CN103965606A - Low dielectric material - Google Patents
Low dielectric material Download PDFInfo
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- CN103965606A CN103965606A CN201310043987.0A CN201310043987A CN103965606A CN 103965606 A CN103965606 A CN 103965606A CN 201310043987 A CN201310043987 A CN 201310043987A CN 103965606 A CN103965606 A CN 103965606A
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- dielectric materials
- bismaleimides
- polyphenylene oxide
- polymeric additive
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- VXEQSSUFHYCCIU-UHFFFAOYSA-N CCC(CC(O)O1)C1=O Chemical compound CCC(CC(O)O1)C1=O VXEQSSUFHYCCIU-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to a low dielectric material. The low dielectric material includes, by weight, 40-80 parts of polyphenyl ether with the number average molecular weight Mn of 1000-4000, the weight average molecular weight Mw of 1000-7000 and the Mw/Mn ratio of 1.0-1.8, 5-30 parts of bimaleimide and 5-30 parts of a polymer additive, and the Dk value and the Df value of the low dielectric material are 3.75-4.0 and 0.0025-0.0045 respectively. The low dielectric material can be applied to semi-cured films or circuit substrate insulating layers, and has the characteristics of high Tg, low thermal expansion coefficient, low water absorption rate, and excellent dielectric properties like dielectric constant (Dk) and dielectric loss (Df).
Description
Technical field
The present invention is about a kind of dielectric materials, particularly a kind of thermosetting resin composition.
Background technology
Along with the leap of the flourish of transmission over radio product and high-frequency transmission technology, the material of existing epoxy resin and phenolic resin systems cannot meet the demand of advanced application, particularly high frequency printed circuit board.
Baseplate material as the printed circuit board (PCB) of low-dielectric loss has fluorine-type resin, but this kind of resin cost is high, processing is difficult for, and application is confined to military affairs and aerospace applications.In addition, polyphenylene oxide (PPE) resin is because having good mechanical characteristics and excellent dielectric properties, and for example specific inductivity (Dk) and dielectric loss (Df) become the resin material of the substrate first-selection of high frequency printed circuit board.
Yet polyphenylene oxide is a kind of thermoplastic resin, is directly used in and in copper clad laminate, is had following shortcoming: melt viscosity is high, is difficult to machine-shaping; Poor solvent resistance easily causes wire adhere to not firm or come off in the environment of the solvent cleaning of print circuit plates making process; And fusing point is close with glass transition temp (Tg), be difficult to bear 250 ℃ of above scolding tin operations in printed circuit board (PCB) processing procedure.Therefore, PPE just can meet the service requirements of printed circuit board (PCB) through thermoset upgrading.
The thermoset upgrading of PPE generally has following two kinds of modes: on PPE molecular structure, introduce crosslinkable active group, make it to become thermosetting resin.Or, by blend upgrading or IPN netted (IPN) technology, introduce other thermosetting resin, form the same with thermosetting compound material of blend.But due to the difference in chemical structure polarity, PPE and those active groups or thermosetting resin often occur that compatibility is not good, processing is difficult for or lose the original excellent specific property of PPE and restriction to some extent.
Therefore, how to develop and there are excellent dielectric properties and meet other characteristic demand of printed circuit board (PCB), material such as the characteristic of high Tg, low thermal coefficient of expansion, low water absorption, and be applied to the manufacture of high frequency printed circuit board, be the problem that present stage printed circuit board material supplier desires most ardently solution.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of dielectric materials, there is excellent dielectric properties, low thermal coefficient of expansion and low water absorbable.
In order to reach above-mentioned purpose, the invention provides a kind of dielectric materials, comprise:
(A) polyphenylene oxide of 40 ~ 80 weight parts (PPE), number average molecular mass Mn=10004000, weight average molecular weight Mw=1000～7000, and Mw/Mn=1.0～1.8;
(B) bismaleimides of 5 ~ 30 weight parts (BMI); And
(C) polymeric additive of 5 ~ 30 weight parts;
Wherein, the Dk value of this dielectric materials: 3.75～4.0, Df value: 0.0025～0.0045.
