CN101781443B - Thermosetting solder masking film composite - Google Patents
Thermosetting solder masking film composite Download PDFInfo
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- CN101781443B CN101781443B CN200910005628XA CN200910005628A CN101781443B CN 101781443 B CN101781443 B CN 101781443B CN 200910005628X A CN200910005628X A CN 200910005628XA CN 200910005628 A CN200910005628 A CN 200910005628A CN 101781443 B CN101781443 B CN 101781443B
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- epoxy resin
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- film composite
- thermosetting solder
- solder masking
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Abstract
The invention provides a thermosetting solder masking film composite, which is applied to a flexible printed circuit board and comprises the following components in part by weight: (a) 50 to 100 parts of epoxy resin, b) 1 to 10 parts of hardening agent and (c) 1 to 10 parts of catalyst. The epoxy resin at least comprises an aliphatic polyester modified epoxy resin represented by the formula (I) or the formula (II), wherein R1 and R2 are saturated or unsaturated C6 to C38 carbon chains respectively; R3 is an ether, a benzene ring, a C6 to C38 heterocycle or a C6 to a C38 saturated carbon chain; n is an integer between 1 and 10; and the weight average molecular weight of the aliphatic polyester modified epoxy resin is 1,000 to 5,000.
Description
Technical field
The present invention relates to a kind of weld-proof membrane compsn, particularly a kind of thermosetting solder masking film composite that is used for bendable printed substrate.
Background technology
Flexible printed wiring board has flexibility, can cooperate light, thin, short, the little demand of electronic product, is widely used in the various industries such as space flight, motor, machinery, automobile, electronics.Because the copper cash on the flexible printed wiring board is influenced and oxidation by external environment easily; Therefore need the protective membrane of the similar scolding tin shielding of one deck (SolderMask) function to prevent the copper cash oxidation; Scolding tin shielding (also claiming green lacquer) is a kind of printing ink of being made up of epoxy resin; Too crisp and flexibility is not good after its film forming, therefore be not suitable for the flexible printed wiring board of high flexibility.
The employed protective membrane material of flexible printed wiring board is a protective membrane for pi (PI) protective membrane or the acryl that contains one deck epoxy resin (epoxy) solid traditionally; When this kind material is applied to not have the copper foil laminates of solid; Will cause the asymmetric of material structure, make that the flexibility (flexibility) of flexible base plate is not good, in addition; Because the poor heat resistance of adhesion agent layer and contraction are big, can cause the heat-resisting character and the dimensional stability variation of flexible base plate.In addition; When being applied to cover brilliant film (chip on flex; Be called for short COF) during product, need be with flexible printed wiring board bending and setting, and that tradition contains the PI protective membrane of adhesion agent layer is too firm; Restorer is difficult for setting greatly when flexible printed wiring board bends, and therefore can't be applied on the COF product.
The liquid protective film material that another kind is used for flexible printed wiring board is an epoxy resin system, and it need add rubber as softening agent, to improve the insufficient problem of flexibility; But the poor heat resistance of rubber; And compatible bad with epoxy resin can make and in high temperature scolding tin preparation technology, have problems protective membrane thermotolerance variation if add too many rubber; And if rubber adds deficiency, then the protective membrane flexibility is understood variation and embrittlement.
In U.S. Pat 6818702 and US2007/0088134, do not carry out modification to the epoxy resin deflection is good; It is utilize terminal group contain-COOH or-OH functional group's polyhutadiene (polybutadiene) and epoxy resin (epoxy) reaction; Though can obtain good flexibility; But its synthesis step is complicated and thermotolerance and then property is not good, in subsequent preparation technology, is prone to peel off with sheet material.
In addition; At Japanese Patent JP2006124681, JP2007246648; And mention in the U.S. Pat 2007/0293636 and utilize urethane (urethane) modified epoxy; To have-OH functional group's polycarbonate (polycarbonate) and vulcabond (diisocyanate), and form with dimethylol propionic acid (dimethylopropionic acid) reaction and have-mixes with epoxy resin again behind COOH functional group's the urethane (PU), though have the flexibility of excellence; But the proportion of urethane (urethane) is too high, makes it heat-resisting not good with endurance.In addition, use acryl rubber to add epoxy resin improving flexibility in addition, but the thermotolerance of acryl still is lower than epoxy resin, causes its thermotolerance not good.
