CN103978766A - Manufacturing mode of high-CTI (comparative tracking index) value copper-clad plate - Google Patents
Manufacturing mode of high-CTI (comparative tracking index) value copper-clad plate Download PDFInfo
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- CN103978766A CN103978766A CN201410226900.8A CN201410226900A CN103978766A CN 103978766 A CN103978766 A CN 103978766A CN 201410226900 A CN201410226900 A CN 201410226900A CN 103978766 A CN103978766 A CN 103978766A
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Abstract
The invention discloses a manufacturing mode of a high-CTI (comparative tracking index) value copper-clad plate. The mode comprises the following manufacturing steps: manufacturing lining glue solution prepregs; manufacturing surface glue solution prepregs; laminating and pressing the lining glue solution prepregs and the surface glue solution prepregs. The CTI of the high-CTI value copper-clad plate manufactured by using the mode reaches 600-700V; the heat resistance reaches 60-120S by detection according to an IPC-TM-650-2.4.8 standard and tin immersion at the temperature of 288 DEG C; the heat resistance performance is excellent; the peeling strength of HOZ copper foil is improved to 1.0-1.5N/mm, and the peeling strength of 1OZ copper foil is 1.5-2.5N.mm generally by detection according to the IPC-TM-650-2.4.8 standard; the flame retardant property reaches V-0 according to a UL94 standard.
Description
Technical field
The present invention relates to printed circuit board (PCB) copper coated foil plate technical field used, relate in particular to a kind of high CTI value copper-clad plate production method.
Background technology
Copper-clad plate with the surface of insulating substrate be subject to that dust adheres to, moisture content dewfall or moisture and while thering is the pollution of negative ions pollutant, under applied voltage effect, its surperficial leakage current is more much bigger than clean surface.The moist pollutant of heat of vaporization that this leakage current produces, makes the surface of insulating substrate in inhomogeneous drying regime, causes substrate surface to form local desiccation point or dry zone.Dry district increases sheet resistance, and electric field just becomes inhomogeneous like this, and then produces flashover electric discharge.Under electric field and hot acting in conjunction, insulating materials surface carbonization, carbide resistance is little, impels to execute the electric-field intensity that alive eletrode tip forms and increase, thereby flashover electric discharge more easily occurs.Between circuit, repeatedly there is flashover discharge generation 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 of the anti-creepage trace on insulating materials surface is called as phase ratio creepage tracking index CTI(Comparative Tracking Index).CTI can weigh the insulation safety performance of insulating materials to a certain extent.Must improve its CTI value to ensure the insulation safety performance under the adverse circumstances such as humidity as the copper-clad plate of printed circuit board insulating body.
Larger its anti creepage trace index of CTI value is higher, and insulating properties is better.In conventional FR-4 copper-clad plate, the main consuming body resin is brominated epoxy resin, and aliphatic chain and aromatic rings are more, have a strong impact on the very low≤250V of its CTI value of base material (according to GB/4207-2003/IEC standard).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, the R&D work personnel of our company are through long capturing, one novel high CTI value copper-clad plate formula and the technique thereof developed, its CTI value of sheet material that uses 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 problem that the object of the invention is to solve is: aliphatic chain and aromatic rings in the brominated epoxy resin molecular structure in conventional FR-4 copper-clad plate are on the high side, C-C chain or alkyl in molecular structure, under flashover discharges the electric spark causing, very easily cause burning and form carbonization path formation conductive channel, cause creepage trace.Be polarity as the bromo element of fire retardation, the facile hydrolysis conductive charged ion that dissociates, 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 high CTI value copper-clad plate production method, and making step is as follows:
A, making lining glue prepreg, resin, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, talcum powder and appropriate stirring solvent are evenly become to liquid, the mixture making is coated in and on 7628 electron level glass cloth, in 150-170 DEG C of baking oven, toasts 5-8Min and make prepreg;
B, making table material glue prepreg, Resin A, flexibilizer B, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, aluminium hydroxide and appropriate stirring solvent are evenly become to liquid, the mixture making is coated in and on 7628 electron level glass cloth, in 150-170 DEG C of baking oven, toasts 7-10Min and make semi-solid preparation;
C, folded joining, join two-layer Copper Foil by folded in two-layer copper coin, in two-layer Copper Foil, fold and join two-layer table material glue prepreg, finally in two-layer table material glue prepreg, fold and join some layers of lining glue prepreg.
