（Mass ratio is 1:100：100）Surface and interface stir process is carried out, treatment temperature is 190 DEG C, and processing time is 180 points Clock；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.2% be slurried, and polyethylene glycol is added（PEG） Dispersant, addition be aramid fiber, Fanglun slurry cake gross mass 1.5%.90000 turns are discongested using dispersion machine, with automatic copy paper Machine vacuum is manufactured paper with pulp molding；
（9）Paper is dried：It will be through step（8）P-aramid fiber based insulation piece obtained is dry under the conditions of 190 DEG C, insulate after dry Piece moisture content is 10%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is expected Temperature is 100 DEG C, pressure 10Mpa, and the time is to carry out densification under the conditions of 20 minutes, to obtain fibre layered structure. Obtain p-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 45g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.By cyanate ester resin and February Dilaurylate is 4 according to mass fraction:1 proportioning mixing, cures 6h, and it is 75 that mass ratio, which is added,:1 acetone is organic molten Agent and N-2-（Aminoethyl）- 3- aminopropyl trimethoxysilanes (KH792 models) coupling agent adjusted epoxy resin viscosity and Its modified interfacial structure.After above-mentioned reactive material is by vacuum mixed at high speed, impregnates p-aramid fiber based insulation piece 40 seconds and take Go out, semi-solid preparation processing is carried out at 200 DEG C, processing time is 40 minutes, that is, obtains p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦2.242%；（2）T- 288 be the non-plate burstings of 10.6min；（3）Glass transition point TG is 168.2 DEG C -169.4 DEG C；（4）Heat decomposition temperature is 362.7 DEG C； （5）With the peel strength of copper foil gluing（Lb/in）For 10.5 Lb/11.1Lb；（6）Thermal shock（288℃）It recycles 13 times and is no different Often；（7）Wicking（T=288℃）It is without exception for 360s；Dielectric constant（10.0GHz）It is 3.3；Dielectric dissipation factor（10.0GHz） It is 0.0071.
Embodiment 5
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 7615 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 7cm, mass ratio 10%：90%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 20~190 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 40%：10%：50%；
（5）The configuration of pretreatment fluid：Sodium hydroxide is dissolved in the water, be configured under the conditions of temperature 70 C solid content account for it is water-soluble 25% preprocessing solution of liquid mass fraction；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid is located in advance Reason, processing time are 45 minutes, and treatment temperature is 120 DEG C；
（7）Aramid fiber surface and interface is modified：By step（6）Pretreated aramid fiber, glass fibre and the pulp obtained It is dried processing, then with γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent and its water are mixed Close liquid（Mass ratio is 1:100）Surface and interface stir process is carried out, treatment temperature is 110 DEG C, and processing time is 240 minutes；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.3% be slurried, and polyethylene glycol oxide is added （PEO）Dispersant, addition be aramid fiber, glass fibre, Fanglun slurry cake gross mass 1.5%.It is discongested using dispersion machine It 80000 turns, is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（8）P-aramid fiber based insulation piece obtained is dry under the conditions of 190 DEG C, insulate after dry Piece moisture content is 10%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is expected Temperature is 100 DEG C, pressure 10Mpa, and the time is to carry out densification under the conditions of 20 minutes, to obtain fibre layered structure. Obtain p-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 145g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.By thermoplastic phenolic resin with Hexamethylenetetramine is 10 according to mass fraction:1 proportioning mixing, cures 1h, and it is 75 that mass ratio, which is added,:1 acetone organic solvent With γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent is adjusted epoxy resin viscosity and is changed Its interfacial structure of property.After above-mentioned reactive material is by vacuum mixed at high speed, impregnates p-aramid fiber based insulation piece 50 seconds and takes out, Semi-solid preparation processing is carried out at 230 DEG C, processing time is 15 minutes, that is, obtains p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦2.242%；（2）T- 288 be the non-plate burstings of 10.6min；（3）Glass transition point TG is 168.2 DEG C -169.4 DEG C；（4）Heat decomposition temperature is 362.7 DEG C； （5）With the peel strength of copper foil gluing（Lb/in）For 10.5 Lb/11.1Lb；（6）Thermal shock（288℃）It recycles 13 times and is no different Often；（7）Wicking（T=288℃）It is without exception for 360s；Dielectric constant（10.0GHz）It is 3.3；Dielectric dissipation factor（10.0GHz） It is 0.0071.