Therefore, industry is needed a kind of weld-proof membrane compsn badly, and it has good flexibility, thermotolerance and other characteristic, to meet the demand of flexible printed wiring board protective membrane.
Summary of the invention
The object of the present invention is to provide a kind of have good flexibility and thermotolerance, can meet the thermosetting solder masking film composite of the demand of flexible printed wiring board protective membrane.
The present invention provides a kind of thermosetting solder masking film composite, is applicable to bendable printed substrate, comprises (a) 50～100 weight part epoxy resin, and this epoxy resin comprises the epoxy resin that an aliphatic poly is ester modified at least, shown in (I) or formula (II):
, R wherein
1With R
2Be independently to be C separately
6-38Saturated or unsaturation carbochain, R
3Be ether, phenyl ring, C
6-38Heterocycle or C
6-38Saturated carbon chains, n are 1～10 integer, and the weight average molecular weight of the ester modified epoxy resin of aliphatic poly is 1000～5000; (b) 1～10 weight part stiffening agent; And (c) 1～10 weight part catalyzer.
Thermosetting solder masking film composite of the present invention has good flexibility, agent of low hygroscopicity and thermostability, meets the demand of flexible printed wiring board protective membrane, can be used as the anti-solder ink of flexible printed wiring board
In order to let above-mentioned purpose of the present invention, characteristic and the advantage can be more obviously understandable, elaborate as follows:
Embodiment
Thermosetting solder masking film composite of the present invention is mainly used in flexible printed wiring board (flexible printedcircuit board; Be called for short FPC) in as protective membrane; With the copper cash on the protection flexible printed wiring board; It has soldering resistance simultaneously, can be used as scolding tin shielding (solder mask), in subsequent preparation technology, avoids copper cash to suffer damage.
At least contain the ester modified epoxy resin of a kind of aliphatic poly in the thermosetting solder masking film composite of the present invention; Aliphatic polyester has flexibility and agent of low hygroscopicity; Can absorb and dash shake and stress; And have hydrophobic property, utilize the ester modified epoxy resin of aliphatic poly can allow that epoxy system imports tool HMW and soft section big polyester construction, with the flexibility that promotes material and reduce permeability rate.In addition; Aliphatic polyester is difficult for because of heat or oxidation decomposition; Therefore thermosetting solder masking film composite of the present invention can have good flexibility, agent of low hygroscopicity and thermostability, meets the demand of flexible printed wiring board protective membrane, as the anti-solder ink of flexible printed wiring board.
In one embodiment of this invention, thermosetting solder masking film composite comprises:
(a) 50～100 weight part epoxy resin, and this epoxy resin comprise the ester modified epoxy resin of aliphatic poly shown in following formula (I) or formula (II) at least:
, R wherein
1With R
2Be independently to be C separately
6-38Saturated or unsaturation carbochain; R
3Be ether, phenyl ring, C
6-38Heterocycle or C
6-38Saturated carbon chains; N is 1～10 integer, and the weight average molecular weight (Mw) of the ester modified epoxy resin of this aliphatic poly is 1000～5000;
(b) 1～10 weight part stiffening agent; And
(c) 1～10 weight part catalyzer.
In above-mentioned epoxy resin, the ratio that the ester modified epoxy resin of aliphatic poly accounts for the overall loop epoxy resins is about 30～100 weight %.Except the ester modified epoxy resin of aliphatic poly; Remaining epoxy resin can be for bisphenol A type epoxy resin, cyclic aliphatic epoxy resin, contain phenyl ring epoxy resins, two phenyl ring epoxy resins, resol epoxy resin, liquid nbr carboxyl terminal (carboxyl-terminatedacrylonitrile-butadiene is called for short CTBN) modification (modified) epoxy resin or aforesaid combination.
Above-mentioned stiffening agent can be acid anhydrides (anhydride) verivate, diamines (diamine) verivate or polyamine (polyamine); Wherein anhydride ester derivs for example is methylhexahydrophthalic anhydride (methylhexahydrophthalic anhydride; Be called for short MHHPA) or methyl tetrahydrophthalic anhydride (methyltetrahydrophthalic anhydride); Diamine derivative for example is 4; 4-diaminodiphenylsulfone(DDS) (4,4-diaminodiphenyl sulfone), polyamine for example are polyetheramine (polyether diamine).
