CN101547558A - Copper clad base plate and preparation method thereof - Google Patents
Copper clad base plate and preparation method thereof Download PDFInfo
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- CN101547558A CN101547558A CN200910038822A CN200910038822A CN101547558A CN 101547558 A CN101547558 A CN 101547558A CN 200910038822 A CN200910038822 A CN 200910038822A CN 200910038822 A CN200910038822 A CN 200910038822A CN 101547558 A CN101547558 A CN 101547558A
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Abstract
The invention discloses a copper clad base plate and a preparation method thereof. The copper clad base plate is formed by pressing prepreg and copper clad and adding compound quartz powder functioning as inorganic filler to glue solution made of the prepreg, wherein the weight of the compound quartz powder occupies 5-50 percent of the total weight of the glue solution. The preparation method of the copper clad base plate comprises the following steps: (1) under the room temperature, respectively adding base raw materials for preparing the glue solution to a dispensing container and mixing the base raw materials, adding the compound quartz powder functioning as inorganic filler to the mixture and mixing with the same for 6h, sampling the gel time of the test glue solution and controlling the time between 200s and 300s; (2) making adhesive plaster impregnated with the glue solution pass through a vertical or horizontal impregnating machine, and preparing the prepreg by controlling wind temperature and furnace temperature; and (3) pressing: after combining the cut prepreg with the copper clad, the cut prepreg and the copper clad are put into a vacuum hot press to be pressed for obtaining the copper clad base plate. The invention can greatly lower the cost of the glue solution, lower the coefficient of heat expansion of the product, improve the reliability of the copper clad base plate in the preparation of printed circuit boards, and ensure the improvement on the mechanical property and the electric property of the product.
Description
Technical field
The present invention relates to a kind of copper clad foil substrate that in the printed circuit board (PCB) industry, uses and preparation method thereof, relate generally to the copper clad foil substrate that fiberglass-based epoxy resin is made, be applicable to various types of copper-clad plate characteristics are promoted.
Background technology
(Claire (Coombs) editor, 3 editions, Mike Lao Xier books company (McGraw-Hill Book Co.) published in 1988) to the classification of copper-clad plate (being copper clad foil substrate), is divided into FR-2, FR-3, FR4, CEM-1 etc. with it according to the printed circuit handbook.FR-2 refers to paper-based phenolic resin making copper-clad plate, and FR-3 refers to paper substrate epoxy resin making copper-clad plate, and FR-4 refers to glass basic ring epoxy resins type making copper-clad plate.
Adding filler in this composite material of copper-clad plate serves as filler, fire retardant etc. and just had been suggested before early.The adding of filler can improve the mechanical performance and the electric property of material.Just propose to add filler in No. 5264065, the United States Patent (USP), in order to reduce the thermal coefficient of expansion of copper-clad plate.And the reliability of copper-clad plate thermal coefficient of expansion when reducing follow-up making printed circuit board (PCB) improves a lot.In addition, No. 222950, Japan Patent, No. 97633, Japan Patent, Japan Patent all have announcement No. 120330, add filler and are used to limit resin flows and improvement punching.Disclose in No. 4960634, the United States Patent (USP) and use zinc oxide as a kind of additive of improveing thermal conductivity.Disclose in No. 133440, the Japan Patent, heating talcum powder to 1000 ℃-2000 ℃, remove the crystallization water after, add in the copper-clad plate dimensional stability with improvement sheet material.No. 6322885, United States Patent (USP) discloses, and uses talcum powder to be used to improve the characteristics such as thermal coefficient of expansion, boring of copper-clad plate, does not reduce the electrical strength of copper-clad plate simultaneously.