Embodiment 6
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By aramid fiber（Including p-aramid fiber and meta-aramid）, 1080 type glass fibre of electron level It is cut to the composite fibre of length difference 3cm and 7cm, mass ratio 70%：30%.P-aramid fiber is fine wherein in aramid fiber The mass ratio of dimension and meta-aramid fibers is 90%：10%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 30~180 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, 1080 type glass fibre of electron level and para-aramid pulp raw material exist It is 2% or less to be dried under the conditions of 100 DEG C of temperature to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 80%：10%：10%；
（5）The configuration of pretreatment fluid：Phosphorous acid is dissolved in the water, being configured to solid content under the conditions of 80 DEG C of temperature accounts for aqueous solution 15% preprocessing solution of mass fraction；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid is located in advance Reason, processing time are 145 minutes, and treatment temperature is 80 DEG C；
（7）Aramid fiber surface and interface is modified：By step（6）Pretreated aramid fiber, glass fibre and the pulp obtained It is dried processing, then with γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane (560 models of KH) coupling agents and its second Alcohol mixed liquor（Mass ratio is 1:200）Surface and interface stir process is carried out, treatment temperature is 110 DEG C, and processing time is 240 minutes；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.3% be slurried, and polyethylene glycol oxide is added （PEO）Dispersant, addition be aramid fiber, glass fibre, Fanglun slurry cake gross mass 2.5%.It is discongested using dispersion machine It 90000 turns, is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（8）P-aramid fiber based insulation piece obtained is dry under the conditions of 180 DEG C, insulate after dry Piece moisture content is 9%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is expected Temperature is 220 DEG C, pressure 12Mpa, and the time is to carry out densification under the conditions of 15 minutes, to obtain fibre layered structure. Obtain p-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 175g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.Melmac is added Mass ratio is 75:1 acetone organic solvent and γ-(the third oxygen of 2,3- epoxies) propyl trimethoxy silicane (560 models of KH) is even Connection agent is adjusted epoxy resin viscosity and its modified interfacial structure.After above-mentioned reactive material is by vacuum mixed at high speed, leaching Stain p-aramid fiber based insulation piece 30 seconds simultaneously takes out, and semi-solid preparation processing is carried out at 80 DEG C, and processing time is 30 minutes, that is, is aligned Aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦4.942%；（2）T- 288 be the non-plate burstings of 6.6min；（3）Glass transition point TG is 135.2 DEG C -141.3 DEG C；（4）Heat decomposition temperature is 358.6 DEG C；（5） With the peel strength of copper foil gluing（Lb/in）For 11.4 Lb/11.8Lb；（6）Thermal shock（288℃）Cycle 15 times it is without exception； （7）Wicking（T=288℃）It is without exception for 369s；Dielectric constant（10.0GHz）It is 2.9；Dielectric dissipation factor（10.0GHz）For 0.0058。
Embodiment 7
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 1080 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 7cm, mass ratio 60%：40%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 20~150 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 30%：20%：50%；
（5）The configuration of pretreatment fluid：By ammonia solvent in water, under the conditions of 90 DEG C of temperature being configured to solid content accounts for aqueous solution matter Measure 45% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid carries out ultrasound Wave pre-processes, and processing time is 145 minutes, and treatment temperature is 90 DEG C；
