CN105196649A - Copper-clad plate manufacturing method - Google Patents
Copper-clad plate manufacturing method Download PDFInfo
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- CN105196649A CN105196649A CN201510554104.1A CN201510554104A CN105196649A CN 105196649 A CN105196649 A CN 105196649A CN 201510554104 A CN201510554104 A CN 201510554104A CN 105196649 A CN105196649 A CN 105196649A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/092—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
- B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
- B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/08—PCBs, i.e. printed circuit boards
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/023—Silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a copper-clad plate manufacturing method, which comprises the following steps of manufacturing an inside material glue solution prepreg, manufacturing a surface material glue solution prepreg, laminating and pressing. The CTI (comparative tracking index) of the CTI copper-clad plate manufactured by applying the method achieves 600-700V, the thermostability achieves 60S-120S (tested according to IPC-TM-650-2.4.8 standard at 288 DEG C through dip soldering), the thermal property is excellent, the peeling strength is characterized in that the peeling strength of an HOZ copper foil is improved to be 1.0-1.5N/mm and the peeling strength of a 1OZ copper foil is generally 1.5-2.5N/mm (tested according to IPC-TM-650-2.4.8 standard), and the flame retardant property can achieve V-0 (UL94 standard).
Description
Technical field
The present invention relates to printed circuit board (PCB) copper coated foil plate technical field used, particularly relate to a kind of high CIT copper-clad plate production method.
Background technology
When the surface of copper-clad plate insulating substrate is subject to dust attachment, moisture content condensation or moisture and has the pollution of negative ions pollutant, under applied voltage effect, the leakage current on its surface is more much bigger than clean surface.The heat of vaporization moisture contamination thing that this leakage current produces, makes the surface of insulating substrate be in uneven drying regime, causes substrate surface to form local desiccation point or dry zone.Dry district makes sheet resistance increase, and such electric field just becomes uneven, and then produces flashover electric discharge.Under electric field and hot acting in conjunction, insulating materials surface carbonation, carbide resistance is little, impels the electric-field intensity increase executed alive eletrode tip and formed, thus flashover electric discharge more easily occurs.Repeatedly there is flashover electric discharge between circuit and produce electric spark, and then form the vestige of charing conducting channel, destroy substrate surface insulating properties, form conductive channel, creepage trace phenomenon occurs.Creepage trace phenomenon is: solid insulating material surface, under the synergy of electric field and electrolyte, forms the process of conductive path gradually.
The Capability index that the tracking-resistant on insulating materials surface plays trace is called as phase ratio creepage tracking index CTI(ComparativeTrackingIndex).CTI can weigh the insulation safety performance of insulating materials to a certain extent.Copper-clad plate as printed circuit board insulating body must improve its CTI value to ensure the insulation safety performance under the adverse circumstances such as humidity.
CTI value its proof tracking index larger is higher, and insulating properties is better.In conventional FR-4 copper-clad plate, the main consuming body resin is brominated epoxy resin, aliphatic chain and aromatic rings more, have a strong impact on its CTI value of base material (according to GB/4207-2003/IEC standard) very low≤250V.Reduce content of Cl element in resin, can reduce the fire resistance of base material, in resin, the minimizing of aliphatic chain and aromatic rings can reduce peel strength and the heat resistance of sheet material.For these technical barriers, our company R&D work personnel capture through long, the one developed novel high CTI value copper-clad plate formula and technique thereof, its CTI value of sheet material using the method to make reaches 600V, fire resistance reaches V-0 level (according to U.S. UL-94 examination criteria), other high comprehensive performances, make the requirement in its applicable market.
Summary of the invention
The object of the invention is solve problem be: the aliphatic chain in the brominated epoxy resin molecular structure in conventional FR-4 copper-clad plate and aromatic rings on the high side, C-C chain in molecular structure or alkyl, under flashover discharges the electric spark that causes, very easily cause burning and form carbonized path and form conductive channel, causing creepage trace.Bromo element as fire retardation is polarity, and facile hydrolysis dissociates conductive charged ion, causes creepage trace; Therefore conventional FR-4 copper-clad plate CTI value very low≤250V.
