CN102010673B - High-performance modified acrylate adhesive used in FPC (Flexible Printed Circuit) filed - Google Patents
High-performance modified acrylate adhesive used in FPC (Flexible Printed Circuit) filed Download PDFInfo
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- CN102010673B CN102010673B CN 200910063929 CN200910063929A CN102010673B CN 102010673 B CN102010673 B CN 102010673B CN 200910063929 CN200910063929 CN 200910063929 CN 200910063929 A CN200910063929 A CN 200910063929A CN 102010673 B CN102010673 B CN 102010673B
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Abstract
The invention relates to a high-performance modified acrylate adhesive used in the FPC (Flexible Printed Circuit) filed, relating to a modified acrylate adhesive and application of the adhesive on a FPC base material. The invention mainly aims at solving the problems of poor weather resistance, low temperature resistance and high moisture absorption rate of the known modified acrylate. The high-performance modified acrylate adhesive comprises the following components in parts by weight: 90-100 parts of acrylate copolymerization water emulsion, 0-10 parts of organic silicon monomer with allyl, 0-10 parts of inorganic filler, 10-20 parts of modified benzoxazinyl with allyl, 1-5 parts of antioxidant and catalyst and 80-120 parts of water. The adhesive has high performance index, ensures that the copper foil, aluminum foil, polyimide film and polyester film can be firmly adhered, can resist a high temperature of 300 degrees for 30 seconds, the folding of more than 3,000 times, soaking in 2NaOH and 2NHC for 130 minutes without foaming, layering, adhering and colour varying, and the low-high-temperature impact from 100 DEF C below zero to 300 DEG C and has the adhesive overflow quality of less than 0.1mm, the flame resistance at 94-V0 level and the water absorption rate of lower than 2%.
Description
Technical field
The present invention relates to a kind of tackiness agent, the application of specifically a kind of modified acrylic ester adhesion agent for flexible printed circuit board (FPC), and this tackiness agent on the FPC base material.
Background technology
Since flexible printed circuit board (FPC) have can deflection characteristic, can reduced volume, can realize the requirement that electronic product is short, little, thin, light, be used widely at products such as automotive electronics, digital camera and Kamera, communication equipment, liquid crystal image demonstrations; Be applied at present the business-like tackiness agent in FPC field and mainly contain modified acrylic ester adhesion agent and epoxy binder modified.The advantage of modification acrylate contrast modified epoxy is that environmental protection, cost are lower, the glue amount of overflowing is little.To be that weathering resistance is relatively poor (just scrapped with interior curing inferior position in six months substantially, placement flavescence more than two months), lower (more than 300 ℃ of modified epoxy of contrast of temperature tolerance, only have about 270 ℃, especially the mandatory use of Pb-free solder causes basically not reaching the requirement of soldering resistance), higher, the poor dimensional stability of moisture absorption ratio, easily produce bubble etc. in the after fixing stage; For the acrylic ester adhesive shortcoming, E.I.Du Pont Company has used phenolic aldehyde to improve its thermotolerance as cure-crosslinking agent, but because phenolic aldehyde exists and easily emit small molecules in solidification process, the stable on heating restriction of phenolic aldehyde itself, and the shortcoming such as the residual excessive phenol of emulsion system or the environmentally harmful material of formaldehyde, so that its use range and market share in the FPC field is restricted, patent of invention CN1827726A adopts the aldehyde amine hardener, and the thermotolerance that obtains only has the modified acrylic ester adhesion agent about 260 ℃.Also have and adopt urethane, organosilicon, modification butyronitrile etc. to be used as some trials of its cure-crosslinking agent and heat-resistant agent, but also do not have the acrylic ester adhesive thermotolerance of bibliographical information modification above 300 ℃ at present.
Summary of the invention
The objective of the invention is for above-mentioned deficiency, and the thermotolerance of a kind of tackiness agent that provides surpasses 300 ℃, and its weathering resistance is high, moisture absorption ratio is low, good stability of the dimension, and cure stage does not produce the modified acrylic ester adhesion agent of bubble.
Technical solution of the present invention is: the FPC field with the prescription of high-performance modified acrylic ester adhesive is by mass:
Acrylic ester copolymer water miscible liquid 90-100 part;
With allylic organosilane monomer 0-10 part;
Mineral filler 0-10 part;
With allylic modified benzoxazine 10-20 part;
Antioxidant and catalyzer 1-5 part;
Distilled water (comprising the water in the acrylic ester copolymer water miscible liquid) 80-100 part.