D, compacting, put into hot press hot pressing 120min-135min by folded group material of having joined, then put into the cold press 55min-65min that colds pressing.
As a further improvement on the present invention, the proportioning of described table material glue prepreg is: matrix resin is 1000 parts of epoxy resin A, flexibilizer B 10-30 part, 534 parts, aluminium hydroxide; Silica 50-100 part; Curing agent is 23.1 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2.5 parts of KH560 type silane coupling agents, solvent 100-250 part.
As a further improvement on the present invention, matrix resin also can mix according to a certain percentage with one or more common brominated epoxy resins and one or more halogen-free epoxy resins; 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 350-450, content of inorganic chlorine≤350ppm, bromine content≤20ppm; Described flexibilizer and silica are all to use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m.
As a further improvement on the present invention, the proportioning of described lining glue prepreg is: matrix resin is that 1000 parts of brominated epoxy resin A, 100 parts of talcum powder, 00 part of silica 1, curing agent are that 21.6 parts of electron level dicyandiamides, promoter are 0.5 part of tertiary amines promoter, coupling agent is 2 parts of KH560 type silane coupling agents, 246.2 parts of solvents.
As a further improvement on the present invention, the epoxide equivalent 400-500 of described matrix resin, content of inorganic chlorine≤500ppm, bromine content≤30ppm; Described talcum powder is for using silanes surface conditioning agent to carry out surface treatment; Solvent is a kind of in dimethyl formamide, acetone, butanone, alcohol or several mixtures.
The invention has the beneficial effects as follows: the CTI value copper-clad plate that practical this method is made, 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, and 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 1.5-2.5 N/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 1000 parts of (epoxide equivalents 350 of epoxy resin A, content of inorganic chlorine 350ppm, bromine content 20ppm), matrix resin also can mix according to a certain percentage with one or more common brominated epoxy resins and one or more halogen-free epoxy resins; 10 parts of flexibilizer B, 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; (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 534 parts, aluminium hydroxide; (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 50 parts of silica; Curing agent is 23.1 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2.5 parts of KH560 type silane coupling agents, 100 parts of solvents (a kind of or several mixtures in dimethyl formamide, acetone, butanone, alcohol).Resin A, flexibilizer B, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, aluminium hydroxide and appropriate stirring solvent are evenly become to liquid; Glue index: GT(gelation time, 171 DEG C) 280s is coated in the mixture making on 7628 electron level glass cloth, in 150-170 DEG C of baking oven, to toast 7Min and make PP sheet, PP sheet GT(171 DEG C) 110S;
Lining glue formula (by mass): matrix resin is 1000 parts of brominated epoxy resin A (epoxide equivalent 400, content of inorganic chlorine 500ppm, bromine content 30ppm); 100 parts of talcum powder (using silanes surface conditioning agent to carry out surface treatment); (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 00 part of silica 1; Curing agent is 21.6 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2 parts of KH560 type silane coupling agents, 246.2 parts of solvents (a kind of or several mixtures in dimethyl formamide, acetone, butanone, alcohol).Resin, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, talcum powder and appropriate stirring solvent are evenly become to liquid; Glue index: GT(gelation time, 171 DEG C of 0.3g) 240s is coated in the mixture making on 7628 electron level glass cloth, in 150 DEG C of baking ovens, to toast 5Min and make PP sheet, PP sheet GT(171 DEG C) 113S.
Folded joining, join two-layer Copper Foil by folded in two-layer copper coin, in two-layer Copper Foil, fold and join two-layer table material glue prepreg, finally in two-layer table material glue prepreg, fold and join some layers of lining glue prepreg;
Folded group material of having joined is put into vacuum press lamination, first in hot press, after hot pressing, proceed in cold press and cold pressing.