Nearly 2 years,, thermal endurance, the mechanical performance of copper-clad plate have been made higher requirement along with the unleaded implementation of electron trade.High glass transition temperature (refer to about 150 ℃ or higher), low-expansion copper-clad plate then can adapt to this requirement preferably, and use amount increases sharply.But also there are some problems in this type of copper-clad plate, and is more crisp such as resin, and with the peel strength decline of Copper Foil, hardness further increases behind interpolation inorganic filler such as the silicon dioxide.When so just having caused punching during making printed circuit board (PCB), cutting, boring, the white edge phenomenon takes place, dust is more, stamping knife, drill point serious wear.At the problems referred to above, carried out a lot of correlative studys in the industry, but found that various inorganic fillers respectively have pluses and minuses, for example the silicon dioxide advantage is significantly not reduce the characteristics such as Copper Foil peel strength of copper-clad plate, but its hardness is very big, and the drill point wearing and tearing when making boring increase very fast.The talcum powder advantage is the boring excellent performance, but can reduce the Copper Foil peel strength of copper-clad plate.Aluminium hydroxide has outstanding fire retardation, but its heat resistance is poor, also can reduce the Copper Foil peel strength of copper-clad plate simultaneously.
Compound silica flour is a kind of composite material of uniqueness, is select for use several inorganic minerals to smelt fusion to make.Silica comprises 58%-62% wherein, alundum (Al accounts for 28%-32%, and other oxides such as diboron trioxide of 9-11%.Compound silica flour is mainly used in the composite filling material of each electronic product, wherein to the west of BIC Corp's trade mark be that the properties of product of G2-C are preferable.
Summary of the invention
The object of the invention provides a kind of copper clad foil substrate and preparation method thereof, to reduce cost, improves mechanical performance of products and electric property.
The present invention seeks to realize like this:
A kind of copper clad foil substrate is formed by prepreg and Copper Foil compacting, adds inorganic filler in making the glue of prepreg, and this inorganic filler is compound silica flour, and addition accounts for the 5%-50% of glue total weight; Preferable addition accounts for the 15%-25% of glue total weight, prepares copper-clad plate with this glue, can improve its many-sided performance.
Described compound silica flour is to select for use several inorganic minerals to smelt fusion to make, as by 55%-65% silicon dioxide, the 15%-35% alundum (Al, other oxide of fusion of 5%-15% diboron trioxide and 0%-10% is formed, and other oxide is meant calcium oxide, sodium oxide molybdena or potassium oxide.Silicon dioxide wherein and alundum (Al by having formed the composite junction crystal after the fusion refining, do not contain free silicon dioxide, alundum (Al composition.Compound silica flour maximum particle diameter is no more than 50 microns, and average grain diameter (D50) is no more than 10 microns, is good with the 1-4 micron.The anionic content that water can extract also should be at percentage by weight below 0.01%.In addition, employed compound silica flour can be not surface treated particle, also can be through the product after certain silane finish surface treatment.
The preparation method of described copper clad foil substrate may further comprise the steps:
(1) preparation of glue: under the room temperature, (basic material is meant that preparation does not contain the required raw material of glue of inorganic filler to add the basic material of preparing glue in proportion container respectively, basic material difference for different copper clad foil substrate preparation glues, as for the halogen-free flameproof copper clad foil substrate, the basic material of preparation glue comprises solvent, curing agent, epoxy resin, fire retardant, special composition in curing accelerator and other prescription, this is a known technology), after the stirring, add the compound silica flour of inorganic filler, stirred again 6 hours, the gel time of sampling and testing glue (170 ℃ of hot plates), gel time is controlled by the addition of curing accelerator, and its gel time should be controlled between 200～300 seconds;
(2) impregnation: the adhesive plaster that will soak glue by control wind-warm syndrome and furnace temperature, makes prepreg by vertical or horizontal type impregnation machine;
(3) compacting: after the prepreg that cuts and Copper Foil combined, put into the vacuum hotpressing machine, press down at certain temperature, pressure, time and vacuum condition and make copper clad foil substrate.
Should note in the present invention:
(1) the adding mode of curing agent and curing accelerator: before use, should earlier curing agent and curing accelerator be dissolved in solvent, be mixed with solution, stand-by.
(2) solvent: with dimethyl formamide DMF, cyclohexanone, butanone, propylene glycol monomethyl ether, propylene glycol monomethyl ether amyl acetate etc. or its combination as dicyandiamide solution, with acetone, butanone or its combination as diluent.