Above-mentioned catalyzer can be imidazoles (imidazole) verivate; 2-ethyl-4-methylimidazole (2-ethyl-4-methyl-imidazole), 2 for example, 4-diamino--6-[2-(2-methyl isophthalic acid-imidazolyl) ethyl]-1,3; 5-thiazine (2; 4-diamino-6-[2-(2-methyl-1-imidazolyl) ethyl] 1,3,5-triazine) or glyoxal ethyline (2-methylimidazole).
In addition; In order to make the processibility and the rerum natura of weld-proof membrane material better; Can also add other additive in the thermosetting solder masking film composite of the present invention; For example smooth dose (leveling agent), inorganic filler (filler), pigment (pigment), skimmer (deformer), flame retardant or aforesaid combination, the total amount of these additives can be 1～10 weight part.
The mode of thermosetting solder masking film composite of the present invention screen painting capable of using (screening printing) is coated on the flexible printed wiring board, hardens with 150～180 ℃ temperature again.In addition, thermosetting solder masking film composite of the present invention also can be used on the rigid printed circuit board as the resist of anti-scolding tin, or is used as solid and uses.
Preparation and its characteristic of the thermosetting solder masking film composite of various embodiments of the present invention and comparative example below are detailed.
[embodiment 1]
50g epoxy resin E-1 and 50g epoxy resin (Epoxy) (product type Epikot 828, Shell company) are dissolved in the gamma-butyrolactone (gamma-butyrolactone is called for short GBL) of 22g, obtain colloidal mixt (Vanish) V-1 behind the uniform mixing.The weight average molecular weight of epoxy resin E-1 is about 2412, and its structure is as follows:
Then; Add the stiffening agent methylhexahydrophthalic anhydride (MHHPA) of 5g, the catalyzer 2 of 2g; 4-diamino--6-[2-(2-methyl isophthalic acid-imidazolyl) ethyl]-1,3, the 5-thiazine (is called for short 2MAZ-PW; Four countries change into company), the veridian (pigment green) of 2g, silica-filled thing (the model Aerosil-380 of 5g; Degussa company) and the skimmer of 1g (model KS-66, Shin-Etsu company) after three roller grinders (thriple-roll mill) grind evenly, obtain the thermosetting solder masking film resin material of embodiment 1.
[embodiment 2]
Method with embodiment 1; Wherein the usage quantity of epoxy resin E-1 is 70g, and the usage quantity of epoxy resin (Epoxy) Epikot 828 is 30g, the stiffening agent MHHPA of 5g; The 2-ethyl-4-methylimidazole of 2g (is called for short 2E4MI; Four countries change into company), after the grinding evenly of three roller grinders, obtain the thermosetting solder masking film resin material of embodiment 2.
[embodiment 3]
70g epoxy resin E-2 and 30g epoxy resin (Epoxy) Epikot 828 are dissolved in the gamma-butyrolactone (GBL) of 22g, obtain colloidal mixt (Vanish) V-2 behind the uniform mixing.The weight average molecular weight of epoxy resin E-2 is about 3984, and its structure is as follows:
Then; The skimmer (KS-66) of the veridian of the stiffening agent MHHPA of adding 5g, the catalyzer 2MAZ-PW of 2g, 2g, the silica-filled thing (Aerosil-380) of 5g and 1g obtains the thermosetting solder masking film resin material of embodiment 3 after three roller grinders grind evenly.
[embodiment 4]
Method with embodiment 3; Wherein the amount of epoxy resin E-2 is epoxy resin (Epoxy) (the product type EPOMIK SR3542 of 80g and 20g CTBN modification; Mitsui Chemical company), is dissolved in the gamma-butyrolactone (GBL) of 35g, obtains colloidal mixt (Vanish) V-4 behind the uniform mixing.
Then; The skimmer (KS-66) of the veridian of the stiffening agent MHHPA of adding 5g, the catalyzer 2E4MI of 2g, 2g, the silica-filled thing (Aerosil-380) of 5g and 1g obtains the thermosetting solder masking film resin material of embodiment 4 after three roller grinders grind evenly.
[embodiment 5]
With 70g epoxy resin E-3 and 30g epoxy resin (Epoxy) Epikot 828, be dissolved in the gamma-butyrolactone (GBL) of 30g, obtain colloidal mixt (Vanish) V-5 behind the uniform mixing.The weight average molecular weight of epoxy resin E-3 is about 2470, and its structure is as follows:
Then; The stiffening agent MHHPA, the catalyzer 2E4MI of 2g, the veridian of 2g, the silica-filled thing (Aerosil-380) of 5g and the skimmer (KS-66) of 1g that add 5g; After three roller grinders grind evenly, obtain the thermosetting solder masking film resin material of embodiment 5.
