CN102166854B - Intermediate-Tg lead-free compatible copper foil-covered board and preparation method thereof - Google Patents
Intermediate-Tg lead-free compatible copper foil-covered board and preparation method thereof Download PDFInfo
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- CN102166854B CN102166854B CN 201010617558 CN201010617558A CN102166854B CN 102166854 B CN102166854 B CN 102166854B CN 201010617558 CN201010617558 CN 201010617558 CN 201010617558 A CN201010617558 A CN 201010617558A CN 102166854 B CN102166854 B CN 102166854B
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Abstract
The invention discloses an intermediate-Tg epoxy glass cloth base copper foil-covered board suitable for the lead-free manufacture procedure and a preparation method thereof. The copper foil-covered board is solidified by modified polyfunctional epoxy resin, high-heat resistance modified epoxy and linear phenolic aldehyde and is added with the other auxiliary materials to properly proportion a prepared binding agent; the binding agent is covered and glued on a glass fiber cloth; and copper foil is covered to prepare the board in a hot-pressing way, so that the thickness of the board is 0.05-3.2mm, and the thickness of the copper foil is 1/3oz-5oz. The epoxy glass cloth base copper foil-covered board prepared by the method has the characteristics of being intermediate in glass transition temperature (which is more than and equal to 150 DEG C), good in heat resistance, CAF (cavitation air flotation) resistance and size stability, low in Z-CTE (thermal expansion coefficient) value and water absorption rate, and good in machinability, electrochemical resistance, flame resistance and the like, thereby being suitable for the lead-free manufacture procedure and the manufacturing and the machining of a sandwich plate in the PCB (printed circuit board) industry.
Description
Technical field
The present invention relates to electronic information technology preparation of product field, be specifically related to a kind of middle Tg lead-free compatible epoxide glass cloth base copper coated foil plate and preparation method thereof, this method can be widely used in multiple-plate production in the PCB industry.
Background technology
Society is improving now, science and technology is in development, we are more and more higher to the demand of electronic product, electronic service, light, thin, short, the little and digitized demand of electronic product, make miniaturization, multi-functional, high-performance become mainstream development direction with high-reliability, as the base material of electronic product, the demand of copper coated foil plate also inevitably strides forward towards the direction of high reliability day by day.
Electronic product is the industry of world today's maximum, and the pollution problem that huge industry like this is brought is the emphasis that people have to pay close attention to.European Union is in the formal ROHS of promulgation on July 1st, 2006 (about ban use of some harmful substance instruction in electronic and electrical equipment) and two instructions of WEEE (instructing about scrapping electronic and electrical equipment), and from then on the global electronic industry has entered the unleaded epoch.Traditional plumber's solder can not re-use, and the required welding temperature of alternative solders such as SAC now all increases substantially.The unleaded simultaneous development of high-density installation technology now of carrying out in an all-round way, especially the develop rapidly of surface mounting technology (SMT), during PCB processing is installed with the complete machine accessory, the number of times that material bears thermal shock repeatedly and temperature are all than conventional need was higher in the past, a series of combined reliabilities such as hear resistance of copper-clad plate material can all be faced with huge challenge, only rely on the copper-clad plate of traditional handicraft can't satisfy the demands, we need have a qualitative leap to comply with the development of whole industry in traditional copper-clad plate reliability.
The FR-4 product Tg (glass transition temperature) of traditional handicraft is all below 140 ℃; Z axle CTE value is about 3.9%; Hear resistance T260 is about 11 minutes, and T288 was less than 1 minute, and TD (heat decomposition temperature) is about 310 ℃.These very important performances all can't satisfy PCB produce in leadless process even the multi-layer sheet demand of producing.
FR-4; It is the code name of a kind of flame resistant material grade of copper-clad plate industry
Z axle CTE: refer to material thermal coefficient of expansion longitudinally
T260: be the thermally stratified layer time, the fingerboard material is under 260 ℃ design temperature, because time that is continued before this lamination appears, in the effect of heat.
T288: be the thermally stratified layer time, the fingerboard material is under 288 ℃ design temperature, because time that is continued before this lamination appears, in the effect of heat.
Tg: be glass transition temperature, the fingerboard material under the situation of being heated by glassy transition be the corresponding temperature of elastomeric state (rubbery state) (℃).
