CN105001582A - Preparation method of low dielectric constant substrate - Google Patents
Preparation method of low dielectric constant substrate Download PDFInfo
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- CN105001582A CN105001582A CN201510543468.XA CN201510543468A CN105001582A CN 105001582 A CN105001582 A CN 105001582A CN 201510543468 A CN201510543468 A CN 201510543468A CN 105001582 A CN105001582 A CN 105001582A
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Abstract
The invention relates to a preparation method of a low dielectric constant substrate. The preparation method comprises the following steps of taking a silica solution, nano hollow aluminum oxide, lauryl sodium sulfate, lauryl alcohol, oleic acid, sodium persulfate and methyl methacrylate as raw materials to obtain a filler; taking monomers of adjacent armour phenolic epoxy resin and cyanate ester resin, lauric acid polyoxyethylene ether, N-methylol acrylamide as raw materials to obtain a resin prepolymer; sequentially adding benzimidazole and the filler into the resin prepolymer, and stirring for two hours at the temperature of 120 DEG C; then adding phenoxy resin for continuously stirring for 2 hours; then adding polyetherimide; then stirring for two hours at the temperature of 150 DEG C; obtaining a compound system; placing the compound system into a die preheated to 150 DEG C, and hot pressing to obtain the low dielectric constant substrate. The low dielectric constant substrate has excellent mechanical property and heat resisting property, and the development and application of the low dielectric constant substrate can be met.
Description
Technical field
The invention belongs to advanced composite material technical field, be specifically related to a kind of preparation method of low dielectric constant base board, the product obtained can be used for electronic applications.
Background technology
Specific inductivity determines the speed that electrical signal is propagated in the medium.Speed and the specific inductivity square root of propagation of electrical signals are inversely proportional to.Specific inductivity is lower, and signal velocity is faster.Specific inductivity is not be very easy to measure or definition, and it is not only relevant with the self character of medium, goes back and testing method, test frequency, and the materials behavior before test and in test is relevant.Specific inductivity also can variation with temperature and changing, some special material factor just considering temperature under development.Humidity is also the important factor affecting specific inductivity, because the specific inductivity of water is 70, little moisture, can cause significant change.
All kinds of consumer electronics with high speed information processing capacity of the develop rapidly of information technology has now been indispensable key component in daily life.The cableless communication of military domain application and wide frequency technology are also rapidly to the transfer of civilian consumer electronics field.The continuous progress of telecommunications product has impelled the integrated level of product component to increase, and shows as PCB to future developments such as high-density, multi-functional, environmental protection; The simultaneously microminiaturization of the device also boosting progress of electronic product.For PCBA package technique, 3D assembling, high density interconnect, green assembling, high reliability assembling, assembling reinforcing etc. will become more and more important.
For high speed, frequency applications, optimal material is the air dielectric wrapped up by Copper Foil.As developing material, everybody is towards this direction effort, as Foamclad is applicable to the application of antenna for base station very much.Specific inductivity, except directly affecting the transmission speed of signal, also determines natural impedance to a great extent, in distinct portions, natural impedance is mated particularly important in micro-wave communication.
To material, particularly to the level of understanding of high performance material, grasp and application power, directly embody scientific and technological level and the economic strength of country.Matrix material is type material, because of its proof voltage, lightweight, can design, diversified function and the outstanding performance such as high temperature resistant, folding, be used widely in fields such as the Aeronautics and Astronautics over nearly 30 years, the energy, traffic, machinery, building, chemical industry, biomedicine and physical culture, 21 century Material Field opened one's arms and met the arrival in matrix material epoch.Along with matrix material development and application, matrix material has been formed in the middle of network penetration to industry-by-industry field.
Summary of the invention
The object of this invention is to provide a kind of preparation method of low dielectric constant base board, the low dielectric constant base board of preparation has low specific inductivity, can be used as electronic circuit materials, electrical insulating material application.