(3) disperse: after adding the compound silica flour of inorganic filler, be evenly distributed in the glue, need to mix, to avoid the adhesive aggregation effect between the particle through higher shear power for making it.
(4) gelation time is regulated: the gelation time of the glue of preparing can be regulated with the addition of curing accelerator.
Gelation time: the gelation time of resin all can prepare sheet material by gluing machine and press in 200～300 seconds scope behind the glue through joining.
Solid content: the solid content of general glue is at 50%--70%wt.
Storage period: the glue of being prepared can at room temperature be stored more than the two weeks.
After adopting such scheme, theory analysis of the present invention:
The filler that is applied to copper clad foil substrate need meet multiple requirement.At first, filler should be compatible with the epoxy-resin systems in the glue, and possess good solvent resistance, can be by the solvent in the glue, and for example dimethyl formamide (DMF) and acetone corrode.Secondly, filler should be dispersed in the epoxy resin adhesive liquid, and its density also should be approaching with glue, thereby after being dispersed in the glue, free settling not in the process that glue is deposited also is difficult for floating.Once more, filler can not significantly reduce the electrical property and the thermal endurance of copper clad foil substrate.And above some compound silica flour all can satisfy.Also there are some can satisfy above some requirement equally in other filler, for example silicon dioxide, talcum powder etc., but silicon dioxide is because hardness is too big, its the copper clad foil substrate hardness that causes making of joining that adds increases, the wearing and tearing of drill point increase greatly when holing in the preparation of printed circuit board, cause the loss of drill point to increase, simultaneously more frequent change the reduction that at the printed circuit board drilling processing procedure, can cause efficient.Though and talcous adding can not increase the wearing and tearing of drill point, it can cause, and the peel strength of resin and Copper Foil significantly reduces in the copper clad foil substrate, thereby influences its reliability.The hardness of compound silica flour is because the mixed reason of various oxide makes relative silicon dioxide reduce greatly.Its adding can't increase the wearing and tearing of drill point significantly.And its adding is to the also not significantly reduction of peel strength of resin in the copper clad foil substrate and Copper Foil.Simultaneously, the adding of compound silica flour also improves significantly to the multinomial performance of copper clad foil substrate, for example, reduced the thermal coefficient of expansion of copper clad foil substrate Z-direction (out-of-plane direction) greatly, increased the reliability in the printed circuit board (PCB) processing procedure, reduced because the printed circuit board (PCB) inefficacy that resin system in the copper clad foil substrate and Copper Foil thermal expansion coefficient difference produce.For another example, the adding of compound silica flour can improve epoxy-resin systems, the toughness of the epoxy-resin systems that solidifies of phenolic aldehyde particularly thinks that in theory its possible reason is to be dispersed in the diffusion that compound silica flour in the resin system can stop the epoxy-resin systems micro-crack.
Glue of the present invention has added the compound silica flour of inorganic filler, possesses following some beneficial effect:
One, the adding of the compound silica flour of inorganic filler can reduce the cost of glue greatly;
Two, the adding of the compound silica flour of inorganic filler can reduce the thermal coefficient of expansion of copper clad foil substrate greatly, and improves its reliability in the printed circuit board (PCB) preparation;
Three, the adding of the compound silica flour of inorganic filler, less to other performance impact of copper clad foil substrate, in can not reduce copper clad foil substrate significantly peel strength or when boring, increase the drill point wearing and tearing, also can remarkable reduction do not arranged to the substrate electrical property.
Embodiment
1, specific embodiment prescription
One of embodiment XUS19074 (epoxy resin that DOW Chemical is produced, possess 170 ℃ Tg after the curing) 49.5%, curing agent 3363 (linear phenolic resin of the gloomy product of writing brush) 16.5%, propylene glycol monomethyl ether 22.0%, curing accelerator 2-ethyl-4-methylimidazole 0.3%, G2-C (gram company in Thebe produces compound silica flour) 11.7%.
