CN100365048C - Resin composition with high dielectric constant and its usage - Google Patents
Resin composition with high dielectric constant and its usage Download PDFInfo
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- CN100365048C CN100365048C CNB031361129A CN03136112A CN100365048C CN 100365048 C CN100365048 C CN 100365048C CN B031361129 A CNB031361129 A CN B031361129A CN 03136112 A CN03136112 A CN 03136112A CN 100365048 C CN100365048 C CN 100365048C
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Abstract
The present invention relates to a resin composition with high dielectric constant, which comprises (a) epoxy resin, (b) hardener, (c) ceramic powder and (d) modification resin with high polar group. The present invention also relates to a method for manufacturing a printed circuit board, which comprises that the composition of the present invention is used in capacitance material embedded in the printed circuit board.
Description
Technical Field
The present invention relates to a resin composition having a high dielectric constant and use thereof.
Prior Art
With the development of technology, various electronic products are not developed towards the trend of light, thin, short, small and high functionality, but due to the increasing number of various passive components on the printed circuit board, especially the passive components of Surface Mount Devices (SMDs) such as resistors, capacitors and inductors, even if the size of hundreds of passive components is continuously reduced, the passive components still occupy a large area on the printed circuit board, thereby hindering the development of miniaturization. In order to improve the defect, the passive components are thinned and then built in the circuit board, thereby effectively reducing the area by 10 to 20 times and improving the reliability because of reducing the welding points.
There have been many studies on the embedded capacitors on printed circuit boards in the past, and for example, taiwan patent publication No. 203677 describes a method of manufacturing an internal capacitor using two conductive foils and an interposed dielectric layer and applying heat and pressure treatment to make it a circuit board, but it does not mention what kind of material can be used as the dielectric layer. In addition, the conductor on the dielectric layer needs to be etched to form a circuit pattern and then laminated on a multilayer board, so the manufacturing process wastes wiring area and is not suitable for build up technology (build up) for manufacturing a multilayer printed circuit board with low line width, line spacing and blind buried holes.
In response to the demand of future high-density package, a new technology is developed to embed capacitors in the substrate to increase the package density and save the wiring area. In the case of embedded capacitor materials, the current general technique is to use highly electrically-attractive ceramic powders (ferro-electrically-ceramic powders), such as barium titanate (BaTiO) 3 ) With lead titanate (PbTiO) 3 ) And the like, or the dielectric material is mixed into an insulating material such as epoxy resin to form a dielectric material, or the dielectric material is soaked into glass fiber cloth to form a film (prepreg) to be applied to the manufacture of the built-in capacitor layer of the multilayer printed circuit board. For example, U.S. Pat. No. 5,796,587 discloses a device for applying electricityThe method for embedding in built-up circuit board uses the mixture of barium titanate powder and epoxy resin whose material weight percentage is 85%, and said material is coated on the conductor layer of pre-drilled hole, then the above-mentioned materials are stacked and pressed together so as to obtain the invented circuit board with built-in capacitor. United states patentU.S. Pat. No. 5,162,977 discloses a process for manufacturing and assembling a printed circuit board containing a high capacitance energy distribution core layer (core), wherein the high dielectric constant material is made by impregnating glass fiber cloth with a glue solution formed by epoxy resin and strong-electrostatic ceramic powder.
The two U.S. patents utilize varying types, loading and particle size of ceramic powders to affect the dielectric constant. However, this method has a limitation that a strongly electrically attractive ceramic powder such as barium titanate (BaTiO) 3 ) Or blends or dopants thereof, after co-firing at high temperatures (about 1300 c) or low temperatures (about 750 c), the resulting perovskite lattice structure has a high dielectric constant. However, the processing temperature of the printed circuit board is not higher than 250 ℃ (which is much lower than the low-temperature co-firing temperature), and at this temperature, the ferroelectric ceramic powder cannot form a lattice with a high dielectric constant. Therefore, the dielectric constant of the embedded capacitor material on the printed circuit board is not high.
In addition, although the effect of increasing the dielectric constant by increasing the filling amount of the ceramic powder is obtained, the filling amount is easily limited, and too high filling amount will make the material brittle and easily broken, and is not suitable for the manufacturing process of printed circuit board.