To achieve the above object of the invention, the technical solution used in the present invention is: a kind of preparation method of low dielectric constant base board, comprises the following steps:
(1) by mass concentration be 45% silicon sol, nano-hollow aluminum oxide mix with sodium lauryl sulphate, lauryl alcohol, oleic acid; 70 DEG C to be stirred after 15 minutes ultrasonic disperse 2 hours; Then add Sodium Persulfate, stir 20 minutes; Drip methyl methacrylate again, 80 DEG C are stirred 2 hours; Filler is obtained after drying;
(2) mix o-cresol formaldehyde epoxy resin and cyanate resin alicyclic monomer, 90 DEG C of stirrings added lauric acid Soxylat A 25-7 after 15 minutes, continued stirring 10 minutes; Then add N hydroxymethyl acrylamide, stir 15 minutes in 100 DEG C; Obtain resin prepolymer;
(3) successively benzoglyoxaline, filler are added in resin prepolymer, stir 2 hours in 120 DEG C; Then add phenoxy resin and continue stirring 2 hours; Then polyetherimide is added; Then stir 2 hours in 150 DEG C; Obtain compound system;
(4) inserted by compound system in the mould of 150 DEG C of preheatings, namely hot pressing obtain low dielectric constant base board.
In the present invention, in step (1), the mass ratio of described silicon sol, nano-hollow aluminum oxide, sodium lauryl sulphate, lauryl alcohol, oleic acid, Sodium Persulfate, methyl methacrylate is 1: 0.4: 0.1: 0.05: 0.3: 0.01: 0.4; The median size of described filler is 130nm.
In the present invention, in step (2), the mass ratio of o-cresol formaldehyde epoxy resin, cyanate resin alicyclic monomer, lauric acid Soxylat A 25-7, N hydroxymethyl acrylamide is 1: 1.4 ~ 1.6: 0.05 ~ 0.08: 0.14 ~ 0.18.
In the present invention, in step (3), the mass ratio of benzoglyoxaline, filler, resin prepolymer, phenoxy resin, polyetherimide is 0.06: 0.22 ~ 0.25: 1: 0.15: 0.1 ~ 0.12.
In the present invention, in step (4), heat pressing process is: 1MPa/150 DEG C/0.5 hour+1.5MPa/170 DEG C/2 hours+5MPa/200 DEG C/2 hours+5MPa/220 DEG C/2 hours.
In the present invention, organic object is the primary bond composition of resin base compound system, and the Nano filling of rigidity can be evenly dispersed in resin, improves intensity and the thermal level of its cured article; Present invention, avoiding especially between compound interface and occur hole, the formation of polymer interpenetration network can not be hindered, ensure the intensity of solidification composition board.For organic-inorganic dielectric materials, the dispersion of inorganic particulate is extremely important for obtaining compared with the matrix material of low-k; The matrix material that prior art uses the preparation of coupling agent treatment inorganic particulate better dispersed, but coupling agent can reduce thermotolerance and dielectric properties, the mechanical property of system, even can affect the solidification of organic materials, the cyanate to condition of cure sensitivity can be disturbed especially; The present invention, without the need to coupling agent, can improve the consistency between organism and inorganic particulate by compatibility organic system, is conducive to inorganic particulate dispersed better in polymeric matrix, thus improves the over-all properties of mixture.
In addition, in mixture disclosed by the invention, reactive group content is high, viscosity is little, so it is higher to participate in the transformation efficiency of polyreaction, what obtain after solidification is crosslinking polymer network, simultaneously due to the existence of filler and micromolecular compound, the spinability of intermolecular segment is better, product good mechanical property.Affect immanent cause mainly high-polymer molecular polarity size and the polar groups density of dielectric material performance.The transformation efficiency that the transfer being added with proton along with epoxide group, amine groups, lauric acid Soxylat A 25-7 facilitates ring-closure reaction increase cyanate functional group significantly improves; In hot pressing, when cyanate functional group conversions leads higher, reaction system mobility is deteriorated, and reacts and is controlled by diffusion process; The diffusion of lauric acid Soxylat A 25-7 in system is more easy, the cyanate group making the polarity that remains larger, epoxide group obtain reacting more fully, be more prone to generate a kind of high degree of symmetry, the cross-linked network structure of height steric hindrance, thus the dielectric properties of whole system are greatly improved.