Two (comparative example) XUS19074 of embodiment (epoxy resin that DOW Chemical is produced, possess 170 ℃ Tg after the curing) 49.5%, curing agent 3363 (linear phenolic resin of the gloomy product of writing brush) 16.5%, propylene glycol monomethyl ether 22.0%, curing accelerator 2-ethyl-4-methylimidazole 0.3%, 925 (gram company in Thebe produces silicon dioxide) 11.7%.
Three (comparative example) XUS19074 of embodiment (epoxy resin that DOW Chemical is produced, possess 170 ℃ Tg after the curing) 49.5%, curing agent 3363 (linear phenolic resin of the gloomy product of writing brush) 16.5%, propylene glycol monomethyl ether 22.0%, 0.3% part of curing accelerator 2-ethyl-4-methylimidazole, talcum powder 11.7%.
Four XUS19074 of the embodiment (epoxy resin that DOW Chemical is produced, possess 170 ℃ Tg after the curing) 49.5%, curing agent 3363 (linear phenolic resin of the gloomy product of writing brush) 16.5%, propylene glycol monomethyl ether 22.0%, curing accelerator 2-ethyl-4-methylimidazole 0.3%, G2-C-ARI (the compound silica flour after certain silane surface treatment of industry of Thebe gram company) 11.7%.
Five XUS19074 of the embodiment (epoxy resin that DOW Chemical is produced, possess 170 ℃ Tg after the curing) 37.4%, curing agent 3363 (linear phenolic resin of the gloomy product of writing brush) 12.5%, propylene glycol monomethyl ether 16.6%, curing accelerator 2-ethyl-4-methylimidazole 0.3%, G2-C (gram company in Thebe produces compound silica flour) 33.2%.
Six XUS19074 of the embodiment (epoxy resin that DOW Chemical is produced, possess 170 ℃ Tg after the curing) 37.4%, curing agent 3363 (linear phenolic resin of the gloomy product of writing brush) 12.5%, propylene glycol monomethyl ether 16.6%, curing accelerator 2-ethyl-4-methylimidazole 0.3%, G2-C-ARI (gram company in Thebe produces compound silica flour) 33.2%.
Seven XUS19041 of the embodiment (epoxy resin that DOW Chemical is produced, possess 150 ℃ Tg after the curing) 62.7%, curing agent dicyandiamide 1.6%, N, dinethylformamide 15.7%, acetone 6.2%, curing accelerator 2-ethyl-4-methylimidazole 0.2%, G2-C (gram company in Thebe produces compound silica flour) 13.6%.
Eight (comparative example) XUS19041 of embodiment (epoxy resin that DOW Chemical is produced, possess 150 ℃ Tg after the curing) 62.7%, curing agent dicyandiamide 1.6%, N, dinethylformamide 15.7%, acetone 6.2%, curing accelerator 2-ethyl-4-methylimidazole 0.2%, 925 (gram company in Thebe produces silicon dioxide) 13.6%.
Nine (comparative example) XUS19041 of embodiment (epoxy resin that DOW Chemical is produced possesses 150 ℃ Tg after the curing) 62.7%, curing agent dicyandiamide 1.6%, N, dinethylformamide 15.7%, acetone 6.2%, curing accelerator 2-ethyl-4-methylimidazole 0.2%, talcum powder 13.6%.
Ten XUS19041 of the embodiment (epoxy resin that DOW Chemical is produced, possess 150 ℃ Tg after the curing) 62.7%, curing agent dicyandiamide 1.6%, N, dinethylformamide 15.7%, acetone 6.2%, curing accelerator 2-ethyl-4-methylimidazole 0.2%, G2-C-ARI (gram company in Thebe produces compound silica flour) 13.6%.
2, the preparation technology of glue
1) solvent is added in the proportion container;
2) stir the solution that adds epoxy resin, curing agent solution and curing accelerator down respectively, curing agent: solvent=1:6 (ratio of weight and number), curing accelerator/solvent=1:6 (ratio of weight and number);
3) behind the stirring 30min, add inorganic filler;
4) continued high-speed stirred 6 hours, the gel time of sampling and testing glue (170 ℃ of constant temperature hot plates) is (200～300) second.
