CN107914403A - A kind of technology of preparing of high temperature resistant flexibility coat copper plate base material - Google Patents

A kind of technology of preparing of high temperature resistant flexibility coat copper plate base material Download PDF

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Publication number
CN107914403A
CN107914403A CN201711121876.1A CN201711121876A CN107914403A CN 107914403 A CN107914403 A CN 107914403A CN 201711121876 A CN201711121876 A CN 201711121876A CN 107914403 A CN107914403 A CN 107914403A
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copper
ether nitrile
poly
technology
temperature
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CN107914403B (en
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徐明珍
李逵
任登勋
袁悦
陈林
杨雨辰
刘孝波
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University of Electronic Science and Technology of China
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/02—Preparation of the material, in the area to be joined, prior to joining or welding
    • B29C66/024—Thermal pre-treatments
    • B29C66/0242—Heating, or preheating, e.g. drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
    • B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
    • B29C66/45—Joining of substantially the whole surface of the articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/74—Joining plastics material to non-plastics material
    • B29C66/742—Joining plastics material to non-plastics material to metals or their alloys
    • B29C66/7428—Transition metals or their alloys
    • B29C66/74281—Copper or alloys of copper
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
    • C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
    • C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
    • C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
    • C08G65/4031—(I) or (II) containing nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2007/00—Flat articles, e.g. films or sheets
    • B29L2007/002—Panels; Plates; Sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2009/00—Layered products
    • B29L2009/003—Layered products comprising a metal layer

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)

Abstract

The present invention relates to a kind of technology of preparing of high temperature resistant flexible copper-clad plate material, the raw material needed for the technology of preparing mainly include homemade poly aromatic ether nitrile high molecular and curing agent.Poly (arylene ether nitrile) and curing agent are pressed 1 first：(0.05~0.2) is dissolved in solvent after mixing obtains homogeneous solution, then casting film-forming；Secondly copper foil will be enclosed up and down after poly (arylene ether nitrile) film neatly stacking, flexibility coat copper plate is prepared through hot extrusion briquetting technique.Finally, by adjusting the ratio of poly aromatic ether nitrile high molecular and curing agent, heat treatment temperature and time, pressure etc., a series of flexible copper-clad plate materials with different temperature tolerances, glass transition temperature and dielectric property be can obtain.Heat decomposition temperature (the T of the flexibility coat copper plate5%) it is 470~490 DEG C, glass transition temperature is 270 DEG C~290 DEG C, dielectric constant 3.1~3.3 under room temperature condition 1KHz frequencies.The technology of preparing of the flexible copper-clad plate material belongs to field of high polymer material processing, specifically can be applied to printed substrate technical field as flexibility coat copper plate.