In the present invention, by acid anhydrides, epoxy/cyanate ester resin, phenoxy resin and polyetherimide resin are combinationally used, the polymer body of excellent in mechanical performance, Good Heat-resistance can be obtained.By adding small molecules, the even density of filler in system, can obtain good mix, becomes the paste-like being easily prepared into and having mobility; Be conducive to polymer polymerization, increase the cross-linking set in system solidification process, obtain interpenetrating polymer structure, ensure the intensity of low dielectric constant base board.
Because technique scheme is used, the present invention compared with prior art has following advantages:
Rationally, between each component, consistency is good, has prepared low dielectric constant base board thus, has good mechanical property, resistance toheat, meets the development and application of low dielectric constant base board for the material system composition that the present invention utilizes.The advantage of comprehensive polymkeric substance, inorganic particulate two component, improves the shortcoming of two components, thus improves the over-all properties obtaining material; Solidification effect is good, crosslinking structure is even, micromolecular compound can as the compatilizer of macromolecule organic, increase the consistency of each component of system on the one hand, avoid on the other hand during hot-press solidifying, forming crosslinked uneven defect, ensure that resin system forms stable structure, mechanical property is strong, achieves beyond thought effect.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
The present embodiment is raw materials used is all commercial, belongs to industrial goods; The molecular weight of wherein said phenoxy resin is 0.8 ~ 1.2 ten thousand; The molecular weight of described polyetherimide resin is 1.1 ~ 1.5 ten thousand.
The preparation method of embodiment one one kinds of low dielectric constant base boards, comprises the following steps:
(1) by 1Kg mass concentration be 45% silicon sol, 400g nano-hollow aluminum oxide mix with 100g sodium lauryl sulphate, 50g lauryl alcohol, 300g oleic acid; 70 DEG C to be stirred after 15 minutes ultrasonic disperse 2 hours; Then add 10g Sodium Persulfate, stir 20 minutes; Drip 400g methyl methacrylate again, 80 DEG C are stirred 2 hours; The filler that median size is 130 nanometers is obtained after dry;
(2) mix 100g o-cresol formaldehyde epoxy resin and 140g cyanate resin alicyclic monomer, 90 DEG C of stirrings added 8g lauric acid Soxylat A 25-7 after 15 minutes, continued stirring 10 minutes; Then add 18gN-n-methylolacrylamide, stir 15 minutes in 100 DEG C; Obtain resin prepolymer;
(3) successively 6g benzoglyoxaline, 22g filler are added in 100g resin prepolymer, stir 2 hours in 120 DEG C; Then add 15g phenoxy resin and continue stirring 2 hours; Then 10g polyetherimide is added; Then stir 2 hours in 150 DEG C; Obtain compound system;
(4) inserted by compound system in the mould of 150 DEG C of preheatings, namely hot pressing obtain low dielectric constant base board; Heat pressing process is: 1MPa/150 DEG C/0.5 hour+1.5MPa/170 DEG C/2 hours+5MPa/200 DEG C/2 hours+5MPa/220 DEG C/2 hours.
The preparation method of embodiment 21 kinds of low dielectric constant base boards, comprises the following steps:
(1) by 1Kg mass concentration be 45% silicon sol, 400g nano-hollow aluminum oxide mix with 100g sodium lauryl sulphate, 50g lauryl alcohol, 300g oleic acid; 70 DEG C to be stirred after 15 minutes ultrasonic disperse 2 hours; Then add 10g Sodium Persulfate, stir 20 minutes; Drip 400g methyl methacrylate again, 80 DEG C are stirred 2 hours; The filler that median size is 130 nanometers is obtained after dry;
(2) mix 100g o-cresol formaldehyde epoxy resin and 160g cyanate resin alicyclic monomer, 90 DEG C of stirrings added 5g lauric acid Soxylat A 25-7 after 15 minutes, continued stirring 10 minutes; Then add 14gN-n-methylolacrylamide, stir 15 minutes in 100 DEG C; Obtain resin prepolymer;
(3) successively 6g benzoglyoxaline, 25g filler are added in 100g resin prepolymer, stir 2 hours in 120 DEG C; Then add 15g phenoxy resin and continue stirring 2 hours; Then 12g polyetherimide is added; Then stir 2 hours in 150 DEG C; Obtain compound system;
(4) inserted by compound system in the mould of 150 DEG C of preheatings, namely hot pressing obtain low dielectric constant base board; Heat pressing process is: 1MPa/150 DEG C/0.5 hour+1.5MPa/170 DEG C/2 hours+5MPa/200 DEG C/2 hours+5MPa/220 DEG C/2 hours.