The technical solution used in the present invention is: a kind of copper-clad plate production method, and making step is as follows:
A, making lining glue prepreg;
B, making table material glue prepreg;
C, folded to join;
D, compacting;
The proportioning of described table material glue prepreg is: matrix resin is epoxy resin B1200 part, flexibilizer B20-25 part, 535 parts, aluminium hydroxide; Inorganic silicon 70-90 part; Curing agent is electron level dicyandiamide 24 parts, and promoter is tertiary amines promoter 0.7 part, and coupling agent is KH560 type silane coupling agent 2.0 parts, solvent 220 parts, and above raw material by mass;
The proportioning of described lining glue prepreg is: matrix resin is brominated epoxy resin B950 part, talcum powder 110 parts, inorganic silicon 130 parts, curing agent are electron level dicyandiamide 21.7 parts, promoter is tertiary amines promoter 0.7 part, coupling agent is KH560 type silane coupling agent 2.1 parts, solvent 249 parts, above raw material by mass.
As a further improvement on the present invention, the proportioning of described table material glue prepreg is: matrix resin is epoxy resin A1000 part, flexibilizer B10-30 part, 534 parts, aluminium hydroxide; Silica 50-100 part; Curing agent is electron level dicyandiamide 23.1 parts, and promoter is tertiary amines promoter 0.5 part, and coupling agent is KH560 type silane coupling agent 2.5 parts, solvent 100-250 part.
As a further improvement on the present invention, matrix resin also can mix with one or more common brominated epoxy resins and one or more halogen-free epoxy resins according to a certain percentage; The optional acrylonitrile-butadiene rubber of described flexibilizer, conventional CTBN are epoxy resin toughened, one or more mixtures in liquid polysulfide rubber, Polyurethane, silicon rubber, Pioloform, polyvinyl acetal, polysulfones PSF, polyether sulfone and nano silicon; Described solvent is one or more mixtures in dimethyl formamide, acetone, butanone and alcohol.
As a further improvement on the present invention, the epoxide equivalent of matrix resin is 390-440, content of inorganic chlorine≤350ppm, bromine content≤20ppm; Described flexibilizer and silica are all use silane surfactant to carry out surface treatment, particle diameter≤6 μm.
As a further improvement on the present invention, the epoxide equivalent 450-480 of matrix resin, content of inorganic chlorine≤500ppm, bromine content≤30ppm; Described talcum powder carries out surface treatment for using silane surfactant; Solvent is a kind of in dimethyl formamide, acetone, butanone, alcohol or several mixtures.
The invention has the beneficial effects as follows: the copper-clad plate that practical this method makes, its performance is as follows:
1, sheet material CTI value reaches 600-700V
2, heat resistance reaches 60S-120S(according to IPC-TM-650-2.4.8 standard detection, 288 DEG C, wicking) fine heat-resisting performance;
3, (its peel strength of HOZ Copper Foil is promoted to 1.0-1.5N/mm to peel strength; Its peel strength of 1OZ Copper Foil is generally 1.5-2.5N/mm, according to IPC-TM-650-2.4.8 standard detection);
4, fire resistance reaches V-0(UL94 standard).
Detailed description of the invention
Embodiment 1:
Table material glue formula (by mass): matrix resin is epoxy resin A1200 part (epoxide equivalent 350, content of inorganic chlorine 350ppm, bromine content 20ppm), matrix resin also can mix with one or more common brominated epoxy resins and one or more halogen-free epoxy resins according to a certain percentage; Flexibilizer B20 part, the optional acrylonitrile-butadiene rubber of flexibilizer, conventional CTBN are epoxy resin toughened, one or more mixtures in liquid polysulfide rubber, Polyurethane, silicon rubber, Pioloform, polyvinyl acetal, polysulfones PSF, polyether sulfone, nano silicon; 535 parts, aluminium hydroxide (using silane surfactant to carry out surface treatment, particle diameter≤5 μm); Inorganic silicon 70 parts (using silane surfactant to carry out surface treatment, particle diameter≤5 μm); Curing agent is electron level dicyandiamide 24 parts, and promoter is tertiary amines promoter 0.7 part, and coupling agent is KH560 type silane coupling agent 2.1 parts, solvent (in dimethyl formamide, acetone, butanone, alcohol a kind of or several mixtures) 220 parts.By Resin A, flexibilizer B, curing agent, promoter, coupling agent and evenly become liquid with the silica of silane surfactant process, aluminium hydroxide with appropriate stirring solvent; Glue index: GT(gelation time, 171 DEG C) obtained mixture is coated in and 7628 E-glass cloth toast 7Min in 150-170 DEG C of baking oven makes PP sheet, PP sheet GT(171 DEG C by 280s) 110S;
Lining glue formula (by mass): matrix resin is brominated epoxy resin A950 part (epoxide equivalent 400, content of inorganic chlorine 500ppm, bromine content 30ppm); Talcum powder 110 parts (using silane surfactant to carry out surface treatment); Inorganic silicon 130 parts (using silane surfactant to carry out surface treatment, particle diameter≤5 μm); Curing agent is electron level dicyandiamide 21.7 parts, and promoter is tertiary amines promoter 0.7 part, and coupling agent is KH560 type silane coupling agent 2.1 parts, solvent (in dimethyl formamide, acetone, butanone, alcohol a kind of or several mixtures) 249 parts.By resin, curing agent, promoter, coupling agent and evenly become liquid with the silica of silane surfactant process, talcum powder with appropriate stirring solvent; Glue index: GT(gelation time, 171 DEG C of 0.3g) obtained mixture is coated in and 7628 E-glass cloth toast 5Min in 150 DEG C of baking ovens makes PP sheet, PP sheet GT(171 DEG C by 240s) 113S.