Description

A kind of technology of preparing of high temperature resistant flexibility coat copper plate base material
Preparation and its processing technology the present invention relates to a kind of fire resistant polymer film belong to Polymer Technology processing neck Domain, can be used as high temperature resistant flexibility coat copper plate substrate applications in printed substrate technical field.
Background technology
With microelectronic industry product towards miniaturization, high speed development, large scale integrated circuit size reduction to sub-micro Meter level, and the raising of the complication degree and signal transmission speed of circuit, have high density, large capacity, the envelope of high reliability Dress and interconnection technique just seem extremely important.Printed circuit board (Printed Circuit Board, abbreviation PCB) be at present just The property taken electronic product, satellite transmission and the most key part of communication article, are important materials of the connection with supporting electronic device, It is that indispensable main building block, its performance quality will directly affect the performance of electronic product in numerous electronic products.And Copper-clad plate (Copper Clad Laminate, abbreviation CCL) is to manufacture the mainstream basic material of PCB, by resin matrix and copper foil It is hot-forming and form substrate.Microelectronics industry develops rapidly in recent years, the feature ruler of large scale integrated circuit such as cpu chip Very little less and less, integrated level is higher and higher, and PCB develops towards high density, more compact, more cheap direction always.In order to alleviate Resulting resistance, capacitance delays, crosstalk and can these good bottleneck problems, the requirement to base material copper-clad plate is more and more harsher, And then increasingly higher demands also are proposed to copper-clad plate resin matrix, except with the due Physical Mechanical of conventional resins Can, outside cementability and electric insulating quality, with greater need for having lower dielectric constant and loss and more preferable heat resistance concurrently.
At present, in the selection of flex plate copper-clad plate base material, electric property that Kapton is protruded by it, thermostabilization Property and mechanical performance, have obtained more concern.However, microelectronics industry application in polyimides dielectric constant still It is higher, it can not meet the higher and higher application demand of integrated level；Meanwhile high-performance polyimide holds at high price, also exist Largely limit its extensive use.Therefore, exploitation novel low-cost has low-k, dielectric loss and protrusion concurrently The high molecular material of heat resistance is extremely urgent.Poly (arylene ether nitrile) is that current comprehensive performance can match in excellence or beauty in the new special height of polyimides Molecular material, because of the benzene ring structure enriched in its structure, makes it show prominent mechanical strength and heat resistance；But because of its structure Asymmetry, the dielectric constant under room temperature 1KHz frequencies of high molecular material maintains 3.6 or so, can not meet low dielectric The application of flexibility coat copper plate.Pi-allyl has non-polar character, can reduce the dielectric constant of polymer；Meanwhile pi-allyl occurs It can further improve the heat resistance of resin after cross-linking reaction；The presence of polarity nitrile group, can reinforced resin matrix and copper foil Bonding effect.Therefore, the present invention by a kind of new low dielectric poly aromatic ether nitrile high molecular of structure design displaying and its is used as flexibility The technology of preparing of copper-clad plate, to enrich the species of current copper-clad plate matrix resin.Therefore, new copper-clad plate resin matrix Exploitation will be of great significance with studying in terms of scientific research and application field.
The content of the invention
The purpose of the present invention is for traditional Kapton dielectric constant it is high, expensive, not easy to be processed etc. no Foot, there is provided a kind of technology of preparing of high temperature resistant flexible copper-clad plate material, realizes the middle low temperature process of flexibility coat copper plate, simplifies and adds Work technique；At the same time, which is significantly improved on the basis of traditional material, has high temperature resistant, low Jie concurrently While electric constant, there is high toughness and elongation at break, to ensure the pliability of copper-clad plate material, meet nowadays harsh answer Use environment.Specifically, to synthesize the poly (arylene ether nitrile) containing allyl functionality as material matrix, prepared and covered using casting film-forming mode Copper coin thin-film material, then by compression molding technology, obtain the copper-clad plate material；The present invention provides a kind of casting film-forming and hot pressing Forming technique, a kind of high temperature resistant flexible copper-clad plate material is obtained by Temperature Treatment.
A kind of technology of preparing of the flexible copper-clad plate material, it is characterised in that：The copper-clad plate is with material using curtain coating It is excellent that film forming and a hot pressing formation process, processing technology simplicity, and the material possess high temperature resistant, low-k and high toughness etc. Point.The concrete operation step of the copper-clad plate material preparation technology is as follows：
(1) self-control obtains new poly aromatic ether nitrile high molecular material and curing agent；
(2) poly aromatic ether nitrile high molecular for obtaining step (1) and curing agent are by 1：(0.05~0.1) it is uniformly rear molten after mixing Solution casts poly (arylene ether nitrile) film in solvent, using casting film-forming mode；
(3) the poly (arylene ether nitrile) film cast in step (2) is obtained into corresponding film in drying box through temperature programming, its In, heating schedule is 80 DEG C -1h-120 DEG C -1h-140 DEG C -1h-160 DEG C -1h-200 DEG C of -2h；
(4) the copper foil stacking after the film obtained step (3) and surface treatment, is placed in thermal station, excludes bubble, apply The laggard trip temperature processing of pressure；
(5) treat step (4) heat treatment after cooled to room temperature, remove mould, that is, obtain flexibility of the present invention Copper-clad plate base material.
In the step (1), the structure of the poly aromatic ether nitrile high molecular is as shown in Equation 1：
Curing agent is maleic anhydride；
Solvent for use in the step (2) is n,N-Dimethylformamide, 1-methyl-2-pyrrolidinone and N, N- dimethyl One or more in acetamide；
Heat treatment temperature is 240-280 DEG C in the step (4), when the time is 1-3 small, pressure 2-5MPa；
Beneficial effects of the present invention：Flexible copper-clad plate material prepared by the present invention is using casting film-forming and once hot-forming Mode, method are easy, cost-effective.By adjusting ratio, the hot-pressing processing temperature and time of poly (arylene ether nitrile) and curing agent, can obtain To the adjustable controllable copper-clad plate material of performance, the species of abundant flexibility coat copper plate base material.Poly (arylene ether nitrile) hair after hot-pressing processing Raw further crosslinking, can improve the heat resistance of material；At the same time, which has from characteristics such as fire-retardant, service life length, Meanwhile processing technology simplifies, batch development benefit is further improved, and easily realize industrialization.