[comparative example 1]
With 70g epoxy resin (Epoxy) (product type Epikot 828; Shell company), 30g epoxy resin (Epoxy) (product type Epon1001; Shell company), 20g stiffening agent diamino diphenyl sulfone (diaminodiphenyl sulphone is called for short DDS) and catalyst B F
3Be dissolved in the gamma-butyrolactone (GBL) of 75g; And then veridian, the silica-filled thing (Aerosil-380) of 5g and the skimmer (KS-66) of 1g of adding 2g; After three roller grinders grind evenly, obtain the thermosetting solder masking film resin material of comparative example 1.
[comparative example 2]
With the method for embodiment 1, wherein the usage quantity of epoxy resin E-1 is 20g, and the usage quantity of epoxy resin (Epoxy) Epikot 828 is 80g, with stiffening agent DDS and the catalyst B F of 20g
3Be dissolved in the gamma-butyrolactone (GBL) of 75g; And then veridian, the silica-filled thing (Aerosil-380) of 5g and the skimmer (KS-66) of 1g of adding 2g; After three roller grinders grind evenly, obtain the thermosetting solder masking film resin material of comparative example 2.
The resin material of the foregoing description 1～5 is coated on the flexible substrate for printed circuit board, after 150 ℃, 60 minutes condition sclerosis film forming, tested its flexibility.In addition, also the resin material of comparative example 1～2 is coated on the flexible substrate for printed circuit board, after 180 ℃, 120 minutes condition sclerosis film forming, tested its flexibility.Flexibility test be with the resin material coat side to the outside, bend testing sample repeatedly, the bending number of times when testing its resin material coating damage with 180 degree.The flexibility test result such as the table 1 of above-mentioned each embodiment and comparative example are listed, and its result shows that the weld-proof membrane of the embodiment of the invention can reach more than 20 times by anti-number of flexings, and the weld-proof membrane of comparative example then only can promptly damage for 1～4 time in anti-deflection.
The resin material of each embodiment of table 1 and comparative example is formed and flexibility
In addition, the thermosetting solder masking film resin material of embodiment 1～3 is carried out various tests, like tests such as physical strength, toughness, thermotolerance, endurance, anti-scolding tin, water-intake rate, chemically-resistant gold, its result such as table 2 are listed.Physical strength in the table 2 is its tensile strength of test and expansion and contraction; Toughness is coated on two-layer copper foil base material (the two-layer copper foil) surface ratio of institute's warpage for its film of test; The thermotolerance test is for to utilize thermogravimetric analyzer (TGA) to test the temperature of its weight loss 5%; Endurance is its acid and alkali-resistance medicine property of test, solvent resistance and chemically-resistant gold; Wherein test solvent is Virahol (isopropyl alcohol; Be called for short IPA) and methylethylketone (methyl ethyl ketone is called for short MEK), the test of chemically-resistant gold mainly is to need in subsequent preparation technology to weld-proof membrane that experience is gold-plated to be designed with nickel plating preparation technology; Wherein gold-plated thickness is 0.03～0.19 μ m, and the nickel plating thickness is 3～9 μ m.
The characteristic of the thermosetting solder masking film of each embodiment of table 2
Result by table 1 and table 2 can learn; Thermosetting solder masking film composite of the present invention has the better flexibility except more traditional weld-proof membrane resin material; Also have characteristics such as good dimensional stability, thermotolerance, endurance, anti-scolding tin, low water absorption, therefore applicable on the flexible printed wiring board as the protective membrane material.
Though the present invention discloses preferred embodiment as above; Right its is not in order to limit the present invention; Any personnel that are familiar with this technology; Do not breaking away from the spirit and scope of the present invention, when can doing a little change and retouching, so protection scope of the present invention is as the criterion when looking the scope that the accompanying Claim book defined.
Claims (8)
1. thermosetting solder masking film composite, it is to be applicable to a bendable printed substrate, comprising:
(a) 50～100 weight part epoxy resin, and said epoxy resin comprise the epoxy resin that an aliphatic poly is ester modified at least, shown in (I) or formula (II):
R wherein
1With R
2Be independently to be C separately
6-38Saturated or unsaturation carbochain, R
3Be ether, phenyl ring, C
6-38Heterocycle or C
6-38Saturated carbon chains, n are 1～10 integer, and the weight average molecular weight of the ester modified epoxy resin of said aliphatic poly is 1000～5000, are benchmark with said epoxy resin integral wherein, and the ester modified epoxy resin of said aliphatic poly accounts for 30～100 weight %;
(b) 1～10 weight part stiffening agent; And
(c) 1～10 weight part catalyzer.