In dielectric materials of the present invention, the structural formula of this polyphenylene oxide is as follows:
Wherein Y can be at least one carbon, at least one oxygen, at least one phenyl ring or above combination.
In dielectric materials of the present invention, bismaleimides is selected from least one in following group:
Phenylmethane maleimide (Phenylmethane maleimide)
N >=1 wherein;
Dihydroxyphenyl propane Diphenyl Ether Bismaleimide (Bisphenol A diphenyl ether bismaleimide)
3,3 '-dimethyl-5,5 '-diethyl-4,4 '-diphenylethane bismaleimides
(3,3’dimethyl-5,5’-diethyl-4,4’-diphenylethane bismaleimide)
1,6-bismaleimides-(2,2,4-trimethylammonium) hexane (1,6-bismaleimide-(2,2,4-trimethyl) hexane)
In dielectric materials of the present invention, this polymeric additive can be selected from least one in following group: dienite (Homopolymers of Butadiene)
Y=70% wherein, x+z=30%;
Divinyl and styrene random multipolymer (Random copolymers of butadiene and styrene)
Y=30% wherein, x+z=70%, w >=1, styrene content is 25wt%;
Maleation polyhutadiene (Maleinized Polybutadiene)
Y=28% wherein, x+z=72%, maleic anhydride (MA) content=8wt%;
The multipolymer of divinyl, vinylbenzene and divinylbenzene; And
Styrene-maleic anhydride copolymer compound (Styrene Maleic Anhydride copolymer)
X=1 ~ 8 wherein, n >=1.
In preferred case, still the alternative linking agent (crosslinking agent) that adds is further to improve the cross-linking density of resin in the present invention, and this linking agent can be selected from least one in the following group of 40 ~ 80 weight parts:
Triallyl isocyanate (TAIC)
Triallyl cyanate (TAC)
4 t-butyl styrene (TBS)
The present invention can add usings the superoxide of 116 ℃ ~ 128 ℃ of 10 hour transformation period, temperature ranges that the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent calculates 2 ~ 8ph as catalyst (catalyst) or is called crosslinking accelerator, for making linking agent and its kind resin that bonding interaction effectively occur.The superoxide that the present invention is applicable, for example dicumyl peroxide, α, α '-bis-(tert-butyl peroxy base) diisopropylbenzene(DIPB) and 2,5-dimethyl 2,5-bis(t-butylperoxy) hexin-3.
The present invention can further add the inorganic fillings (filler) that calculates 8 ~ 50phr with the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent, with increase dielectric materials heat conductivity, improve the characteristics such as its thermal expansivity and physical strength.The applicable inorganic fillings of the present invention is fused silica, spherical silica, talcum and pure aluminium silicate for example.
In order to improve the flame retardancy of dielectric materials of the present invention, it is that the non-halogen of incombustible agent or 12 ~ 14phr is incombustible agent that the present invention still can add the halogen that calculates 7 ~ 15phr with the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent.Halogen is that incombustible agent comprises, for example TDE.Non-halogen is that incombustible agent comprises, for example, purchased from phosphonium flame retardant, the phosphoric acid ester of ALBEMARLE company.Phosphoric acid ester for example has the compound (Resorcinol two [two (2,6 3,5-dimethylphenyl) phosphoric acid ester]) of following molecular formula:
〔OC
6H
3(CH
3)
2〕
2P(O)OC
6H
4OP(O)〔OC
6H
3(CH
3)
2〕
2
Dielectric materials of the present invention, not containing epoxy resin, can cause Dk/Df cannot reach desired value because add epoxy resin, and its reason is that epoxy resin can produce too much OH base after open loop, and then causes Dk and Df value to reduce.
Dielectric materials provided by the present invention, can be applicable to semicure film or circuit substrate insulation layer, and has for example characteristic of specific inductivity (Dk) and dielectric loss (Df) of high Tg, low thermal coefficient of expansion, low water absorption and excellent dielectric properties.