Embodiment：
The embodiment of preparation method of the present invention introduced below, but following embodiments are the examples for illustrating the present invention, and Any restriction to the claims in the present invention is not formed.
Embodiment 1：
Step (1) is by 10g poly (arylene ether nitrile)s and 0.5g curing agent uniform dissolution in the 1-methyl-2-pyrrolidinone of 50ml；
Step (2) is cast in the poly (arylene ether nitrile) solution being uniformly dissolved on glass plate, is placed in drying box and removes solvent；
The poly (arylene ether nitrile) film that step (3) obtains step (2) encloses copper foil up and down after being neatly laminated, and is placed in steel plate mould In, it is 280 DEG C to set thermal station temperature, after slowly applying pressure exclusion bubble, maintains pressure 2MP, keeps temperature and pressure processing 2 Hour；
Step (4) cures after step (3) to be finished and after cooled to room temperature, removes mould, you can obtain the flexibility and cover Copper sheet material.
The defects of flexibility coat copper plate material surface obtained after being cured by step (4) is smooth, bubble-free；Test its heat point Solve temperature (T5%) it is 480 DEG C, glass transition temperature is 275 DEG C, and dielectric constant is 3.2 under room temperature condition 1KHz frequencies, loss For 0.011, all data are satisfied by the standard requirement of flexible copper-clad plate material.
Embodiment 2：
Step (1) is by 10g poly (arylene ether nitrile)s and 0.6g curing agent uniform dissolution in the 1-methyl-2-pyrrolidinone of 50ml；
Step (2) is cast in the poly (arylene ether nitrile) solution being uniformly dissolved on glass plate, is placed in drying box and removes solvent；
The poly (arylene ether nitrile) film that step (3) obtains step (2) encloses copper foil up and down after being neatly laminated, and is placed in steel plate mould In, it is 260 DEG C to set thermal station temperature, after slowly applying pressure exclusion bubble, maintains pressure 2MP, keeps temperature and pressure processing 2 Hour；
Step (4) cures after step (3) to be finished and after cooled to room temperature, removes mould, you can obtain the flexibility and cover Copper sheet material.
The defects of flexibility coat copper plate material surface obtained after being cured by step (4) is smooth, bubble-free；Test its heat point Solve temperature (T5%) it is 485 DEG C, glass transition temperature is 279 DEG C, and dielectric constant is 3.22 under room temperature condition 1KHz frequencies, damage Consume for 0.013, all data are satisfied by the standard requirement of flexible copper-clad plate material.
Embodiment 3：
Step (1) is by 10g poly (arylene ether nitrile)s and 0.7g curing agent uniform dissolution in the 1-methyl-2-pyrrolidinone of 50ml；
Step (2) is cast in the poly (arylene ether nitrile) solution being uniformly dissolved on glass plate, is placed in drying box and removes solvent；
The poly (arylene ether nitrile) film that step (3) obtains step (2) encloses copper foil up and down after being neatly laminated, and is placed in steel plate mould In, it is 260 DEG C to set thermal station temperature, after slowly applying pressure exclusion bubble, maintains pressure 2MP, keeps temperature and pressure processing 2 Hour；
Step (4) cures after step (3) to be finished and after cooled to room temperature, removes mould, you can obtain the flexibility and cover Copper sheet material.
The defects of flexibility coat copper plate material surface obtained after being cured by step (4) is smooth, bubble-free；Test its heat point Solve temperature (T5%) it is 484 DEG C, glass transition temperature is 286 DEG C, and dielectric constant is 3.18 under room temperature condition 1KHz frequencies, damage Consume for 0.0107, all data are satisfied by the standard requirement of flexible copper-clad plate material.
Embodiment 4：
Step (1) is by 10g poly (arylene ether nitrile)s and 0.8g curing agent uniform dissolution in the 1-methyl-2-pyrrolidinone of 50ml；
Step (2) is cast in the poly (arylene ether nitrile) solution being uniformly dissolved on glass plate, is placed in drying box and removes solvent；
The poly (arylene ether nitrile) film that step (3) obtains step (2) encloses copper foil up and down after being neatly laminated, and is placed in steel plate mould In, it is 260 DEG C to set thermal station temperature, after slowly applying pressure exclusion bubble, maintains pressure 2MP, keeps temperature and pressure processing 2 Hour；
Step (4) cures after step (3) to be finished and after cooled to room temperature, removes mould, you can obtain the flexibility and cover Copper sheet material.
The defects of flexibility coat copper plate material surface obtained after being cured by step (4) is smooth, bubble-free；Test its heat point Solve temperature (T5%) it is 490 DEG C, glass transition temperature is 288 DEG C, and dielectric constant is 3.11 under room temperature condition 1KHz frequencies, damage Consume for 0.0098, all data are satisfied by the standard requirement of flexible copper-clad plate material.
Embodiment 5：
Step (1) is by 10g poly (arylene ether nitrile)s and 0.8g curing agent uniform dissolution in the 1-methyl-2-pyrrolidinone of 50ml；
Step (2) is cast in the poly (arylene ether nitrile) solution being uniformly dissolved on glass plate, is placed in drying box and removes solvent；
The poly (arylene ether nitrile) film that step (3) obtains step (2) encloses copper foil up and down after being neatly laminated, and is placed in steel plate mould In, it is 280 DEG C to set thermal station temperature, after slowly applying pressure exclusion bubble, maintains pressure 2MP, keeps temperature and pressure processing 2 Hour；
Step (4) cures after step (3) to be finished and after cooled to room temperature, removes mould, you can obtain the flexibility and cover Copper sheet material.
The defects of flexibility coat copper plate material surface obtained after being cured by step (4) is smooth, bubble-free；Test its heat point Solve temperature (T5%) it is 498 DEG C, glass transition temperature is 292 DEG C, and dielectric constant is 3.16 under room temperature condition 1KHz frequencies, damage Consume for 0.0096, all data are satisfied by the standard requirement of flexible copper-clad plate material.
Embodiment 6：
Step (1) is by 10g poly (arylene ether nitrile)s and 0.8g curing agent uniform dissolution in the 1-methyl-2-pyrrolidinone of 50ml；
Step (2) is cast in the poly (arylene ether nitrile) solution being uniformly dissolved on glass plate, is placed in drying box and removes solvent；
The poly (arylene ether nitrile) film that step (3) obtains step (2) encloses copper foil up and down after being neatly laminated, and is placed in steel plate mould In, it is 280 DEG C to set thermal station temperature, after slowly applying pressure exclusion bubble, maintains pressure 3MP, keeps temperature and pressure processing 1.5 it is small when；
Step (4) cures after step (3) to be finished and after cooled to room temperature, removes mould, you can obtain the flexibility and cover Copper sheet material.
The defects of flexibility coat copper plate material surface obtained after being cured by step (4) is smooth, bubble-free；Test its heat point Solve temperature (T5%) it is 482 DEG C, glass transition temperature is 284 DEG C, and dielectric constant is 3.17 under room temperature condition 1KHz frequencies, damage Consume for 0.0099, all data are satisfied by the standard requirement of flexible copper-clad plate material.