Td: be heat decomposition temperature, the fingerboard material under the effect of heat, produce pyrolysis temperature (℃).
Psi: be pressure unit, namely the pound/square inch
Summary of the invention
Technical problem to be solved by this invention is, overcomes problems of the prior art, and a kind of middle Tg lead-free compatible epoxide glass cloth base copper coated foil plate and preparation method thereof is provided.
Be such in order to address the above problem technical scheme of the present invention:
Middle Tg lead-free compatible epoxide glass cloth base copper coated foil plate, mainly by modification polyfunctional epoxy resin, high heat resistance modified bisphenol type epoxy, linear phenolic curing agent, and interpolation auxiliary material, the adhesive that is modulated into, adhesive applies gluing on glass fabric, be covered with Copper Foil again and prepare through hot pressing, thickness of slab is 0.05～3.2mm, and used copper thickness is 1/3oz～5oz.
The main composition of adhesive according to the quality proportioning is:
Nitrogen heterocyclic ring modification polyfunctional epoxy resin, 40～90 parts;
High heat resistance modified bisphenol type epoxy, 1～20 part;
Linear phenolic curing agent, 20～60 parts;
Imidazoles promoter, 0.05～5.0 part;
Silicon powder, i.e. SiO2 powder, average grain diameter＜8 μ m, 5～60 parts;
Silane, 0.05～5.0 part;
Butanone, 5～50 parts;
Propylene glycol monomethyl ether, 5～50 parts.
The preparation method of middle Tg lead-free compatible epoxide glass cloth base copper coated foil plate may further comprise the steps,
1) impregnation;
A) in tank diameter, add propylene glycol monomethyl ether, butanone, silane successively by formula ratio, turn on agitator, 500～1500 rev/mins of rotating speeds keep continuing stirring and control flume body temperature degree at 20～50 ℃, add silicon powder again, add the back that finishes and continue to stir 10～50 minutes;
B) in tank diameter, add nitrogen heterocyclic ring modification polyfunctional epoxy resin, high heat resistance modified bisphenol type epoxy, linear phenolic curing agent more successively by formula ratio, keep stirring with 1000～1500 rev/mins of rotating speeds in the reinforced process, open efficient shearing and emulsification 0.5～4 hour after interpolation finishes, carry out cooling water simultaneously and circulate with 20～50 ℃ again of retentive control cell body problems;
C) take by weighing imidazoles promoter by formula ratio, and the adding propylene glycol monomethyl ether, make the dissolving of imidazoles promoter fully, confirm after the no crystallization consoluet imidazoles promoter to be added in the tank diameter, and continuing to keep 1000～1500 rev/mins of stirrings 3～15 hours, impregnation is finished;
2) gluing, prepreg processed;
A) adhesive is recycled to gluing machine, through preimpregnation, main soaking, evenly is coated on adhesive on the glass fabric; The gluing machine linear velocity is controlled to be 6～28m/min;
B) glass fabric of application of adhesive toasts through 120 ℃～250 ℃ drying bakers, makes solvent evaporates, and the adhesive initial reaction solidifies, and makes prepreg;
The control of prepreg physical parameter: gelation time: 60～150 seconds, the resin quality percentage composition was 36%～75%, and the resin ratio flow is 15%～40%, volatile matter＜0.75%;
3) set type, suppress;
Prepreg is cut into same size, 1～18 one group, superimposed with Copper Foil again, compacting then.
Imidazoles promoter be methylimidazole, diethyl tetramethyl imidazoles, diphenyl-imidazole one of them.
The control of compacting parameter is as follows:
A. pressure: 100～550psi;
B. temperature: 80～220 ℃;
C. vacuum: 0.030～0.080Mpa;
D. press time: 90～150 minutes;
E. hardening time: 30～60 minutes.
Above-mentioned epoxide glass cloth base copper coated foil plate can have various types of specifications, as: 36 * 48, (units: inch) such as 36.5 * 48.5,37 * 49,40 * 48,40.5 * 48.5,41 * 49,42 * 48,42.5 * 48.5,43 * 49.
Glass fabric can be selected the E level for use, and it is 101,104,106,1078,1080,1086,2113,2313,2116,1506 or 7628 etc. all kinds of that specification can be selected for use.