Acrylic acid copolymer whey liquid water described in the technology of the present invention solution carries out mixed preparing by 122.2 parts of 67 parts of butyl acrylates, 29 parts of vinyl cyanide, 3 parts in vinylformic acid, 0.5 part of sodium lauryl sulphate, 0.51 part of Sodium Persulfate, distilled water.Reaction is 3-4 hour in 80-85 ℃ of reactor, be cooled to room temperature after, with ammoniacal liquor and water viscosity is regulated, viscosity controller is 15-20 second (being coated with-4 glasss records), the filtration of 400 order filtering nets obtains stable acrylic ester copolymer water miscible liquid.
Comprising with allylic organosilane monomer described in the technology of the present invention solution: one or more mixtures of r-propyl methacrylate trimethoxy silane, r-β-dimethyl-aminoethylmethacrylate trimethoxy silane, r-β-dimethyl-aminoethylmethacrylate three ethoxy silane, r-propyl methacrylate triethoxyl silane, preferably r-propyl methacrylate trimethoxy silane and r-propyl methacrylate triethoxyl silane.
Comprising with allylic modified benzoxazine described in the technology of the present invention solution: diallyl Er benzoxazine, with the benzoxazine of maleimide and propylene ether, with the benzoxazine of clothing health imide and propylene ether, with the benzoxazine of maleimide and propenyl, with one or more mixtures of the benzoxazine of clothing health imide and propenyl, preferably with the benzoxazine of maleimide and propylene ether, with the benzoxazine of clothing health imide and propylene ether.
Mineral filler described in the technology of the present invention solution comprises: one or more mixtures of silicon-dioxide, aluminum oxide, talcum, mica powder, silicon nitride, boron nitride, aluminium hydroxide, preferably silicon nitride and aluminium hydroxide.
Antioxidant described in the technology of the present invention solution comprises: 2,2,4-trimethylammonium-1, a kind of or both mixtures of 2-dihyaroquinoline polymer and sulfuration dipropionic acid two lauryls.
Catalyzer described in the technology of the present invention solution comprises: imidazoles, Methylimidazole, Witco 1298 Soft Acid etc., preferred imidazoles.
FPC field described in the technology of the present invention solution with the preparation method of high-performance modified acrylic ester adhesive is:
1. prepare stable acrylic ester copolymer water miscible liquid as response composite 1;
2. will mix as response composite 2 with allylic organosilane monomer with allylic modified benzoxazine and mineral filler, oxidation inhibitor, catalyzer, distilled water under the normal temperature;
3. under the normal temperature response composite 1 and 2 is mixed in colloidal mill, the solution combination treatment of gained 2-3 time, each about 10 minutes, leave standstill at last froth breaking, obtaining viscosity is the stable emulsion of 14-18 about second.
FPC field described in the technology of the present invention solution with the preparation method of high-performance modified acrylic ester adhesive is:
1. will be prepared into first the copolymerization water miscible liquid as response composite 3 by the prescription requirement with the organosilane monomer of propyl group with allylic modified benzoxazine and acrylic ester monomer;
2. under the normal temperature, with mineral filler, oxidation inhibitor and catalyzer, distilled water mix as response composite 4;
3. under the normal temperature, in colloidal mill with the solution combination treatment of composition 3 and composition 4 gained 2-3 time, each about 10 minutes, leave standstill at last froth breaking, obtaining viscosity is the stable emulsion of 14-18 about second.
The high-performance modified acrylic ester adhesive in FPC field described in the technology of the present invention solution, sticking with glue the method that agent prepares the FPC base material is: the one side that tackiness agent is evenly coated in polyimide or polyester film, the thick 0.2-0.4mm of glue, in 110 ℃ baking oven, processed 20-30 minute, obtain the prepreg film (thickness 10-40um) of tackiness agent; Plastic packaging machine by 110 ℃ will carry out tentatively compound with the adhesive faec of the polyimide of prepreg film or polyester film and Copper Foil or aluminium foil again; Then with its in the pressure bonding machine take temperature as 180-200 ℃, pressure is 20-60Kgf/cm
2, the time is to process in 20-60 minute, makes the FPC base material; Described Copper Foil is rolled copper foil or electrolytic copper foil, and its thickness is in the 12-38um scope, and rolled copper foil is preferably 18um.