Embodiment 2:
Table material glue formula (by mass): matrix resin is 1000 parts of (epoxide equivalents 380 of epoxy resin A, content of inorganic chlorine≤350ppm, bromine content≤20ppm), matrix resin also can mix according to a certain percentage with one or more common brominated epoxy resins and one or more halogen-free epoxy resins; 15 parts of flexibilizer B, 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; (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 534 parts, aluminium hydroxide; (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 65 parts of silica; Curing agent is 23.1 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2.5 parts of KH560 type silane coupling agents, 165 parts of solvents (a kind of or several mixtures in dimethyl formamide, acetone, butanone, alcohol).Resin A, flexibilizer B, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, aluminium hydroxide and appropriate stirring solvent are evenly become to liquid; Glue index: GT(gelation time, 171 DEG C) 295s is coated in the mixture making on 7628 electron level glass cloth, to toast 8Min in 155 DEG C of baking ovens and make PP sheet (prepreg), PP sheet GT(171 DEG C) 128S;
Lining glue formula (by mass): matrix resin is 1000 parts of brominated epoxy resin A (epoxide equivalent 430, content of inorganic chlorine≤500ppm, bromine content≤30ppm); 100 parts of talcum powder (using silanes surface conditioning agent to carry out surface treatment); (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 00 part of silica 1; Curing agent is 21.6 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2 parts of KH560 type silane coupling agents, 246.2 parts of solvents (a kind of or several mixtures in dimethyl formamide, acetone, butanone, alcohol).Resin, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, talcum powder and appropriate stirring solvent are evenly become to liquid; Glue index: GT(gelation time, 171 DEG C of 0.3g) 240-280s is coated in the mixture making on 7628 electron level glass cloth, in 150-170 DEG C of baking oven, to toast 6Min and make PP sheet, PP sheet GT(171 DEG C) 116S;
Folded joining, join two-layer Copper Foil by folded in two-layer copper coin, in two-layer Copper Foil, fold and join two-layer table material glue prepreg, finally in two-layer table material glue prepreg, fold and join some layers of lining glue prepreg;
Folded group material of having joined is put into vacuum press lamination, first in hot press, after hot pressing, proceed in cold press and cold pressing.
Embodiment 3:
Table material glue formula (by mass): matrix resin is 1000 parts of (epoxide equivalents 400 of epoxy resin A, content of inorganic chlorine≤350ppm, bromine content≤20ppm), matrix resin also can mix according to a certain percentage with one or more common brominated epoxy resins and one or more halogen-free epoxy resins; Flexibilizer B 10-30 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; (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 534 parts, aluminium hydroxide; (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for silica 50-100 part; Curing agent is 23.1 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2.5 parts of KH560 type silane coupling agents, 200 parts of solvents (a kind of or several mixtures in dimethyl formamide, acetone, butanone, alcohol).Resin A, flexibilizer B, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, aluminium hydroxide and appropriate stirring solvent are evenly become to liquid; Glue index: GT(gelation time, 171 DEG C) 280-320s is coated in the mixture making on 7628 electron level glass cloth, to toast 10Min in 158 DEG C of baking ovens and make PP sheet (prepreg), PP sheet GT(171 DEG C) 145S;
Lining glue formula (by mass): matrix resin is 1000 parts of brominated epoxy resin A (epoxide equivalent 400-500, content of inorganic chlorine≤500ppm, bromine content≤30ppm); 100 parts of talcum powder (using silanes surface conditioning agent to carry out surface treatment); (use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m) for 00 part of silica 1; Curing agent is 21.6 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2 parts of KH560 type silane coupling agents, 246.2 parts of solvents (a kind of or several mixtures in dimethyl formamide, acetone, butanone, alcohol).Resin, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, talcum powder and appropriate stirring solvent are evenly become to liquid; Glue index: GT(gelation time, 171 DEG C of 0.3g) 280s is coated in the mixture making on 7628 electron level glass cloth, in 154 DEG C of baking ovens, to toast 8Min and make PP sheet, PP sheet GT(171 DEG C) 126S;
Folded joining, join two-layer Copper Foil by folded in two-layer copper coin, in two-layer Copper Foil, fold and join two-layer table material glue prepreg, finally in two-layer table material glue prepreg, fold and join some layers of lining glue prepreg;
Folded group material of having joined is put into vacuum press lamination, first in hot press, after hot pressing, proceed in cold press and cold pressing.
Below the parameter list of heat pressing process and cold-press process:
Heat pressing process:
The pressing process of colding pressing:
Table material matrix resin has used more expensive new type resin, but has taked mode to optimize 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, the prepreg that only has the 2 layers of PP in surface to 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; The 1.2-1.3 that this new formulation integrated cost is common FR-4 cost times, but this sheet material price reaches 1.8-2.0 times of common FR-4, has increased greatly product profit.
Above embodiments of the present invention are described, but the invention is not restricted to above-mentioned embodiment, in the ken possessing at affiliated technical field those of ordinary skill, can also under the prerequisite that does not depart from aim of the present invention, make a variety of changes.