Embodiment
For above-mentioned purpose of the present invention and other object, feature & benefits can be become apparent, especially exemplified by a plurality of embodiment, be described in detail as follows:
Following examples 1 ~ 7 are used compositions of thermosetting resin of the present invention to manufacture prepreg in a continuous process.Normally with glasscloth, make base material.The glasscloth of web-like enters gluing groove through a series of rollers continuously, and thermoset composition of the present invention is housed in groove.In gluing groove, glasscloth is fully infiltrated by compositions of thermosetting resin, then through metering roll, strikes off unnecessary resin, enters the roasting regular hour of gluing bake oven, solvent is evaporated and compositions of thermosetting resin is solidified, cooling, rolling, forms prepreg.
The electronic-grade of certain number 2116 glasscloths were soaked to the prepreg stack alignment that above-mentioned compositions of thermosetting resin is made, respectively join up and down the electrolytic copper foil of a loz, in vacuum press, under pressure 40-900psi, temperature rises to 200 ℃ by 80 ℃ in 30min, then at 200 ℃ of hot pressing 120min, then in 30min, be cooled to room temperature, make certain thickness double face copper.Usually, 1.0nm thickness needs 4 2116 prepregs, and 0.8mm needs 4 2116 prepregs, and 2.0mm needs 10 21160 prepregs.
Compositions of thermosetting resin provided by the invention forms stable homogeneous phase solution in low boiling point solvent, the copper-clad plate of manufacturing with it, with reference to IPC-TM-650, carry out second-order transition temperature, heat decomposition temperature, the thermally stratified layer time, scolding tin thermotolerance (288 ℃), thermal expansivity, water-intake rate, thermal conductivity, specific inductivity and dielectric loss factor, flame resistivity index detects, detected result shows: have high glass-transition temperature (Tg), excellent dielectric properties, low-expansion coefficient, low water absorption, the characteristics such as high heat shock resistance and high thermoconductivity, be suitable for doing the baseplate material of electronic component and unicircuit (IC) encapsulation.
The impact of embodiment 1PPE proportional difference
The usage ratio relation of comparison Tg and Dk, Df and PPE, the too high or too low meeting of PPE amount causes Tg too low, and the amount of PPE also has impact to Dk, Df simultaneously, and when PPE measures highly, Dk, Df are all high, and when PPE measures when low, Dk, Df are all low.Want better situation, Dk and Df are all low.In addition, add PPE and can promote thermal expansivity, therefore reduce thermal expansivity to add the mode of BMI.PPE(polyphenylene oxide in table) model SA9000 is purchased from Sabic company.Chemical name, for poly-2,6-dimethyl Isosorbide-5-Nitrae-phenylate, is called for short PPO(Polyphenylene Oxide) or PPE(Polypheylene ether), polyphenylene oxide or polyhenylene ether be called again.
The impact of embodiment 2BMI resin structure and proportional difference
Comparison thermal expansivity and BMI(bismaleimides) usage ratio relation, the ratio of BMI is higher, it is lower that thermal expansivity falls.In the present embodiment, the comparison of BMI can be divided into three parts, and A1～A5 is the one species BMI resin of different ratios, and A6-A8 is same ratio but different types of BMI, and A9-A15 is the comparison that mixes multiple BMI.In table, BMI model 2300,4000,5100, TMH are purchased from large and change into industry (DaiwakaseilndustryCO., LTD), the following synopsis of chemical name.
| BMI-2300 | Toluene maleimide |
| BMI-4000 | Two [4-(the 4-maleimide phenoxy group) phenyl] propane of 2,2'- |
| BMI-5100 | 3,3'-dimethyl 5,5'-diethyl-4,4 '-dimethylbenzene bismaleimides |
| BMI-TMH | 1,6'-bismaleimides-(2,2,4-trimethylammonium) hexane |
From A1～A5, the different ratios of identical type BMI can effectively reduce thermal expansivity, but the effect that also can be improved water-intake rate.From A6-A8, different BMI can effectively reduce thermal expansivity, but water-intake rate is also had to impact.From A9-A15, different BMI combinations also can effectively reduce thermal expansivity, also can take into account water-intake rate.The object that the present invention adds BMI is to reduce thermal expansivity, but because water-intake rate also can improve with usage ratio and the combination difference of BMI, therefore reduce water-intake rate to add polymeric additive again.