Because adopting to have, the present invention heat-resistingly surpasses 400 ℃ with the cure-crosslinking agent of allylic benzoxazine as acrylic ester adhesive, utilize allyl group and the acrylate at initial stage to pass through free-radical polymerized, utilize the ring-opening polymerization of benzoxazine in the after fixing stage, so that cured glue stick System forming inierpeneirating network structure, therefore greatly improved the thermotolerance of tackiness agent, its thermotolerance surpasses 300 ℃, and the allylic organosilicon of combined belt has improved the weathering resistance of acrylate greatly; And tackiness agent moisture absorption ratio of the present invention is lower, and good stability of the dimension can not produce bubble in the after fixing stage; Tackiness agent of the present invention also has very high performance index value: can the good bond Copper Foil, aluminium foil, Kapton, polyester film, and can high temperature resistant 300 ℃ of 30s; Folding is greater than 3000 times; Anti-2NNaOH, 2NHCl30 minute immersion without foaming, layering, be clamminess and colour-change, the stripping strength conservation rate reaches 85%; Tolerate-100 ℃ to 300 ℃ low high temperature impacts; Dimensional stability is less than 0.2% after solidifying; The glue amount of overflowing is less than 0.1mm; Flame retardant resistance is by the 94-V0 level; Water-intake rate is lower than 2%; Solidification process is emitted without small molecules, and tackiness agent is the water-based emulsion system simultaneously, and eco-friendly characteristics are arranged.
The tackiness agent that uses the present invention to make, bonding Copper Foil, aluminium foil and Kapton, polyester film are made flexible circuit board (FPC) base material, and its characteristics are:
(1) tackiness agent prepreg preparation temperature＜130 ℃, time＜30 minute;
(2) adhesive solidification temperature＜200 ℃, pressure 2.5-3.0Kgf, time＜60 minute;
(3) solidify with the pressing of 18um rolled copper foil after, stripping strength (peeling off Copper Foil for 90 °)＞0.8Kgf/cm;
(4) 300 ℃ of 30S of immersed solder property testing are without bubbling layering;
(5) excessive glue measures examination＜0.1mm;
(6) the dimensional stability test＜0.2%;
(7) insulation resistance: Rs1 * 10
12Ω, Rv1 * 10
14Ω;
(8) volatile content＜1.0%;
(9) flame resistivity is by the 94-V0 level;
(10) chemical resistant properties: 2NNaOH, 2NHCl30 minute immersion without foaming, layering, be clamminess and colour-change, the stripping strength conservation rate reaches 85%;
(11) water-intake rate＜2.0%.
Embodiment
The invention will be further described with following example.
Embodiment 1
Under the normal temperature, in the 300ml three-necked bottle, add successively sodium lauryl sulphate 0.5g, distilled water 122.2g, middling speed stirs and forms uniformly emulsify liquid; Again in whipping process with butyl acrylate 67g, vinyl cyanide 29g, vinylformic acid 3g, Sodium Persulfate 0.4g, add rear lasting stirring 20-30 minute, form not stratified pre-emulsion.Get out approximately 2/3 pre-emulsion with beaker, set up reflux condensing tube, constant pressure funnel, water-bath, make remaining about 1/3 pre-emulsion stirring reaction 0.5 hour under 78-80 ℃ condition, then be warming up to 80-85 ℃, utilize constant pressure funnel that approximately 2/3 the pre-emulsion in the beaker was continued to add uniformly three-necked bottle at 2.5 hours and participate in reaction, add Sodium Persulfate 0.1g after dripping off, insulation reaction 1-1.5 hour again, be cooled at last room temperature, available suitable ammoniacal liquor and water are regulated viscosity, general viscosity controller is 15-20 second (being coated with-4 glasss records), 400 order filtering nets filter and obtain stable acrylate copolymer emulsion, obtain response composite 1.
Under the normal temperature, in the 100ml flask, add successively r-propyl methacrylate trimethoxy silane 5g, with the benzoxazine 15g of maleimide and propylene ether, silicon nitride 2g, sulfuration dipropionic acid two lauryl 0.5g, imidazoles 1g, distilled water 35g, high-speed stirring was disperseed 1 hour.Obtain response composite 2.
Under the normal temperature, with response composite 1 and 2 in colloidal mill, combination treatment 3 times, each 10 minutes, froth breaking was left standstill about 3 minutes at last in the interval, obtained viscosity and was 14-18 and stablize high-performance modified acrylic ester adhesive emulsion about second.