Claims (3)

  1. A kind of technology of preparing of flexible copper-clad plate material described in 1., it is characterised in that：The copper-clad plate material is used and is cast into It is excellent that film and a hot pressing formation process, processing technology simplicity, and the material possess high temperature resistant, low-k and high toughness etc. Point.The concrete operation step of the copper-clad plate material preparation technology is as follows：
    (1) self-control obtains new poly aromatic ether nitrile high molecular material and curing agent；
    (2) poly aromatic ether nitrile high molecular for obtaining step (1) and curing agent are by 1：(0.05~0.1) mix after uniformly after be dissolved in In solvent, poly (arylene ether nitrile) film is cast using casting film-forming mode；
    (3) the poly (arylene ether nitrile) film cast in step (2) is obtained into corresponding film in drying box through temperature programming, wherein, Heating schedule is 80 DEG C -1h-120 DEG C -1h-140 DEG C -1h-160 DEG C -1h-200 DEG C of -2h；
    (4) the copper foil stacking after the film obtained step (3) and surface treatment, is placed in thermal station, excludes bubble, apply pressure Laggard trip temperature processing；
    (5) treat step (4) heat treatment after cooled to room temperature, remove mould, that is, obtain flexible copper-clad of the present invention Plate base material.
  2. A kind of 2. technology of preparing of copper-clad plate material according to claim 1, it is characterised in that：In the step (1), The structure of the poly aromatic ether nitrile high molecular is as shown in Equation 1：
    Curing agent is maleic anhydride.
  3. A kind of 3. technology of preparing of copper-clad plate material according to claim 1, it is characterised in that：In the step (4) Heat treatment temperature is 240-280 DEG C, when the time is 1-3 small, pressure 2-5MPa.
CN201711121876.1A 2017-11-14 2017-11-14 A kind of technology of preparing of high temperature resistant flexibility coat copper plate substrate Active CN107914403B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0448678A (en) * 1990-06-13 1992-02-18 Idemitsu Kosan Co Ltd Flexible printed circuit board
US20020072585A1 (en) * 2000-10-17 2002-06-13 Industrial Technology Research Institute PPE derivatives and resin composition having the same
JP2006002013A (en) * 2004-06-16 2006-01-05 Mitsui Chemicals Inc Polyether ketone-based resin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0448678A (en) * 1990-06-13 1992-02-18 Idemitsu Kosan Co Ltd Flexible printed circuit board
US20020072585A1 (en) * 2000-10-17 2002-06-13 Industrial Technology Research Institute PPE derivatives and resin composition having the same
JP2006002013A (en) * 2004-06-16 2006-01-05 Mitsui Chemicals Inc Polyether ketone-based resin

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