U.S. Pat. No. 5,800,575 discloses filling an insulating material with nanopowders (nanopowders) to increase the dielectric constant. Although the nano powder can increase the filling density and thus increase the dielectric constant, the nano powder is not easy to process, and the increase of the specific surface area causes the viscosity of the glue solution to increase, which makes the filling difficult, and the filling amount is greatly reduced, which causes difficulty in the manufacturing process.
In addition, it is known that a high dielectric constant can be obtained by adding a ceramic powder to a polymer material, but satisfactory results cannot be obtained because problems such as a high powder filling technique, control of rheological properties of a rubber material, and temperature and humidity dependence of a material have to be solved.
The general mixing procedure can be represented by the following mixing rule, which is represented by formula (1):
wherein v represents a volume fraction and k represents a dielectric constant;
when n = -1 table serial mixing rule;
n =1 table parallel mixing rule (parallel mixing rule);
n =0 table logarithmic mixing rule, also known as the lickeneker equation.
The mixing rule adopted in the capacitor material embedded in the printed circuit board is a logarithmic mixing rule, and when the mixture is simplified into two kinds, namely ceramic powder (powder) and resin substrate (matrix), the formula (1) can be derived into the formula (2):
logK＝V p logK p +V m logK m (2)
wherein, V p And V m Volume fractions, K, of the ceramic powder and the resin base material, respectively p And K m The dielectric constants of the ceramic powder and the resin substrate, respectively.
The dielectric constant of a general epoxy resin is not high, and the volume fraction (V) of a ceramic powder is generally used p ) The upper limit is 50% or 60%, and the dielectric constant (K) of the ceramic powder p ) The dielectric constant of the capacitor material cannot be increased because the processing temperature is not high enough. Therefore, if the dielectric constant of the resin can be increased, the overall dielectric constant can be effectively increased and the capacitance can be increased.
The inventor of the present invention has found that the dielectric constant (K) of a resin substrate can be effectively increased by adding a high-polarity modifier to a capacitor material m ) Thereby meeting the requirement of high dielectric constant of the whole capacitor material and overcoming the defects of the prior art of the embedded capacitor material.
Disclosure of Invention
The object of the present invention is to provide a composition comprising (a) an epoxy resin; (b) a hardener; (c) a ceramic powder; and (d) a high polarity modifier. The composition has the characteristic of high dielectric constant, and is suitable for capacitor materials embedded in printed circuit boards.
The epoxy resin is present in the composition of the invention in an amount of from 5 to 20wt%, preferably from 7 to 15wt%, based on the total weight of the composition. The epoxy resin that can be used in the composition of the present invention is not particularly limited, and may be a liquid epoxy resin or a solid epoxy resin, or a mixture thereof. In general, suitable epoxy resins have an epoxy equivalent weight of from 50 to 800 (g/eq), preferably from 130 to 500 (g/eq). Epoxy resins useful in the present invention include, but are not limited to, bisphenol A epoxy resins (bisphenol A epoxy), such as those available under the trade names EPON 828 (Shell petrochemistry), EPON 1001 (Shell petrochemistry), and DER 331 (Dow chemical); tetrabromobisphenol a type epoxy resin (tetrabromobisphenol a epoxy), such as trade name DIC 153 (big japanese ink) and DIC 152 (big japanese ink), and the like; bisphenol F type epoxy resins (bisphenol F epoxy) such as EPON 862 (shell petrochemical) and the like; a methylphenol type epoxy resin such as NPCN-703 and NPCN-704 (south Asia plastics); novolac type epoxy resins such as NPPN-638 (south asian plastics) and the like; multi-functional epoxy resins such as EPPN 501 (japanese chemical) and EPPN 502H (japanese chemical); and dicyclopentadiene type epoxy resins such as those sold under the trade names XD-1000 2L (Japan chemical) and HP-7200L (Dajapan ink); and mixtures thereof, preferably bisphenol A type epoxy resins.