The impact of embodiment 3 polymeric additive structures and proportional difference
The usage ratio relation of comparison water-intake rate and polymeric additive (polymeradditves), use two kinds of polyhutadiene (Polybutadiene) and styrene-maleic anhydride copolymer compounds (SMA), when using same polyhutadiene, ratio is higher, water-intake rate is lower, but thermal expansivity also can be along with rising.Using polyhutadiene not of the same race, and collocation SMA is when used, and can find out that SMA is comparatively effective to reducing water-intake rate, also can reduce thermal expansivity, but poor in the part performance of Df, and use polyhutadiene can make up SMA in the deficiency of Df part.In table, divinyl model Ricon100, Ricon130MA8, Ricon150, Ricon257 are purchased from Sartomer, the following synopsis of chemical name.
| Ricon100 | Butadiene-styrene copolymer |
| Ricon130MA8 | Polyhutadiene-maleic anhydride adduct |
| Ricon150 | Polybutadiene |
| Ricon257 | The polyhutadiene of graft phenylethene and benzene class in toluene solution |
In table, SMA lists the ratio that S:M=3:1 means vinylbenzene (Styrene) and maleic anhydride (MaleicAnhydride), and general more conventional proportional range is 1:1 ~ 12:1.
The impact of embodiment 4 linking agent kind differences
Dielectric materials of the present invention more comprises at least one linking agent in the following group of being selected from of 40 ~ 80 weight parts: triallyl cyanate, triallyl isocyanate and 4 t-butyl styrene.Compare the impact of different linking agents (crosslinkingagent) on physical property of the present invention, use Tg, the thermal expansivity of triallyl cyanate (TAC) poor, Dk, Df and water-intake rate are general.Use the physical properties of triallyl isocyanate (TAIC) comparatively average.Use thermal expansivity, water-intake rate and the Df of 4 t-butyl styrene (TBS) better, but Dk value is on the low side.
The impact of embodiment 5 incombustible agent kind differences
The part of incombustible agent, depending on physical properties demand, the different incombustible agent of can arranging in pairs or groups.The part that contains halogen incombustible agent can be added 7～15phr (with PPE, BMI, polymeric additive and linking agent weight part summation are calculated) TDE (decabromodiphenylethane), the part of halogen incombustible agent can be added 12～14phr (with PPE, BMI, polymeric additive and linking agent weight part summation are calculated) be selected from least one in following group: purchased from phosphonium flame retardant and the phosphoric acid ester of ALBEMARLE company (Resorcinol pairs [two (2, 6 3,5-dimethylphenyls) phosphoric acid ester) (Tetrakis (2, 6-dimethylphenyl) 1, 3-phenylene bisphosphate)).
The impact of embodiment 6 inorganic fillings kinds and proportional difference
As for inorganic fillings, depending on physical properties demand, can add 8 ~ 50phr (calculating with PPE, BMI, polymeric additive and linking agent summation) different inorganic fillings, for example fused silica, spherical silica.In the fused silica of same ratio, the situation of spherical silica, use spherical silica, Dk, Df are all used fused silica person low.
The impact of embodiment 7 crosslinking accelerator kinds and proportional difference
Dielectric materials of the present invention more comprises 10 hour transformation period of the 2 ~ 8phr weight part summation of PPE, BMI, polymeric additive and linking agent (take calculate) and the superoxide that temperature range is 116 ℃～128 ℃.The part of crosslinking accelerator (catalyst (catalysts)), depending on physical properties demand, the different crosslinking accelerator of can arranging in pairs or groups.The present invention can use the superoxide of 116 ℃～128 ℃ of 10 hour transformation period, temperature range, 10 hour transformation period of better use, the temperature superoxide of 119 ℃.