Tackiness agent is evenly coated in the one side of polyimide or polyester film, the thick 0.2-0.4mm of glue processed 20-30 minute in 110 ℃ baking oven, obtained the prepreg film (thickness 10-40um) of tackiness agent; Plastic packaging machine by 110 ℃ will carry out tentatively compound with the adhesive faec of the polyimide of prepreg film or polyester film and Copper Foil or aluminium foil again; Then with its in the pressure bonding machine take temperature as 180 ℃, pressure is 40Kgf/cm
2, the time is to process in 40 minutes, makes the FPC base material.
Embodiment 2
Under the normal temperature, add successively sodium lauryl sulphate 0.5g, distilled water 152.2g in the 300ml three-necked bottle, middling speed stirs and forms uniformly emulsify liquid; Again in whipping process with butyl acrylate 67g, vinyl cyanide 29g, vinylformic acid 3g, Sodium Persulfate 0.4g, r-propyl methacrylate trimethoxy silane 5g, with the benzoxazine 15g of maleimide and propylene ether, add rear lasting stirring 20-30 minute, form not stratified pre-emulsion.Get out approximately 2/3 pre-emulsion with beaker, set up reflux condensing tube, constant pressure funnel, water-bath, make remaining about 1/3 pre-emulsion stirring reaction 0.5 hour under 78-80 ℃ condition, then be warming up to 80-85 ℃, utilize constant pressure funnel that approximately 2/3 the pre-emulsion in the beaker was continued to add uniformly three-necked bottle at 2.5 hours and participate in reaction.Add Sodium Persulfate 0.1g after dripping off, insulation reaction 1-1.5 hour again, be cooled at last room temperature, available suitable ammoniacal liquor and water are regulated viscosity, general viscosity controller is 15-20 second (being coated with-4 glasss records), 400 order filtering nets filter and obtain stable acrylate copolymer emulsion, obtain response composite 3.
Under the normal temperature, in the 50ml flask, add successively silicon nitride 2g, sulfuration dipropionic acid two lauryl 0.5g, imidazoles 1g, distilled water 10g, high-speed stirring was disperseed 1 hour, obtained response composite 4.
Under the normal temperature, with response composite 3 and 4 in colloidal mill, combination treatment 3 times, each 10 minutes, froth breaking was left standstill about 3 minutes at last in the interval, obtained viscosity and was 14-18 and stablize high-performance modified acrylic ester adhesive emulsion about second.
Tackiness agent is evenly coated in the one side of polyimide or polyester film, the thick 0.2-0.4mm of glue processed 20-30 minute in 110 ℃ baking oven, obtained the prepreg film (thickness 10-40um) of tackiness agent; Plastic packaging machine by 110 ℃ will carry out tentatively compound with the adhesive faec of the polyimide of prepreg film or polyester film and Copper Foil or aluminium foil again; Then with its in the pressure bonding machine take temperature as 180 ℃, pressure is 40Kgf/cm
2, the time is to process in 40 minutes, makes the FPC base material.
Embodiment 3
Prepare response composite 3 by embodiment 2, under the normal temperature with composition 3 and sulfuration dipropionic acid two lauryl 0.5g, imidazoles 1g, distilled water 4g is in colloidal mill, combination treatment 3 times, each 10 minutes, the interval was about 3 minutes, leave standstill at last froth breaking, obtain viscosity and be 14-18 and stablize high-performance modified acrylic ester adhesive emulsion about second.
Tackiness agent is evenly coated in the one side of polyimide or polyester film, the thick 0.2-0.4mm of glue processed 20-30 minute in 110 ℃ baking oven, obtained the prepreg film (thickness 10-40um) of tackiness agent; Plastic packaging machine by 110 ℃ will carry out tentatively compound with the adhesive faec of the polyimide of prepreg film or polyester film and Copper Foil or aluminium foil again; Then with its in the pressure bonding machine take temperature as 180 ℃, pressure is 40Kgf/cm
2, the time is to process in 40 minutes, makes the FPC base material.