The preparation method of embodiment 31 kinds of low dielectric constant base boards, comprises the following steps:
(1) by 1Kg mass concentration be 45% silicon sol, 400g nano-hollow aluminum oxide mix with 100g sodium lauryl sulphate, 50g lauryl alcohol, 300g oleic acid; 70 DEG C to be stirred after 15 minutes ultrasonic disperse 2 hours; Then add 10g Sodium Persulfate, stir 20 minutes; Drip 400g methyl methacrylate again, 80 DEG C are stirred 2 hours; The filler that median size is 130 nanometers is obtained after dry;
(2) mix 100g o-cresol formaldehyde epoxy resin and 150g cyanate resin alicyclic monomer, 90 DEG C of stirrings added 7g lauric acid Soxylat A 25-7 after 15 minutes, continued stirring 10 minutes; Then add 16gN-n-methylolacrylamide, stir 15 minutes in 100 DEG C; Obtain resin prepolymer;
(3) successively 6g benzoglyoxaline, 24g filler are added in 100g resin prepolymer, stir 2 hours in 120 DEG C; Then add 15g phenoxy resin and continue stirring 2 hours; Then 11g polyetherimide is added; Then stir 2 hours in 150 DEG C; Obtain compound system;
(4) inserted by compound system in the mould of 150 DEG C of preheatings, namely hot pressing obtain low dielectric constant base board; Heat pressing process is: 1MPa/150 DEG C/0.5 hour+1.5MPa/170 DEG C/2 hours+5MPa/200 DEG C/2 hours+5MPa/220 DEG C/2 hours.
The preparation method of comparative example one one kinds of low dielectric constant base boards, comprises the following steps:
(1) by 1Kg mass concentration be 45% silicon sol, 400g nano-hollow aluminum oxide mix with 100g sodium lauryl sulphate, 50g lauryl alcohol, 300g oleic acid; 70 DEG C to be stirred after 15 minutes ultrasonic disperse 2 hours; Then add 10g Sodium Persulfate, stir 20 minutes; Drip 400g methyl methacrylate again, 80 DEG C are stirred 2 hours; The filler that median size is 130 nanometers is obtained after dry;
(2) mix 100g o-cresol formaldehyde epoxy resin and 150g cyanate resin alicyclic monomer, 90 DEG C are stirred after 15 minutes, stir 15 minutes in 100 DEG C; Obtain resin prepolymer;
(3) successively 6g benzoglyoxaline, 20g filler are added in 100g resin prepolymer, stir 2 hours in 120 DEG C; Then add 15g phenoxy resin and continue stirring 2 hours; Then 10g polyetherimide is added; Then stir 2 hours in 150 DEG C; Obtain compound system;
(4) inserted by compound system in the mould of 150 DEG C of preheatings, namely hot pressing obtain low dielectric constant base board; Heat pressing process is: 1MPa/150 DEG C/0.5 hour+1.5MPa/170 DEG C/2 hours+5MPa/200 DEG C/2 hours+5MPa/220 DEG C/2 hours.
The performance test results of above-mentioned low dielectric constant base board is in table 1.
The performance of table 1 low dielectric constant base board
To sum up, rationally, between each component, consistency is good for low dielectric constant base board composition disclosed by the invention, prepare low dielectric constant base board thus, there is good mechanical property, there is excellent resistance toheat especially, meet the development and application of low dielectric constant base board.