（7）Aramid fiber surface and interface modificationization：By step（6）Pretreated aramid fiber, glass fibre and the slurry obtained The dregs of rice are dried processing, then with γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent and its second Alcohol mixed liquor（Mass ratio is 1:100）Surface and interface stir process is carried out, treatment temperature is 80 DEG C, and processing time is 120 minutes；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.3% be slurried, and cation polypropylene is added Amide（PAM）Dispersant, addition be aramid fiber, glass fibre, Fanglun slurry cake gross mass 3.5%.It is discongested using dispersion machine It 100000 turns, is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（9）P-aramid fiber based insulation piece obtained is dry under the conditions of 150 DEG C, insulate after dry Piece moisture content is 3%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is in temperature It it is 250 DEG C, pressure 15Mpa, the time is to carry out densification under the conditions of 15 minutes, to obtain fibre layered structure.It obtains P-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 185g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.Epoxy resin modification will be gathered Phenylene ether resins are 10 according to mass fraction with dicy-curing agent:1 proportioning mixing, cures 2h, and it is 75 that mass ratio, which is added,:The third of 1 Ketone organic solvent and γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent is adjusted asphalt mixtures modified by epoxy resin Fat viscosity and its modified interfacial structure.After above-mentioned reactive material is by vacuum mixed at high speed, p-aramid fiber based insulation piece is impregnated It 30 seconds and takes out, semi-solid preparation processing is carried out at 138 DEG C, processing time is 40 minutes, that is, obtains p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦2.942%；（2）T- 288 be the non-plate burstings of 8.6min；（3）Glass transition point TG is 161.8 DEG C -169.6 DEG C；（4）Heat decomposition temperature is 348.8 DEG C；（5） With the peel strength of copper foil gluing（Lb/in）For 10.6 Lb/10.2Lb；（6）Thermal shock（288℃）Cycle 12 times it is without exception； （7）Wicking（T=288℃）It is without exception for 361s；Dielectric constant（10.0GHz）It is 3.1；Dielectric dissipation factor（10.0GHz）For 0.0055。
Embodiment 8
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 1080 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 6cm, mass ratio 80%：20%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 10~120 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 60%：5%：35%；
（5）The configuration of pretreatment fluid：Phosphoric acid is dissolved in the water, solid content is configured under the conditions of temperature 70 C and accounts for aqueous solution matter Measure 45% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid carries out ultrasound Wave pre-processes, and processing time is 100 minutes, and treatment temperature is 80 DEG C；
（7）Aramid fiber surface and interface modificationization：By step（6）Pretreated aramid fiber, glass fibre and the slurry obtained The dregs of rice are dried processing, then with γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent and its second Alcohol mixed liquor（Mass ratio is 1:200）Surface and interface stir process is carried out, treatment temperature is 70 DEG C, and processing time is 100 minutes；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.25% be slurried, and cation polypropylene is added Amide（PAM）Dispersant, addition be aramid fiber, glass fibre, Fanglun slurry cake gross mass 2.5%.It is discongested using dispersion machine It 80000 turns, is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（9）P-aramid fiber based insulation piece obtained is dry under the conditions of 110 DEG C, insulate after dry Piece moisture content is 3%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is in temperature It it is 220 DEG C, pressure 12Mpa, the time is to carry out densification under the conditions of 10 minutes, to obtain fibre layered structure.It obtains P-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 45g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.Epoxy resin modification will be gathered Phenylene ether resins are 10 according to mass fraction with dicy-curing agent:1 proportioning mixing, cures 2h, and it is 75 that mass ratio, which is added,:The third of 1 Ketone organic solvent and γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent is adjusted asphalt mixtures modified by epoxy resin Fat viscosity and its modified interfacial structure.After above-mentioned reactive material is by vacuum mixed at high speed, p-aramid fiber based insulation piece is impregnated It 30 seconds and takes out, semi-solid preparation processing is carried out at 138 DEG C, processing time is 40 minutes, that is, obtains p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦3.245%；（2）T- 288 be the non-plate burstings of 9.6min；（3）Glass transition point TG is 166.7 DEG C -169.5 DEG C；（4）Heat decomposition temperature is 355.7 DEG C；（5） With the peel strength of copper foil gluing（Lb/in）For 11.5 Lb/12.2Lb；（6）Thermal shock（288℃）Cycle 11 times it is without exception； （7）Wicking（T=288℃）It is without exception for 355s；Dielectric constant（10.0GHz）It is 3.5；Dielectric dissipation factor（10.0GHz）For 0.0075。