The amount of hardener in the composition of the invention is from 0.1 to 15wt%, preferably from 7 to 12wt%, based on the total weight of the composition. The hardener which can be used in the composition of the present invention is a latent hardener (latent curing agent) selected from the group consisting of acid anhydride compounds, phenolic resins containing two or more functional groups, aromatic diamines, and epoxy resins, and these hardeners may be used alone or in combination.
Examples of the acid anhydride compound used in the present invention include, but are not limited to, hexahydrophthalic anhydride (hexahydrophthalic anhydride), methylhexahydrophthalic anhydride (methylhexahydrophthalic anhydride), and maleic anhydride (maleic anhydride), and these acid anhydride compounds may be used alone or in combination.
The phenolic resin containing two or more functional groups used in the present invention has a hydroxyl group equivalent of 50 to 500 (g/eq), preferably 100 to 300 (g/eq). Examples thereof include, but are not limited to, meta-methyl phenol resin (cresol novolak resin), such as trade names TD-2093 and TD-2090 (Japanese Dacron ink), and the like; polyfunctional phenol resins such as MEH-7500 (Minam and Chemicals), etc.; dicyclopentadiene type phenol resins such as those sold under the tradenames DPP-M and DPP-L (Nippon petrochemistry), etc.; and mixtures thereof.
Examples of the latent hardener for epoxy resins used in the present invention include, but are not limited to, dicyanodiamide (DICY), boron trifluoride monoethylamine complex (BF) 3 MEA), imidazole (imidazole) and derivatives thereof, triphenyl phosphite (TPP), copper (II) acetoacetate (copper (II), dimethylaniline (N' -dimethyl benzamine, BDMA), 1,8-diazabicyclo- (5, 4, 0) -undec-7-ene (DBU), and salts thereof, and mixtures thereof.
The ceramic powder is present in the composition of the invention in an amount of 60 to 85wt%, preferably 64 to 74wt%, based on the total weight of the composition. Ceramic powders useful in the compositions of the present invention generally have a powder particle size of between 0.05 μm and 20 μm, preferably between 0.1 μm and 10 μm; the ceramic powder may be any known to those skilled in the art, and may be, for example, aluminum hydroxide, metalAn oxide, or a mixture thereof. The metal oxide used in the present invention includes, but is not limited to, barium titanate (BaTiO) 3 ) Lead titanate (PbTiO) 3 ) Titanium oxide (TiO) 2 ) Aluminum oxide (Al) 2 O 3 ) Lead oxide (PbO), and mixtures thereof. Such as the trade name BT-4 (Nippon)Chemical), XJ4000 (Ferro), YL12000 (Ferro), TAMTRONY5V183U (TAM Ceramic), etc.
The highly polar modifier is present in the composition of the invention in an amount of from 1 to 10wt%, preferably from 1 to 5wt%, based on the total weight of the composition. The highly polar modifier which may be used in the composition of the present invention means a monomer, oligomer, or polymer having an amine group (NH 2-) or a cyano group (CN-) in the main chain or side chain. Non-limiting examples thereof are Cyano resins (Cyano Resin) such as those under the trade name CR-S (Beacon chemical), N-methyl acetate (N-methyl acetate), or acrylonitrile acrylate (Acrylic nitrile), and the like. Wherein, the content of the amino group is 5 to 30wt percent, preferably 7 to 20wt percent based on the total weight of the high polarity modifier; the cyano group content is 1 to 40wt%, preferably 5 to 20wt%, based on the total weight of the highly polar modifier.
The compositions of the present invention may optionally contain additives known to those skilled in the art, such as accelerators, defoamers, fillers, dispersants, coupling agents, and organic solvents, among others.
The filler used in the present invention is a conductive or non-conductive inorganic, metal or resin powder, and such filler is also helpful to increase the dielectric constant of the capacitor material.
The solvents used in the present invention are well known to those skilled in the art, such as acetone, methyl ethyl ketone, dimethyl amide, xylene, and methoxy propanol. The amount of solvent in the composition of the invention is generally from 3 to 15% by weight, based on the total weight of the composition.