Claims (8)
1. FPC field modified acrylic ester adhesion agent, its prescription is by mass:
Acrylic ester copolymer water miscible liquid 90-100 part;
Mineral filler 0-10 part;
With allylic modified benzoxazine 10-20 part;
Antioxidant and catalyzer 1-5 part;
Distilled water, it comprises the water 80-100 part in the acrylic ester copolymer water miscible liquid;
One or more mixtures 0-10 part in γ-propyl methacrylate Trimethoxy silane, γ-β-dimethyl-aminoethylmethacrylate Trimethoxy silane, γ-β-dimethyl-aminoethylmethacrylate triethoxyl silane or the γ-propyl methacrylate triethoxyl silane;
Wherein, the preparation method of described acrylic ester copolymer water miscible liquid is: carry out mixed preparing by 122.2 parts of 67 parts of butyl acrylates, 29 parts of vinyl cyanide, 3 parts in vinylformic acid, 0.5 part of sodium lauryl sulphate, 0.51 part of Sodium Persulfate, distilled water, reaction is 3-4 hour in 80-85 ℃ of reactor, after being cooled to room temperature, with ammoniacal liquor and water viscosity is regulated, by being coated with-4 glasss of viscosity controller that record in 15-20 second, 400 order filtering nets filter and obtain stable acrylic ester copolymer water miscible liquid.
2. FPC according to claim 1 field modified acrylic ester adhesion agent is characterized in that described is diallyl Er benzoxazine with allylic modified benzoxazine.
3. FPC according to claim 1 field modified acrylic ester adhesion agent is characterized in that described mineral filler comprises: one or more mixtures of silicon-dioxide, aluminum oxide, talcum, mica powder, silicon nitride, boron nitride, aluminium hydroxide.
4. FPC according to claim 3 field modified acrylic ester adhesion agent is characterized in that described mineral filler is one or more mixtures in silicon nitride and the aluminium hydroxide.
5. FPC according to claim 1 field modified acrylic ester adhesion agent is characterized in that described antioxidant is 2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer and Tyox B a kind of or both mixtures.
6. FPC according to claim 1 field modified acrylic ester adhesion agent is characterized in that described catalyzer is imidazoles.
7. FPC according to claim 1 field is with the method for modified acrylic ester adhesion agent for the preparation of the FPC base material, it is characterized in that described method is: the one side that tackiness agent is evenly coated in polyimide or polyester film, the thick 0.2-0.4mm of glue, in 110 ℃ baking oven, processed 20-30 minute, obtain the prepreg film of tackiness agent, thickness 10-40 μ m; Plastic packaging machine by 110 ℃ will carry out tentatively compound with the adhesive faec of the polyimide of prepreg film or polyester film and Copper Foil or aluminium foil again; Then with its in the pressure bonding machine take temperature as 180-200 ℃, pressure is 20-60Kgf/cm
2, the time is to process in 20-60 minute, makes the FPC base material; Described Copper Foil is rolled copper foil or electrolytic copper foil, and its thickness is in 12-38 μ m scope.
8. FPC according to claim 7 field is characterized in that with the method for modified acrylic ester adhesion agent for the preparation of the FPC base material described rolled copper foil thickness is 18 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200910063929 CN102010673B (en) | 2009-09-07 | 2009-09-07 | High-performance modified acrylate adhesive used in FPC (Flexible Printed Circuit) filed |
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|---|---|---|---|
| CN 200910063929 CN102010673B (en) | 2009-09-07 | 2009-09-07 | High-performance modified acrylate adhesive used in FPC (Flexible Printed Circuit) filed |
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| CN102010673B true CN102010673B (en) | 2013-02-06 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102936474B (en) * | 2012-10-17 | 2014-08-27 | 烟台德邦科技有限公司 | Heating curing type modified acrylate pressure sensitive adhesive and preparation method thereof |
| CN105315903B (en) * | 2015-11-24 | 2018-01-16 | 徐昌虎 | A kind of high temperature resistant acrylate pressure-sensitive adhesive and preparation method thereof |
| CN106686898A (en) * | 2017-01-06 | 2017-05-17 | 安徽鹏展电子科技有限公司 | Manufacturing method of flexible printed circuit board for LED light |
| CN110769618B (en) * | 2019-11-05 | 2021-04-06 | 东莞市科佳电路有限公司 | Method for plating copper in PCB hole |
| CN113597088B (en) * | 2021-07-22 | 2022-08-26 | 深圳市华鼎星科技有限公司 | Circuit material, preparation method and circuit board thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101465409A (en) * | 2008-12-31 | 2009-06-24 | 电子科技大学 | Substrate for flexible organic optoelectronic device and preparation method thereof |
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| US7649060B2 (en) * | 2005-12-02 | 2010-01-19 | Henkel Corporation | Curable compositions |
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| CN101465409A (en) * | 2008-12-31 | 2009-06-24 | 电子科技大学 | Substrate for flexible organic optoelectronic device and preparation method thereof |
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