Fold and join, join two-layer Copper Foil by folded in two-layer copper coin, fold in two-layer Copper Foil and join two-layer table material glue prepreg, finally fold in two-layer table material glue prepreg and join some layers of lining glue prepreg;
Folded group material of having joined is put into vacuum press lamination, first proceeds in cold press after hot pressing in hot press and cold pressing.
Embodiment 2:
Table material glue formula (by mass): matrix resin is epoxy resin A1000 part (epoxide equivalent 380, content of inorganic chlorine≤350ppm, bromine content≤20ppm), matrix resin also can mix with one or more common brominated epoxy resins and one or more halogen-free epoxy resins according to a certain percentage; Flexibilizer B22 part, the optional acrylonitrile-butadiene rubber of flexibilizer, conventional CTBN are epoxy resin toughened, one or more mixtures in liquid polysulfide rubber, Polyurethane, silicon rubber, Pioloform, polyvinyl acetal, polysulfones PSF, polyether sulfone, nano silicon; 534 parts, aluminium hydroxide (using silane surfactant to carry out surface treatment, particle diameter≤5 μm); Inorganic silicon 65 parts (using silane surfactant to carry out surface treatment, particle diameter≤5 μm); Curing agent is electron level dicyandiamide 23.1 parts, and promoter is tertiary amines promoter 0.5 part, and coupling agent is KH560 type silane coupling agent 2.5 parts, solvent (in dimethyl formamide, acetone, butanone, alcohol a kind of or several mixtures) 165 parts.By Resin A, flexibilizer B, curing agent, promoter, coupling agent and evenly become liquid with the silica of silane surfactant process, aluminium hydroxide with appropriate stirring solvent; Glue index: GT(gelation time, 171 DEG C) obtained mixture is coated in and 7628 E-glass cloth toast 8Min in 155 DEG C of baking ovens makes PP sheet (prepreg), PP sheet GT(171 DEG C by 295s) 128S;
Lining glue formula (by mass): matrix resin is brominated epoxy resin A960 part (epoxide equivalent 430, content of inorganic chlorine≤500ppm, bromine content≤30ppm); Talcum powder 115 parts (using silane surfactant to carry out surface treatment); Inorganic silicon 100 parts (using silane surfactant to carry out surface treatment, particle diameter≤5 μm); Curing agent is electron level dicyandiamide 21.6 parts, and promoter is tertiary amines promoter 0.5 part, and coupling agent is KH560 type silane coupling agent 2 parts, solvent (in dimethyl formamide, acetone, butanone, alcohol a kind of or several mixtures) 246.2 parts.By resin, curing agent, promoter, coupling agent and evenly become liquid with the silica of silane surfactant process, talcum powder with appropriate stirring solvent; Glue index: GT(gelation time, 171 DEG C of 0.3g) obtained mixture is coated in and 7628 E-glass cloth toast 6Min in 150-170 DEG C of baking oven makes PP sheet, PP sheet GT(171 DEG C by 240-280s) 116S;
Fold and join, join two-layer Copper Foil by folded in two-layer copper coin, fold in two-layer Copper Foil and join two-layer table material glue prepreg, finally fold in two-layer table material glue prepreg and join some layers of lining glue prepreg;
Folded group material of having joined is put into vacuum press lamination, first proceeds in cold press after hot pressing in hot press and cold pressing.