Copper Foil can be selected 1/3oz, Hoz, 1oz, 2oz, 3oz, 4oz or 5oz etc. for use.
Beneficial effect, the present invention mentions this in Tg point 〉=150 ℃ of the unleaded epoxide glass cloth base copper coated foil plate of Tg; Z axle CTE≤3.5%; Hear resistance aspect TD 〉=325 ℃, T260 was above 60 minutes, T288 is more than 15 minutes, the outstanding general performance of performances such as very little water absorption rate, outstanding anti-CAF (energy of anti-the ion transport) and machining property in addition, can satisfy fully PCB produce in leadless process and the multi-layer sheet demand of producing.
The specific embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Tg lead-free compatible epoxide glass cloth base copper coated foil plate primary raw material is in the preparation:
1. nitrogen heterocyclic ring modification polyfunctional epoxy resin
Chemical composition: nitrogen heterocyclic ring modification polyfunctional epoxy resin (80%)+acetone (20%) resinous principle requires:
| Project | Specifications parameter |
| Epoxide equivalent EEW (g/eq) | 250～280 |
| Hydrolyzable chlorine (p propylene glycol monomethyl ether) | 400MAX |
| Solid (wt%) | 79～81 |
| Bromine content (wt%) | 12～18 |
| Color | Yellow |
TG after nitrogen heterocyclic ring modification polyfunctional epoxy resin solidifies 〉=150 ℃, good toughness is easy to machining, but cooperative flame retardant is good with the glass fibre impregnation, and the resin kinetic viscosity changes slow, processing temperature wide ranges, easy operating and stay in grade in the hot pressing.
2. high heat resistance modified bisphenol type epoxy
Chemical composition: high heat resistance modified bisphenol type epoxy (100%)
Resinous principle requires:
Can significantly promote the hear resistance after the material cured after high heat resistance modified bisphenol type epoxy adds by a certain percentage, performances such as Td, T260 obviously improve.
The prescription of adhesive:
| Former material | Formula rate (mass ratio) |
| Nitrogen heterocyclic ring modification polyfunctional epoxy resin | 80 |
| High heat resistance modified bisphenol type epoxy | 10 |
| Linear phenolic curing agent | 25 |
| Imidazoles promoter | 0.3 |
| Silicon powder (being the SiO2 powder, average grain diameter＜8 μ m) | 35 |
| Silane | 0.2 |
| Butanone | 15 |
| Propylene glycol monomethyl ether | 20 |
3. glass fabric, electron level, its component is:
| SiO 2 | 55.5％ | Na 2O and K 2O | 0.5％ |
| AL 2O 3 | 14.6％ | B 2O 3 | 7.2％ |
| CaO | 18.5％ | Fe 2O 3 | 0.3％ |
| MgO | 3.5％ |
Performance indications (7628-electronic-grade glass fiber cloth a kind of, 7628 is code):
4. electrolytic copper foil
Performance indications (1OZ):
| The Interventions Requested title | Unit (/ condition) | Specification requirement | Assay |
| Indicated weight | g/m2 | 290±10 | 292 |
| Ra | um | ＜0.43 | 0.26 |
| Rz | um | ＜5.1 | 4.58 |
| Peel strength | N/mm | ＞1.05 | 1.62 |
| Tensile strength | Kg/mm2 | ＞28 | 34.6 |
| Percentage elongation | ％ | ＞10 | 13 |
| Oxidisability | 200℃/0.5h | Pass | Pass |
Below with three kinds give an example to describe in detail how to prepare in Tg lead-free compatible epoxide glass cloth base copper coated foil plate.