The invention also relates to a method for manufacturing a printed circuit board, which comprises using the composition of the invention in a capacitor material embedded in the printed circuit board. The composition of the invention can not only avoid the problem of material brittleness caused by increasing the filling amount of ceramic powder for improving the dielectric constant in the process of preparing the printed circuit board, but also obtain the printed circuit board with a capacitor embedded with high dielectric constant.
The following examples are intended to illustrate the present invention but not to limit the scope of the invention, and any modifications and variations that can be made by one skilled in the art without departing from the spirit of the invention are intended to be included within the scope of the invention.
Detailed description of the preferred embodiments
Table 1 shows the formulation composition of the examples, wherein formulation 1 is a control formulation without the addition of high polarity modifier and ceramic powder, and formulations 2 to 6 are formulations with different proportions of high polarity modifier. The formulas 8 to 12 are added with ceramic powder and high-polarity modifier in different proportions.
Table 1: prescription composition table
| Bisphenol A type epoxy Resin (EPON) 828) | Hardening agent (Methylhexahydrobenzene) Phthalic anhydride) | Hardener II Methylaniline) | High polarity modification Agents (Cyanotrey) Fat [ CR-S ] | Solvent(s) (dimethyl) Amides) | Ceramic powder (barium titanate) 【XJ-4000】) | |
| Formulation 1 | 20 | 20 | 0.06 | ～ | ～ | ～ |
| Formulation 2 | 20 | 20 | 0.06 | 2 | 6 | ～ |
| Formulation 3 | 20 | 20 | 0.06 | 4 | 12 | ～ |
| Formulation 4 | 20 | 20 | 0.06 | 6 | 18 | ～ |
| Formulation 5 | 20 | 20 | 0.06 | 8 | 24 | ～ |
| Formulation 6 | 20 | 20 | 0.06 | 12 | 36 | ～ |
| Formulation 7 | 20 | 20 | 0.06 | ～ | ～ | 120 |
| Formulation 8 | 20 | 20 | 0.06 | 2 | 6 | 126 |
| Formulation 9 | 20 | 20 | 0.06 | 4 | 12 | 132 |
| Formulation 10 | 20 | 20 | 0.06 | 6 | 18 | 138 |
| Formulation 11 | 20 | 20 | 0.06 | 8 | 24 | 144 |
| Formulation 12 | 20 | 20 | 0.06 | 12 | 36 | 156 |
Unit: keke (Chinese character of 'Keke')
The experimental steps are as follows:
1. the preparation method comprises the steps of adding the epoxy resin, the hardener, the high-polarity modifier, the ceramic powder and the solvent which are metered into a container with a stirrer, stirring and dissolving at room temperature, adding the latent hardener of the epoxy resin, stirring uniformly, mixing and dispersing by using three rollers, standing and defoaming to obtain the resin composition (the composition is shown in table 1).
2. The front side of a polyethylene terephthalate (PET) carrier film was placed on a coater table with its front side facing upward, and the doctor blade was adjusted so that the thickness of the resin composition obtained in step 1 was 60 μm. The carrier film coated with the resin composition was baked in an oven at 140 ℃ for 10 minutes for the purpose of removing the solvent and half-curing the resin (B-stage), and the thickness of the dry film was 40 μm.
3. The half-cured resin on the PET film was peeled off, ground in a mortar, and then pressed into a sheet with a thickness of about 1mm by a mold. The test piece was placed in an oven at 150 ℃ and heat-cured for 1 hour.
4. The thickness of the cooled test piece is measured, and then the test piece is placed in a vacuum gold plating machine to plate gold on the surface, and then the dielectric constants (D) under high and low frequencies are measured respectively by using HP-4291B and 4338LCR scores k ) And dissipation factor (D) f )。