Embodiment 9
A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, includes the following steps and process conditions：
（1）The cutting of aramid fiber：By para-aramid fiber, 7637 type glass fibre of electron level be cut to length difference 3cm and The composite fibre of 6cm, mass ratio 90%：10%；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp is dispersed in water, by its dispersion liquid by pressurized screen into one Step screening, takes the Fanglun slurry cake by 10~120 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material it is dry under the conditions of 100 DEG C of temperature It is 2% or less to moisture content；
（4）In step（3）The mass ratio of middle aramid fiber, glass fibre and pulp material is 60%：0%：40%；
（5）The configuration of pretreatment fluid：Phosphoric acid is dissolved in the water, solid content is configured under the conditions of temperature 70 C and accounts for aqueous solution matter Measure 45% preprocessing solution of score；
（6）Pretreating process process：By step（4）In mixture in step（5）Middle configured pretreatment fluid carries out ultrasound Wave pre-processes, and processing time is 100 minutes, and treatment temperature is 80 DEG C；
（7）Aramid fiber surface and interface modificationization：By step（6）Pretreated aramid fiber, glass fibre and the slurry obtained The dregs of rice are dried processing, then with γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent and its second Alcohol mixed liquor（Mass ratio is 1:200）Surface and interface stir process is carried out, treatment temperature is 70 DEG C, and processing time is 100 minutes；
（8）Handsheet technique：It will be through step（7）It is cleaned in treated aramid fiber, glass fibre and Fanglun slurry cake to go Except residues such as extra coupling agents, after be diluted with water the dense fiber dispersion for being 0.25% be slurried, and cation polypropylene is added Amide（PAM）Dispersant, addition be aramid fiber, glass fibre, Fanglun slurry cake gross mass 2.5%.It is discongested using dispersion machine It 80000 turns, is manufactured paper with pulp molding with automatic paper machine vacuum；
（9）Paper is dried：It will be through step（9）P-aramid fiber based insulation piece obtained is dry under the conditions of 110 DEG C, insulate after dry Piece moisture content is 3%；
（10）Aramid fiber surface and interface is partly dissolved and welding procedure：It will be through step（9）Obtained p-aramid fiber based insulation piece is in temperature It it is 220 DEG C, pressure 12Mpa, the time is to carry out densification under the conditions of 10 minutes, to obtain fibre layered structure.It obtains P-aramid fiber based insulation piece.The grammes per square metre for the p-aramid fiber based insulation piece produced is 45g/m2；
（11）By step（10）The p-aramid fiber based insulation piece of making carries out semi-solid preparation process.Epoxy resin modification will be gathered Phenylene ether resins are 10 according to mass fraction with dicy-curing agent:1 proportioning mixing, cures 2h, and it is 75 that mass ratio, which is added,:The third of 1 Ketone organic solvent and γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH) coupling agent is adjusted asphalt mixtures modified by epoxy resin Fat viscosity and its modified interfacial structure.After above-mentioned reactive material is by vacuum mixed at high speed, p-aramid fiber based insulation piece is impregnated It 30 seconds and takes out, semi-solid preparation processing is carried out at 138 DEG C, processing time is 40 minutes, that is, obtains p-aramid fiber base prepreg.
The technical indicator of p-aramid fiber base prepreg is after testing：（1）Coefficient of thermal expansion（CTE）≦3.221%；（2）T- 288 be the non-plate burstings of 9.6min；（3）Glass transition point TG is 166.8 DEG C -168.2 DEG C；（4）Heat decomposition temperature is 355.8 DEG C；（5） With the peel strength of copper foil gluing（Lb/in）For 12.1 Lb/12.5Lb；（6）Thermal shock（288℃）Cycle 11 times it is without exception； （7）Wicking（T=288℃）It is without exception for 365s；Dielectric constant（10.0GHz）It is 3.0；Dielectric dissipation factor（10.0GHz）For 0.0058。

Claims (8)

1. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg, it is characterised in that include the following steps And process conditions：
（1）The cutting of fiber：By aramid fiber and glass fibre be cut to length difference 2~5cm or 5~8cm in one kind or The mixing of two kinds of length fibers；The aramid fiber is para-aramid fiber or the aramid fiber is p-aramid fiber fibre Peacekeeping meta-aramid fibers；