Claims (7)
1. a preparation method for low dielectric constant base board, is characterized in that, comprises the following steps:
(1) by mass concentration be 45% silicon sol, nano-hollow aluminum oxide mix with sodium lauryl sulphate, lauryl alcohol, oleic acid; 70 DEG C to be stirred after 15 minutes ultrasonic disperse 2 hours; Then add Sodium Persulfate, stir 20 minutes; Drip methyl methacrylate again, 80 DEG C are stirred 2 hours; Filler is obtained after drying;
(2) mix o-cresol formaldehyde epoxy resin and cyanate resin alicyclic monomer, 90 DEG C of stirrings added lauric acid Soxylat A 25-7 after 15 minutes, continued stirring 10 minutes; Then add N hydroxymethyl acrylamide, stir 15 minutes in 100 DEG C; Obtain resin prepolymer;
(3) successively benzoglyoxaline, filler are added in resin prepolymer, stir 2 hours in 120 DEG C; Then add phenoxy resin and continue stirring 2 hours; Then polyetherimide is added; Then stir 2 hours in 150 DEG C; Obtain compound system;
(4) inserted by compound system in the mould of 150 DEG C of preheatings, namely hot pressing obtain low dielectric constant base board.
2. the preparation method of low dielectric constant base board according to claim 1, it is characterized in that, in step (1), the mass ratio of described silicon sol, nano-hollow aluminum oxide, sodium lauryl sulphate, lauryl alcohol, oleic acid, Sodium Persulfate, methyl methacrylate is 1: 0.4: 0.1: 0.05: 0.3: 0.01: 0.4; The median size of described filler is 130nm.
3. the preparation method of low dielectric constant base board according to claim 1, it is characterized in that, in step (2), the mass ratio of o-cresol formaldehyde epoxy resin, cyanate resin alicyclic monomer, lauric acid Soxylat A 25-7, N hydroxymethyl acrylamide is 1: 1.4 ~ 1.6: 0.05 ~ 0.08: 0.14 ~ 0.18.
4. the preparation method of low dielectric constant base board according to claim 1, it is characterized in that, in step (3), the mass ratio of benzoglyoxaline, filler, resin prepolymer, phenoxy resin, polyetherimide is 0.06: 0.22 ~ 0.25: 1: 0.15: 0.1 ~ 0.12.
5. the preparation method of low dielectric constant base board according to claim 1, it is characterized in that, in step (4), heat pressing process is: 1MPa/150 DEG C/0.5 hour+1.5MPa/170 DEG C/2 hours+5MPa/200 DEG C/2 hours+5MPa/220 DEG C/2 hours.
6. the preparation method of low dielectric constant base board according to claim 1, it is characterized in that, the molecular weight of described phenoxy resin is 0.8 ~ 1.2 ten thousand; The molecular weight of described polyetherimide resin is 1.1 ~ 1.5 ten thousand.
7. the low dielectric constant base board prepared of the preparation method of any one low dielectric constant base board according to claims 1 to 6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276557A (en) * | 2018-01-10 | 2018-07-13 | 苏州益可泰电子材料有限公司 | Heat resistant resin material and preparation method thereof |
| CN108943550A (en) * | 2017-05-17 | 2018-12-07 | 台光电子材料(昆山)有限公司 | The method for manufacturing naval stores |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115600A (en) * | 2010-11-26 | 2011-07-06 | 苏州生益科技有限公司 | Thermosetting resin composition, prepreg and laminated board |
| CN104194333A (en) * | 2014-09-01 | 2014-12-10 | 黑龙江省科学院石油化学研究院 | Cyanate ester resin with low dielectric loss and preparation method thereof |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115600A (en) * | 2010-11-26 | 2011-07-06 | 苏州生益科技有限公司 | Thermosetting resin composition, prepreg and laminated board |
| CN104194333A (en) * | 2014-09-01 | 2014-12-10 | 黑龙江省科学院石油化学研究院 | Cyanate ester resin with low dielectric loss and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108943550A (en) * | 2017-05-17 | 2018-12-07 | 台光电子材料(昆山)有限公司 | The method for manufacturing naval stores |
| CN108943550B (en) * | 2017-05-17 | 2020-11-13 | 台光电子材料(昆山)有限公司 | Method for manufacturing resin product |
| CN108276557A (en) * | 2018-01-10 | 2018-07-13 | 苏州益可泰电子材料有限公司 | Heat resistant resin material and preparation method thereof |
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