5. The results of the experiment are shown in table 2.
Table 2: test results
| D K (1GHz) | D K (100MHz) | D K (1MHz) | D f (1GHz) | D f (100MHz) | D f (1MHz) | |
| Formulation 1 | 2.7826 | 2.8245 | 3.2822 | 0.0701 | 0.0209 | 0.0289 |
| Formulation 2 | 3.4139 | 3.6399 | 4.2695 | 0.03681 | 0.02216 | 0.0346 |
| Formulation 3 | 3.7558 | 4.1737 | 5.2014 | 0.05721 | 0.04006 | 0.0420 |
| Formulation 4 | 4.0546 | 4.6595 | 5.7732 | 0.07333 | 0.05932 | 0.0478 |
| Formulation 5 | 4.1046 | 4.7627 | 6.4409 | 0.07495 | 0.06289 | 0.0502 |
| Formulation 6 | 5.5727 | 7.3959 | 8.7241 | 0.15367 | 0.10666 | 0.0546 |
| Formulation 7 | 15.5370 | 15.5850 | 15.5241 | 0.01725 | 0.01199 | 0.0290 |
| Formulation 8 | 18.9520 | 20.7990 | 21.6720 | 0.06164 | 0.04213 | 0.0387 |
| Formulation 9 | 20.5650 | 21.8020 | 24.5740 | 0.07870 | 0.05446 | 0.0531 |
| Formulation 10 | 23.4980 | 28.4220 | 31.2103 | 0.13348 | 0.09296 | 0.0780 |
| Formulation 11 | 27.7800 | 31.3150 | 33.9722 | 0.09345 | 0.07476 | 0.0853 |
| Formulation 12 | 31.2900 | 35.4200 | 38.0705 | 0.09261 | 0.07848 | 0.0976 |
And (4) conclusion:
1. from the comparison of the test results of formula 1 and formula 7, the capacitor material with the ceramic powder added can have a higher dielectric constant, and the dielectric constant of the material can be increased by the ceramic powder.
2. From the comparison of the test results of formula 1 and formulas 2 to 6, the dielectric constant of the capacitor material after the addition of the cyanoresin is slightly increased, and it is known that the high polarity modifier can increase the dielectric constant of the capacitor material, but the effect is limited.
3. By comparing the test results of the formulations 2 to 6 with those of the formulations 8 to 12, the dielectric constant of the capacitor material can be greatly improved by adding the ceramic powder and the high-polarity modifier at the same time, and the capacitor material with high dielectric constant can be obtained by adding the ceramic powder and the high-polarity modifier at the same time. The following claims should be studied to determine the true scope of the invention. It should be understood that various obvious modifications can be made by those skilled in the art based on the disclosure of the present invention, and the reasonable scope of the invention should be determined.
Claims (18)
1. A high dielectric constant capacitor material composition for printed circuit board embedding comprising:
(a) 5-20wt% of epoxy resin with epoxy equivalent of 50-800 (g/eq);
(b) 0.1-15wt% of a hardener;
(c) 60-85wt% of ceramic powder having a particle size of 0.05-20 (μm);
(d) 1-10wt% of high polarity modifier, wherein the high polarity modifier is on main chain or side chain
A cyano group containing monomer, or a polymer, or a mixture thereof.
2. The composition of claim 1, wherein the epoxy resin is a liquid epoxy resin or a solid epoxy resin or a mixture thereof.
3. The composition of claim 1, wherein the epoxy resin is selected from the group consisting of bisphenol a type epoxy resins, tetrabromobisphenol a type epoxy resins, bisphenol F type epoxy resins, methyl novolac type epoxy resins, multifunctional epoxy resins, and dicyclopentadiene type epoxy resins, and mixtures thereof.
4. The composition of claim 1, wherein the epoxy resin has an epoxy equivalent weight of between 130 to 500 (g/eq).
5. The composition of claim 1, wherein the hardener is a latent hardener selected from the group consisting of anhydride compounds, phenolic resins containing two or more functional groups, aromatic diamines, epoxy resins, and mixtures thereof.
6. The composition of claim 5, wherein the anhydride compound is selected from the group consisting of hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, and maleic anhydride, and mixtures thereof.
7. The composition of claim 5, wherein the phenolic resin with two or more functional groups has a hydroxyl equivalent weight of between 50 and 500 (g/eq).
8. The composition of claim 7, wherein the phenolic resin with two or more functional groups has a hydroxyl equivalent weight of between 100 and 300 (g/eq).