（2）The screening and cooperation of Fanglun slurry cake：Para-aramid pulp or meta-aramid pulp are dispersed in water, pressurized screen is passed through Further screening, takes the Fanglun slurry cake by 10~200 mesh to be used as raw material；
（3）By step（1）、（2）In obtained aramid fiber, glass fibre and pulp material under the conditions of 80~120 DEG C of temperature Drying to moisture content is less than 3%；The weight ratio of aramid fiber, glass fibre and Fanglun slurry cake is（10~90%）：（0~20%）： （1~50%）；
（4）The configuration of pretreatment fluid：It will be one or more in phosphorous acid, sodium hydroxide, ammonium hydroxide, phosphoric acid, hydrochloric acid and citric acid Be dissolved in the water, be configured under the conditions of 10 DEG C~100 DEG C of temperature solid content account for aqueous solution quality 1%~50% pretreatment it is molten Liquid；
（5）Pretreatment：By step（3）Products therefrom is placed in step（4）It is pre-processed in middle configured pretreatment fluid, it is pre- to locate It is 10 seconds~90 minutes to manage the time, and pretreatment temperature is 30~120 DEG C；
（6）Aramid fiber surface and interface functionalization：By step（5）Pretreated aramid fiber, glass fibre and the slurry obtained The dregs of rice are dried processing, then carry out surface and interface functionalization with coupling agent, and treatment temperature is 20~200 DEG C, and processing time is 10 seconds~240 minutes；
（7）Papermaking process：It will be through step（6）Treated aramid fiber, glass fibre, Fanglun slurry cake wash with water, with removal Extra coupling agent, after be diluted with water be slurried a concentration of 0.05~0.5% fiber dispersion, and dispersant is added, using dispersion Machine or fluffer are discongested with 3000~100000r/min rotating speeds, are manufactured paper with pulp molding with automatic paper machine vacuum；
（8）Paper is dried：It will be through step（7）P-aramid fiber based insulation piece obtained is dry under the conditions of 50~200 DEG C, after dry Insulating trip moisture content is less than 3%；
（9）Tablet forming technique：It will be through step（8）Obtained p-aramid fiber based insulation piece temperature be 20~300 DEG C, pressure be 1~ 50Mpa, processing time are that the processing of fine and close and dissolution of partial fiber surfaceization is carried out under conditions of 1~60 minute, to obtain air permeability as 2 The p-aramid fiber based insulation piece of the fibre layered structure of~30ml/min；
（10）By step（9）The p-aramid fiber based insulation piece of making carries out varnished insulation resin treatment；By insulating resin and solidification Agent is according to 1：0.2~1：0.5 proportioning mixing, is added is equivalent to insulating resin and curing agent gross mass 1%~10% after evenly mixing Acetone and 0.1%~10% coupling agent, configure resin solution；It is molten that the p-aramid fiber based insulation piece produced is impregnated in resin 1~60 second in liquid, it is placed in 70~300 DEG C of drying boxes and processing is dried, obtain p-aramid fiber base prepreg.
2. the high-frequency high-speed circuit board manufacturing method of p-aramid fiber base prepreg according to claim 1, feature It is：The para-aramid fiber of use is poly(p-phenylene terephthalamide), and the meta-aramid fibers of use are poly- isophthalic diformazans Acyl p-phenylenediamine；Para-aramid pulp（Poly(p-phenylene terephthalamide)）, meta-aramid pulp（Phenyl-diformyl isophthalic two between poly- Amine）Any one of or both mixture；
The glass fibre of use is electron level alkali-free glass fibre or fiber cloth or fiber mat, specification 7637,7630,7628, Any type of 7615,1506,2116,2113,3313,1080,106,104 models or two or more composite fibre；
When aramid fiber and fiberglass fibers are the mixture of the two length, length is 2~5cm and length is the two of 5~8cm Fiber mass values are（10~80%）：（10~60%）.
3. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg according to claim 1, It is characterized in that, the silane coupling agent is methyltrimethoxysilane (6070 model), γ-aminopropyl triethoxysilane (550 models of KH), γ-(the third oxygen of 2,3- epoxies) propyl trimethoxy silicane (560 models of KH), γ-（Methacryl Oxygen）Propyl trimethoxy silicane (570 models of KH), N-2-（Aminoethyl）- 3- aminopropyl trimethoxysilanes (KH792 models) In it is one or more；The addition of coupling agent be para-aramid fiber, glass fibre, Fanglun slurry cake gross mass 0.1~ 10%。
4. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg according to claim 1, It is characterized in that, the dispersant is polyethylene glycol oxide（PEO）, polyethylene glycol（PEG）And polyacrylamide（PAM）It is middle a kind of or A variety of mixtures.
5. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg according to claim 1, Be characterized in that, the pretreatment and with coupling agent carry out surface and interface functionalization all include impregnate, stirring, microwave treatment and It is one or more in ultrasonication.
6. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg according to claim 1, It is characterized in that, the insulating resin includes epoxy resin, polyimide resin, polyphenylene oxide resin, cyanate ester resin, phenolic aldehyde tree Any one or more of fat, isocyanate resin and melmac.
7. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg according to claim 1, It is characterized in that, the organic solvent includes mainly any one of acetone, butanone, ether, is mainly used for diluting insulating resin Or reduce resin viscosity.
8. a kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg according to claim 1, It is characterized in that adaptable coupling agent to be also added in resin, includes mainly：Silane coupling agent methyltrimethoxysilane (6070 model), γ-aminopropyl triethoxysilane (550 models of KH), γ-(the third oxygen of 2,3- epoxies) propyl trimethoxy Silane (560 models of KH), γ-（Methacryloxypropyl）Propyl trimethoxy silicane (570 models of KH), N-2-（Aminoethyl）- Any one of 3- aminopropyl trimethoxysilanes (KH792 models) or two kinds of mixing or two or more mixing；
The p-aramid fiber base prepreg manufactured by patent is applied not only to the high-frequency high-speed circuit board of manufacture hard, is additionally operable to make Make soft or flexible high-frequency high-speed circuit board.
CN201710148573.2A 2017-03-14 2017-03-14 A kind of manufacturing method of high-frequency high-speed circuit board p-aramid fiber base prepreg Pending CN108570877A (en)

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CN109082944A (en) * 2018-09-30 2018-12-25 深圳昊天龙邦复合材料有限公司 Novel aramid fiber paper-based copper-coated board and preparation method thereof
CN109318116A (en) * 2018-09-30 2019-02-12 深圳昊天龙邦复合材料有限公司 Composite material wafer support plate and its manufacturing method based on p-aramid paper
CN111825955A (en) * 2020-07-23 2020-10-27 海南大学 High-frequency prepreg, preparation method thereof, copper-clad plate and preparation method thereof
CN114311883A (en) * 2022-01-06 2022-04-12 株洲时代新材料科技股份有限公司 Copper-clad plate and preparation method thereof
CN115323828A (en) * 2022-08-11 2022-11-11 黄河三角洲京博化工研究院有限公司 Para-aramid paper cyanate ester high-frequency copper-clad plate and preparation method thereof
CN115339191A (en) * 2022-08-15 2022-11-15 黄河三角洲京博化工研究院有限公司 Para-aramid paper composite base halogen-free low-dielectric copper-clad plate and preparation method thereof
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CN109082944A (en) * 2018-09-30 2018-12-25 深圳昊天龙邦复合材料有限公司 Novel aramid fiber paper-based copper-coated board and preparation method thereof
CN109318116A (en) * 2018-09-30 2019-02-12 深圳昊天龙邦复合材料有限公司 Composite material wafer support plate and its manufacturing method based on p-aramid paper
CN109318116B (en) * 2018-09-30 2020-10-13 赣州龙邦材料科技有限公司 Composite material wafer carrier plate based on para-aramid paper and manufacturing method thereof
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CN111825955B (en) * 2020-07-23 2023-07-21 海南大学 Prepreg for high frequency, preparation method thereof and copper-clad plate and preparation method thereof
CN114311883A (en) * 2022-01-06 2022-04-12 株洲时代新材料科技股份有限公司 Copper-clad plate and preparation method thereof
CN115323828A (en) * 2022-08-11 2022-11-11 黄河三角洲京博化工研究院有限公司 Para-aramid paper cyanate ester high-frequency copper-clad plate and preparation method thereof
CN115339191A (en) * 2022-08-15 2022-11-15 黄河三角洲京博化工研究院有限公司 Para-aramid paper composite base halogen-free low-dielectric copper-clad plate and preparation method thereof
CN117230651A (en) * 2023-09-28 2023-12-15 陕西科技大学 Electric insulation paper material and preparation method and application thereof

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Application publication date: 20180925