Dielectric materials of the present invention is used PPE but does not add epoxy resin, because add epoxy resin, can cause Dk/Df cannot reach desired value, and its reason is that epoxy resin can produce too much OH base after open loop, and then causes Dk and Df value to reduce.
The above; be only preferred embodiment of the present invention, not in order to limit the present invention, all scopes of the present invention should be as the criterion with the content of claims; all and patent spirit of the present invention has the embodiment of similar variation, all should be contained in scope of patent protection of the present invention.
Claims (11)
1. a dielectric materials, is characterized in that, comprises:
(A) polyphenylene oxide of 40 ~ 80 weight parts, number average molecular mass Mn=1000 ~ 4000, weight average molecular weight Mw=1000 ~ 7000, and Mw/Mn=1.0 ~ 1.8;
(B) bismaleimides of 5 ~ 30 weight parts; And
(C) polymeric additive of 5 ~ 30 weight parts;
Wherein, the Dk value of this dielectric materials: 3.75 ~ 4.0, Df value: 0.0025 ~ 0.0045.
2. dielectric materials as claimed in claim 1, is characterized in that, the structural formula of this polyphenylene oxide is as follows:
Y is at least one carbon, at least one oxygen, at least one phenyl ring or above combination.
3. dielectric materials as claimed in claim 1, is characterized in that, this bismaleimides is selected from least one in following group:
Phenylmethane maleimide
N >=1 wherein;
Dihydroxyphenyl propane Diphenyl Ether Bismaleimide
；
3,3 '-dimethyl-5,5 '-diethyl-4,4 '-diphenylethane bismaleimides
；
1,6-bismaleimides-(2,2,4-trimethylammonium) hexane
。
4. dielectric materials as claimed in claim 1, is characterized in that, this polymeric additive is selected from least one in following group:
Dienite
Y=70% wherein, x+z=30%;
Divinyl and styrene random multipolymer
Y=30% wherein, x+z=70%, w >=1, styrene content=25 wt %;
Maleation polyhutadiene
Y=28% wherein, x+z=72%, maleic anhydride content=8 wt %;
The multipolymer of divinyl, vinylbenzene and divinylbenzene; And
Styrene-maleic anhydride copolymer compound
X=1 ~ 8 wherein, n >=1.
5. dielectric materials as claimed in claim 1, is characterized in that, more comprises at least one linking agent in the following group of being selected from of 40 ~ 80 weight parts:
Triallyl isocyanate
Triallyl cyanate
4-t-butyl styrene
。
6. dielectric materials as claimed in claim 5, it is characterized in that, with the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent, calculate the superoxide that more comprises 116 ℃ ~ 128 ℃ of 10 hour transformation period of 2 ~ 8phr and temperature ranges.
7. dielectric materials as claimed in claim 6, it is characterized in that, this superoxide is selected from least one crosslinking accelerator in following group: dicumyl peroxide, two (tert-butyl peroxy base) diisopropylbenzene(DIPB)s and 2 of α α ’ –, 5-dimethyl-2,5-bis(t-butylperoxy) hexin-3.
8. dielectric materials as claimed in claim 5, it is characterized in that, with the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent, calculate and more comprise 8 ~ 50 phr and be selected from least one inorganic fillings in following group: fused silica, spherical silica, talcum and pure aluminium silicate.
9. dielectric materials as claimed in claim 5, is characterized in that, with the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent, calculates the TDE that more comprises 7 ~ 15phr.
10. dielectric materials as claimed in claim 5, it is characterized in that, with the weight part summation of polyphenylene oxide, bismaleimides, polymeric additive and linking agent, calculate and more comprise 12 ~ 14phr and be selected from least one in following group: phosphonium flame retardant and phosphoric acid ester.
11. dielectric materials as claimed in claim 1, is characterized in that, this dielectric materials is not containing epoxy resin.
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