2. thermosetting solder masking film composite according to claim 1 is a benchmark with said epoxy resin integral wherein, and the ester modified epoxy resin of said aliphatic poly accounts for 50,70 or 80 weight %.
3. thermosetting solder masking film composite according to claim 1, wherein said epoxy resin comprise cyclic aliphatic epoxy resin, contain the phenyl ring epoxy resins, liquid nbr carboxyl terminal modified epoxy or aforesaid combination.
4. thermosetting solder masking film composite according to claim 3, the wherein said phenyl ring epoxy resins that contains comprises bisphenol A type epoxy resin, two phenyl ring epoxy resins, resol epoxy resin or aforesaid combination.
5. thermosetting solder masking film composite according to claim 1, wherein said stiffening agent are anhydride ester derivs, diamine derivative or polyamine;
Wherein said anhydride ester derivs is methylhexahydrophthalic anhydride or methyl tetrahydrophthalic anhydride;
Wherein said diamine derivative is 4, the 4-diaminodiphenylsulfone(DDS);
Wherein said polyamine is a polyetheramine.
6. thermosetting solder masking film composite according to claim 1, wherein said catalyzer are imdazole derivatives;
Wherein said imdazole derivatives is a 2-ethyl-4-methylimidazole, 2,4-diamino--6-[2-(2-methyl isophthalic acid-imidazolyl) ethyl]-1,3,5-thiazine or glyoxal ethyline.
7. thermosetting solder masking film composite according to claim 1 also comprises an additive.
8. thermosetting solder masking film composite according to claim 7, wherein said additive are smooth dose, inorganic filler, pigment, skimmer, flame retardant or aforesaid combination.
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| CN200910005628XA CN101781443B (en) | 2009-01-20 | 2009-01-20 | Thermosetting solder masking film composite |
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| CN200910005628XA CN101781443B (en) | 2009-01-20 | 2009-01-20 | Thermosetting solder masking film composite |
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| CN101781443B true CN101781443B (en) | 2012-03-28 |
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| KR101983420B1 (en) * | 2011-12-12 | 2019-05-29 | 미쓰비시 마테리알 가부시키가이샤 | Power module substrate, substrate for power module with heat sink, power module, paste for forming flux component penetration prevention layer, and bonding method for article to be bonded |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337975A (en) * | 1998-12-23 | 2002-02-27 | 3M创新有限公司 | Electronic circuit device comprising an epoxy-modified aromatic vinyl-conjugated diene block copolymer |
| CN1654540A (en) * | 2005-01-11 | 2005-08-17 | 大连理工大学 | High temperature resistant epoxy resin composite with lasting storage stability and temperature thixotropy |
| CN1745138A (en) * | 2003-02-10 | 2006-03-08 | 株式会社可乐丽 | Epoxy resin composition |
| CN1948392A (en) * | 2006-10-26 | 2007-04-18 | 复旦大学 | Epoxy resin composition |
| CN101343498A (en) * | 2008-09-01 | 2009-01-14 | 天津科瑞达涂料化工有限公司 | Paint for high-class woodenware artwork and preparation thereof |
-
2009
- 2009-01-20 CN CN200910005628XA patent/CN101781443B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337975A (en) * | 1998-12-23 | 2002-02-27 | 3M创新有限公司 | Electronic circuit device comprising an epoxy-modified aromatic vinyl-conjugated diene block copolymer |
| CN1745138A (en) * | 2003-02-10 | 2006-03-08 | 株式会社可乐丽 | Epoxy resin composition |
| CN1654540A (en) * | 2005-01-11 | 2005-08-17 | 大连理工大学 | High temperature resistant epoxy resin composite with lasting storage stability and temperature thixotropy |
| CN1948392A (en) * | 2006-10-26 | 2007-04-18 | 复旦大学 | Epoxy resin composition |
| CN101343498A (en) * | 2008-09-01 | 2009-01-14 | 天津科瑞达涂料化工有限公司 | Paint for high-class woodenware artwork and preparation thereof |
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