Below the parameter list of heat pressing process and cold-press process:
Heat pressing process:
To cold pressing pressing process:
Table material matrix resin employs new type resin costly, but takes method optimizing board cost: (1), in table material formula 1 glue aluminium hydroxide and silica filler content very high, and filler is with low cost; (2), plate construction optimization, only have the prepreg that the 2 layers of PP in surface use optimization of C/C composites to make, to ensure the CTI performance of sheet material, the one deck in nexine or multilayer PP glue formula still use conventional FR-4 formula Design; This new formulation integrated cost is 1.2-1.3 times of common FR-4 cost, but this sheet material price reaches the 1.8-2.0 of common FR-4 doubly, significantly increases product profit.
Above embodiments of the present invention are described, but the invention is not restricted to above-mentioned embodiment, in the ken that art those of ordinary skill possesses, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (4)
1. a copper-clad plate production method, making step is as follows:
A, making lining glue prepreg;
B, making table material glue prepreg;
C, folded to join;
D, compacting;
It is characterized in that:
The proportioning of described table material glue prepreg is: matrix resin is epoxy resin B1200 part, flexibilizer B20-25 part, 535 parts, aluminium hydroxide; Inorganic silicon 70-90 part; Curing agent is electron level dicyandiamide 24 parts, and promoter is tertiary amines promoter 0.7 part, and coupling agent is KH560 type silane coupling agent 2.0 parts, solvent 220 parts, and above raw material by mass;
The proportioning of described lining glue prepreg is: matrix resin is brominated epoxy resin B950 part, talcum powder 110 parts, inorganic silicon 130 parts, curing agent are electron level dicyandiamide 21.7 parts, promoter is tertiary amines promoter 0.7 part, coupling agent is KH560 type silane coupling agent 2.1 parts, solvent 249 parts, above raw material by mass.
2. a kind of copper-clad plate production method according to claim 1, is characterized in that: matrix resin also can mix with one or more common brominated epoxy resins and one or more halogen-free epoxy resins according to a certain percentage; The optional acrylonitrile-butadiene rubber of described flexibilizer, conventional CTBN are epoxy resin toughened, one or more mixtures in liquid polysulfide rubber, Polyurethane, silicon rubber, Pioloform, polyvinyl acetal, polysulfones PSF, polyether sulfone and nano silicon; Described solvent is one or more mixtures in dimethyl formamide, acetone, butanone and alcohol.
3. a kind of copper-clad plate production method according to claim 1, is characterized in that: the epoxide equivalent of matrix resin is 390-440, content of inorganic chlorine≤350ppm, bromine content≤20ppm; Described flexibilizer and silica are all use silane surfactant to carry out surface treatment, particle diameter≤6 μm.
4. a kind of copper-clad plate production method according to claim 1, is characterized in that the epoxide equivalent 450-480 of described matrix resin, content of inorganic chlorine≤500ppm, bromine content≤30ppm; Described talcum powder carries out surface treatment for using silane surfactant; Solvent is a kind of in dimethyl formamide, acetone, butanone, alcohol or several mixtures.
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Cited By (2)
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| CN108181342A (en) * | 2017-12-11 | 2018-06-19 | 广州兴森快捷电路科技有限公司 | Flexible sheet detection method |
| CN110435254A (en) * | 2019-08-29 | 2019-11-12 | 山东金宝电子股份有限公司 | A kind of high heat resistance, high CTI CEM-3 copper-clad plate preparation method |
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| CN104066277A (en) * | 2014-06-30 | 2014-09-24 | 铜陵浩荣华科复合基板有限公司 | White CTI-600 printed circuit board fabrication method |
| CN104163030A (en) * | 2014-06-30 | 2014-11-26 | 铜陵浩荣华科复合基板有限公司 | A method of manufacturing a halogen-free high-conductivity high-heat resistance copper-clad metal substrate |
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| CN103978766A (en) * | 2014-05-27 | 2014-08-13 | 铜陵浩荣华科复合基板有限公司 | Manufacturing mode of high-CTI (comparative tracking index) value copper-clad plate |
| CN104066277A (en) * | 2014-06-30 | 2014-09-24 | 铜陵浩荣华科复合基板有限公司 | White CTI-600 printed circuit board fabrication method |
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