Embodiment 1:
1. impregnation formula rate (weight share meter):
| Former material | Formula rate (mass ratio) |
| Nitrogen heterocyclic ring modification polyfunctional epoxy resin | 68 |
| High heat resistance modified bisphenol type epoxy | 8 |
| Linear phenolic curing agent | 21 |
| Methylimidazole | 0.28 |
| Silicon powder (being the SiO2 powder, average grain diameter＜8 μ m) | 32 |
| Silane | 0.3 |
| Butanone | 14 |
| Propylene glycol monomethyl ether | 23 |
2. gluing baking: prepreg gluing speed 10m/min
3. prepreg is controlled parameter: gel time 72 seconds
Resin content 45.1%
Resin flow 17.8%
Fugitive constituent 0.30%
4. sheet material composing structure: thickness 1.6mm after 8 7628 prepreg pressings
5. pressing plate parameter: vacuum-0.088MPa
Pressure 120-500psi
Temperature of heat plate 90-210 ℃
58 minutes hardening times
6. substrate performance parameter:
Embodiment 2:
1. impregnation formula rate (weight share meter):
| Former material | Formula rate (mass ratio) |
| Nitrogen heterocyclic ring modification polyfunctional epoxy resin | 75 |
| High heat resistance modified bisphenol type epoxy | 5 |
| Linear phenolic curing agent | 24 |
| Dimethyl tetraethyl imidazoles | 2.5 |
| Silicon powder (being the SiO2 powder, average grain diameter＜8 μ m) | 28 |
| Silane | 1.2 |
| Butanone | 18 |
| Propylene glycol monomethyl ether | 19 |
2. gluing baking: prepreg gluing speed 23m/min
3. prepreg is controlled parameter: gel time 118 seconds
Resin content 44.6%
Resin flow 24.1%
Fugitive constituent 0.41%
4. sheet material composing structure: thickness 1.6mm after 8 7628 prepreg pressings
5. pressing plate parameter: vacuum-0.078MPa
Pressure 240-520psi
Temperature of heat plate 100-215 ℃
50 minutes hardening times
6. substrate performance parameter:
Embodiment 3:
1. impregnation formula rate (weight share meter):
| Former material | Formula rate (mass ratio) |
| Nitrogen heterocyclic ring modification polyfunctional epoxy resin | 55 |
| High heat resistance modified bisphenol type epoxy | 15 |
| Linear phenolic curing agent | 39 |
| Diphenyl-imidazole | 3.3 |
| Silicon powder (being the SiO2 powder, average grain diameter＜8 μ m) | 12 |
| Silane | 0.8 |
| Butanone | 13 |
| Propylene glycol monomethyl ether | 15 |
2. gluing baking: prepreg gluing speed 18m/min
3. prepreg is controlled parameter: gel time 107 seconds
Resin content 46.2%
Resin flow 19.9%
Fugitive constituent 0.36%
4. sheet material composing structure: thickness 1.6mm after 8 7628 prepreg pressings
5. pressing plate parameter: vacuum-0.092MPa
Pressure 130-450psi
Temperature of heat plate 80-220 ℃
60 minutes hardening times
6. substrate performance parameter:
Above-mentioned epoxide glass cloth base copper coated foil plate TG 〉=150 that make ℃, have outstanding hear resistance and anti-CAF, very low Z-CTE value and water absorption rate, also have good comprehensive Performance Characteristicses such as good dimensional stability and machining property, anti-electrification, flame resistance, be applicable to the demand that PCB leadless process and multi-layer sheet are produced fully.
More than show and described basic principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (2)
1. middle Tg lead-free compatible epoxide glass cloth base copper coated foil plate, it is characterized in that, mainly by modification polyfunctional epoxy resin, high heat resistance modified bisphenol type epoxy, linear phenolic curing agent, and interpolation auxiliary material, the adhesive that is modulated into, adhesive apply gluing on glass fabric, are covered with Copper Foil again and prepare through hot pressing, thickness of slab is 0.05～3.2mm, and used copper thickness is 1/3oz～5oz;
The composition of adhesive according to the quality proportioning is:
Nitrogen heterocyclic ring modification polyfunctional epoxy resin, 40～90 parts;
High heat resistance modified bisphenol type epoxy, 1～20 part;
Linear phenolic curing agent, 20～60 parts;
Imidazoles promoter, 0.05～5.0 part;
Silicon powder, i.e. SiO
2Powder, average grain diameter＜8 μ m, 5～60 parts;
Silane, 0.05～5.0 part;
Butanone, 5～50 parts;
Propylene glycol monomethyl ether, 5～50 parts.