3, impregnation
The adhesive plaster that will soak the halogen-free flameproof glue by conditions such as control extruding wheel speed, linear speed, wind-warm syndrome and furnace temperature, makes prepreg by vertical or horizontal type impregnation machine.
With vertical impregnation machine is example:
The proportion of glue: 1.10～1.20;
Extruding wheel speed :-1.8～-2.5 ± 0.1M/min;
Main line speed: 5～14M/min;
Wind-warm syndrome: 130～160 ℃;
Furnace temperature: 140～180 ℃.
Make prepreg by above condition.
4, compacting
After the prepreg that cuts and Copper Foil combined, put into the vacuum hotpressing machine, obtaining substrate by following formula compacting.
Temperature formula: 130 ℃/30min+160 ℃/30min+180 ℃/20min+210 ℃/180min
Pressure formula: 20Kgf.cm-2/30min+50Kgf.cm-2/15min+95Kgf.cm-2/150min+20Kg f.cm-2/65min
Vacuum is set: 30mmHg/130min+760mmHg/130min
5, following is the substrate performance of part prescription
Conclusion:
1, add various inorganic fillers all have reduction to the thermal coefficient of expansion of copper-clad plate effect, addition is big more, and it is big more that thermal coefficient of expansion reduces amplitude;
2, the compound silica flour of adding is little to the peel strength influence of copper-clad plate, and adds the peel strength that talcum powder can reduce copper-clad plate significantly;
3, the compound silica flour of adding can influence not quite the basic electric property of copper-clad plate.
Claims (8)
1, a kind of copper clad foil substrate is formed by prepreg and Copper Foil compacting, and it is characterized in that: add inorganic filler in making the glue of prepreg, this inorganic filler is compound silica flour, and addition accounts for the 5%-50% of glue total weight.
2, a kind of copper clad foil substrate as claimed in claim 1, it is characterized in that: compound silica flour addition accounts for the 15%-25% of glue total weight.
3, a kind of copper clad foil substrate as claimed in claim 1, it is characterized in that: compound silica flour is by 55%-65% silicon dioxide, the 15%-35% alundum (Al, other oxide of fusion of 5%-15% diboron trioxide and 0%-10% is formed, and other oxide is meant calcium oxide, sodium oxide molybdena or potassium oxide.
4, a kind of copper clad foil substrate as claimed in claim 3 is characterized in that: silicon dioxide and alundum (Al have formed the composite junction crystal after refining by fusion, do not contain free silicon dioxide, alundum (Al composition.
5, a kind of copper clad foil substrate as claimed in claim 1 is characterized in that: compound silica flour maximum particle diameter is no more than 50 microns, and average grain diameter is no more than 10 microns.
6, a kind of copper clad foil substrate as claimed in claim 1 is characterized in that: the anionic content that the compound silica flour that adds in the glue, its water can extract is at percentage by weight below 0.01%.
7, a kind of copper clad foil substrate as claimed in claim 1 is characterized in that: compound silica flour is not surface treated particle, or through the product after certain silane finish surface treatment.
8, a kind of copper clad foil substrate as claimed in claim 1, it is characterized in that: the preparation method may further comprise the steps:
(1) preparation of glue: under the room temperature, after in proportion container, adding the basic material and stirring of preparation glue respectively, add the compound silica flour of inorganic filler, stirred again 6 hours, the gel time of sampling and testing glue, gel time is controlled by the addition of curing accelerator, and its gel time should be controlled between 200～300 seconds;
(2) impregnation: the adhesive plaster that will soak glue by control wind-warm syndrome and furnace temperature, makes prepreg by vertical or horizontal type impregnation machine;
(3) compacting: after the prepreg that cuts and Copper Foil combined, put into the vacuum hotpressing machine, suppress obtaining copper clad foil substrate.
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