9. The composition of claim 5, wherein the phenolic resin containing two or more functional groups is selected from meta-methyl phenolic resin, multifunctional phenolic resin, and dicyclopentadiene type phenolic resin, and mixtures thereof.
10. The composition of claim 5, wherein the latent hardener of the epoxy resin is selected from dicyanodiamide, boron trifluoride monoethylamine complex, imidazole and its derivatives, triphenyl phosphite, copper (II) acetoacetate, dimethylaniline, 1,8-diazabicyclo- (5, 4, 0) -undec-7-ene and its salts, and mixtures thereof.
11. The composition of claim 1, wherein the ceramic powder has a powder particle size of 0.1 μ ι η to 10 μ ι η.
12. The composition of claim 1, wherein the ceramic powder is selected from the group consisting of barium titanate, lead titanate, titanium oxide, lead oxide, and mixtures thereof.
13. The composition of claim 1, wherein the cyano group is present in an amount of 1 to 40 wt.%, based on the total weight of the highly polar modifier.
14. The composition of claim 13, wherein the cyano group is present in an amount of 5 to 20 wt.%, based on the total weight of the highly polar modifier.
15. The composition of claim 1, further comprising an additive.
16. The composition of claim 1, wherein the additive is selected from the group consisting of accelerators, defoamers, fillers, dispersants, coupling agents, and organic solvents, and mixtures thereof.
17. The composition of claim 16, wherein the organic solvent is selected from the group consisting of acetone, methyl ethyl ketone, dimethyl formamide, xylene, and methoxypropanol, and mixtures thereof.
18. A method of manufacturing a printed circuit board comprising using the composition of any one of claims 1 to 17 in a capacitive material embedded on a printed circuit board.
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| CN101760112B (en) * | 2010-03-01 | 2011-10-05 | *** | Low-carbon paint |
| CN103374205A (en) * | 2012-04-26 | 2013-10-30 | 富葵精密组件(深圳)有限公司 | Epoxy resin composite material and preparation method thereof |
| CN103101252B (en) * | 2013-01-23 | 2016-04-13 | 陕西生益科技有限公司 | The preparation method of a kind of high-k, low-loss CEM-3 copper-clad plate |
| CN105693141B (en) * | 2014-08-29 | 2017-08-04 | 天津德高化成新材料股份有限公司 | A kind of preparation method of dielectric composite material for fingerprint sensor inductive layer |
| CN104403262B (en) * | 2014-11-06 | 2016-09-07 | 上海复合材料科技有限公司 | A kind of high-dielectric and low-loss phenolic glass fiber composite and preparation method thereof |
| CN106995584B (en) * | 2016-10-27 | 2019-08-23 | 武汉市三选科技有限公司 | The preparation and packaging method of capactive film constituent and capactive film and the capactive film |
| CN107344993B (en) * | 2017-06-14 | 2018-09-11 | 建滔(番禺南沙)石化有限公司 | A kind of preparation method of antiultraviolet epoxy resin and the product of acquisition |
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|---|---|---|---|---|
| JPH04341711A (en) * | 1991-05-17 | 1992-11-27 | Meidensha Corp | Epoxy resin molding |
| JPH06172618A (en) * | 1992-12-10 | 1994-06-21 | Denki Kagaku Kogyo Kk | Epoxy resin composition and printed board |
| JPH06283343A (en) * | 1993-03-25 | 1994-10-07 | Hitachi Ltd | Manufacture of flyback transformer |
| JP2604197B2 (en) * | 1988-04-02 | 1997-04-30 | 新日本理化株式会社 | Liquid epoxy resin composition |
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2003
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2604197B2 (en) * | 1988-04-02 | 1997-04-30 | 新日本理化株式会社 | Liquid epoxy resin composition |
| JPH04341711A (en) * | 1991-05-17 | 1992-11-27 | Meidensha Corp | Epoxy resin molding |
| JPH06172618A (en) * | 1992-12-10 | 1994-06-21 | Denki Kagaku Kogyo Kk | Epoxy resin composition and printed board |
| JPH06283343A (en) * | 1993-03-25 | 1994-10-07 | Hitachi Ltd | Manufacture of flyback transformer |
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