2. the preparation method of the described middle Tg lead-free compatible epoxide glass cloth base copper coated foil plate of claim 1 is characterized in that, may further comprise the steps,
1) impregnation;
A) in tank diameter, add propylene glycol monomethyl ether, butanone, silane successively by formula ratio, turn on agitator, 500～1500 rev/mins of rotating speeds keep continuing stirring and control flume body temperature degree at 20～50 ℃, add silicon powder again, add the back that finishes and continue to stir 10～50 minutes;
B) in tank diameter, add nitrogen heterocyclic ring modification polyfunctional epoxy resin, high heat resistance modified bisphenol type epoxy, linear phenolic curing agent more successively by formula ratio, keep stirring with 1000～1500 rev/mins of rotating speeds in the reinforced process, open efficient shearing and emulsification 0.5～4 hour after interpolation finishes, carry out cooling water simultaneously and circulate with retentive control cell body temperature at 20～50 ℃;
C) take by weighing imidazoles promoter by formula ratio, and the adding propylene glycol monomethyl ether, make the dissolving of imidazoles promoter fully, confirm after the no crystallization consoluet imidazoles promoter to be added in the tank diameter, and continuing to keep 1000～1500 rev/mins of stirrings 3～15 hours, impregnation is finished;
2) gluing, prepreg processed;
A) adhesive is recycled to gluing machine, through preimpregnation, main soaking, evenly is coated on adhesive on the glass fabric; The gluing machine linear velocity is controlled to be 6～28m/min;
B) glass fabric of application of adhesive toasts through 120 ℃～250 ℃ drying bakers, makes solvent evaporates, and the adhesive initial reaction solidifies, and makes prepreg;
The control of prepreg physical parameter: gelation time: 60～150 seconds, the resin quality percentage composition was 36%～75%, and the resin ratio flow is 15%～40%, volatile matter＜0.75%;
3) set type, suppress;
Prepreg is cut into same size, 1～18 one group, superimposed with Copper Foil again, compacting then;
Described imidazoles promoter be methylimidazole, diethyl tetramethyl imidazoles, diphenyl-imidazole one of them;
In the described step 3), the compacting parameter is as follows:
A. pressure: 100～550psi;
B. temperature: 80～220 ℃;
C. vacuum: 0.030～0.080MPa;
D. press time: 90～150 minutes;
E. hardening time: 30～60 minutes.
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| CN102166854B true CN102166854B (en) | 2013-07-10 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110116541A (en) * | 2019-05-13 | 2019-08-13 | 广德龙泰电子科技有限公司 | A kind of middle TG reheating deformation solidification copper-clad laminate production technology |
| CN110239164B (en) * | 2019-06-13 | 2021-08-27 | 重庆德凯实业股份有限公司 | High-heat-resistance middle-Tg copper-clad plate and preparation method thereof |
| CN110588116A (en) * | 2019-09-04 | 2019-12-20 | 重庆德凯实业股份有限公司 | Flame-retardant heat-resistant copper foil-coated epoxy glass fiber cloth-based laminated board and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827365A (en) * | 2006-04-13 | 2006-09-06 | 上海南亚覆铜箔板有限公司 | Epoxide woven glass fabric copper-clad laminates for leadless process and method for preparing same |
| CN101790278A (en) * | 2010-02-10 | 2010-07-28 | 上海南亚覆铜箔板有限公司 | Full photophobic copper-clad laminate and preparation method thereof |
| CN101797825A (en) * | 2010-02-10 | 2010-08-11 | 上海南亚覆铜箔板有限公司 | Copper-clad laminate suitable for high-order high density interconnect build-up multilayer and preparation method thereof |
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2010
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827365A (en) * | 2006-04-13 | 2006-09-06 | 上海南亚覆铜箔板有限公司 | Epoxide woven glass fabric copper-clad laminates for leadless process and method for preparing same |
| CN101790278A (en) * | 2010-02-10 | 2010-07-28 | 上海南亚覆铜箔板有限公司 | Full photophobic copper-clad laminate and preparation method thereof |
| CN101797825A (en) * | 2010-02-10 | 2010-08-11 | 上海南亚覆铜箔板有限公司 | Copper-clad laminate suitable for high-order high density interconnect build-up multilayer and preparation method thereof |
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Address after: Shanghai city Chang Cheung Road 201812 Jiading District Nanxiang Town, No. 158 Patentee after: South Asia new materials Polytron Technologies Inc Address before: Shanghai city Chang Cheung Road 201812 Jiading District Nanxiang Town, No. 158 Patentee before: Shanghai Nanya Copper Clad Laminate Co., Ltd. |