Claims (6)
1. a high CTI value copper-clad plate production method, is characterized in that: making step is as follows:
A, making lining glue prepreg, resin, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, talcum powder and appropriate stirring solvent are evenly become to liquid, the mixture making is coated in and on 7628 electron level glass cloth, in 150-170 DEG C of baking oven, toasts 5-8Min and make prepreg;
B, making table material glue prepreg, Resin A, flexibilizer B, curing agent, promoter, coupling agent and the silica of processing with silanes surface conditioning agent, aluminium hydroxide and appropriate stirring solvent are evenly become to liquid, the mixture making is coated in and on 7628 electron level glass cloth, in 150-170 DEG C of baking oven, toasts 7-10Min and make semi-solid preparation;
C, folded joining, join two-layer Copper Foil by folded in two-layer copper coin, in two-layer Copper Foil, fold and join two-layer table material glue prepreg, finally in two-layer table material glue prepreg, fold and join some layers of lining glue prepreg.
2.d, compacting, put into hot press hot pressing 120min-135min by folded group material of having joined, then put into the cold press 55min-65min that colds pressing.
3. a kind of high CTI value copper-clad plate production method according to claim 1, is characterized in that the proportioning of described table material glue prepreg is: matrix resin is 1000 parts of epoxy resin A, flexibilizer B 10-30 part, 534 parts, aluminium hydroxide; Silica 50-100 part; Curing agent is 23.1 parts of electron level dicyandiamides, and promoter is 0.5 part of tertiary amines promoter, and coupling agent is 2.5 parts of KH560 type silane coupling agents, solvent 100-250 part, and above raw material is calculated by mass.
4. a kind of high CTI value copper-clad plate production method according to claim 2, is characterized in that: matrix resin also can mix according to a certain percentage with one or more common brominated epoxy resins and one or more halogen-free epoxy resins; 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.
5. a kind of high CTI value copper-clad plate production method according to claim 2, is characterized in that: the epoxide equivalent of matrix resin is 350-450 content of inorganic chlorine≤350ppm, bromine content≤20ppm; Described flexibilizer and silica are all to use silanes surface conditioning agent to carry out surface treatment, particle diameter≤5 μ m;
A kind of high CTI value copper-clad plate production method according to claim 1, the proportioning that it is characterized in that described lining glue prepreg is: matrix resin is that 1000 parts of brominated epoxy resin A, 100 parts of talcum powder, 00 part of silica 1, curing agent are that 21.6 parts of electron level dicyandiamides, promoter are 0.5 part of tertiary amines promoter, coupling agent is 2 parts of KH560 type silane coupling agents, 246.2 parts of solvents, above raw material is calculated by mass.
6. a kind of high CTI value copper-clad plate production method according to claim 4, the epoxide equivalent 400-500 of the matrix resin described in it is characterized in that, content of inorganic chlorine≤500ppm, bromine content≤30ppm; Described talcum powder is for using silanes surface conditioning agent to carry out surface treatment; Solvent is a kind of in dimethyl formamide, acetone, butanone, alcohol or several mixtures.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105196649A (en) * | 2015-09-02 | 2015-12-30 | 铜陵翔宇商贸有限公司 | Copper-clad plate manufacturing method |
| CN105196665A (en) * | 2015-09-02 | 2015-12-30 | 铜陵翔宇商贸有限公司 | High frequency copper-clad plate manufacturing method |
| CN105196678A (en) * | 2015-09-02 | 2015-12-30 | 铜陵翔宇商贸有限公司 | Method for manufacturing gray copper-clad plate |
| CN107163274A (en) * | 2017-06-20 | 2017-09-15 | 苏州生益科技有限公司 | A kind of low flow prepreg |
| CN107791627A (en) * | 2017-10-27 | 2018-03-13 | 景旺电子科技(龙川)有限公司 | A kind of metal-based copper-clad plate preparation method of resinous composition |
| CN111605269A (en) * | 2020-05-20 | 2020-09-01 | 山东金宝电子股份有限公司 | FR4 copper-clad plate with high relative tracking index and high heat resistance and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105196649A (en) * | 2015-09-02 | 2015-12-30 | 铜陵翔宇商贸有限公司 | Copper-clad plate manufacturing method |
| CN105196665A (en) * | 2015-09-02 | 2015-12-30 | 铜陵翔宇商贸有限公司 | High frequency copper-clad plate manufacturing method |
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| CN111605269A (en) * | 2020-05-20 | 2020-09-01 | 山东金宝电子股份有限公司 | FR4 copper-clad plate with high relative tracking index and high heat resistance and preparation method thereof |
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Application publication date: 20140813 |