CN103881473B - A kind of color inhibition photosensitive solder resist ink and its preparation method - Google Patents
A kind of color inhibition photosensitive solder resist ink and its preparation method Download PDFInfo
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- CN103881473B CN103881473B CN201410128205.8A CN201410128205A CN103881473B CN 103881473 B CN103881473 B CN 103881473B CN 201410128205 A CN201410128205 A CN 201410128205A CN 103881473 B CN103881473 B CN 103881473B
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Abstract
The present invention relates to ink area, it is specifically related to a kind of color inhibition photosensitive solder resist ink and its preparation method. A kind of color inhibition photosensitive solder resist ink, is made up of the component of following mass fraction: ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin 50 ~ 150 parts; Reaction diluent 40 ~ 120 parts; Poly-silazane resin 5 ~ 15 parts; Epoxy resin 15 ~ 50 parts; Light-initiated dose 4 ~ 12 parts; Pigment 120 ~ 200 parts; Filler 4 ~ 10 parts; Auxiliary agent 4 ~ 10 parts. The present invention provides a kind of LED color inhibition photosensitive solder resist ink, this solder mask is compared with traditional LED photosensitive solder resist ink of domestic production, solder mask prepared by the present invention has high reflectance, excellent thermotolerance, soldering resistance, yellowing resistance, is specially adapted to LED photosensitive solder resist ink.
Description
Technical field
The present invention relates to ink area, it is specifically related to a kind of color inhibition photosensitive solder resist ink and its preparation method.
Background technology
China's LED market demand reaches 875.7 hundred million at present, and following 3 to five years, the demand of LED will constantly be increased by market. Expecting 2015, China's LED market demand will reach 1927.4 hundred million, and market scale will reach 406.7 hundred million yuan; 2013��2015 years, China's LED market annual average compound growth rate will reach 14.3%. The growth in LED market will constantly expand the demand to LED liquid photosensitive solder mask.
The substrate installing LED is also aluminium base, is a kind of metal-based copper-clad plate with good heat radiating function, and it is made up of the three-decker of uniqueness, is circuit layer (Copper Foil), insulation layer and metal-based layer respectively. Usually our said aluminium base is rigidity aluminium base, but, due to the development of LED industry, the demand of flexible aluminum based plate is got more and more, therefore, the pliability of LED photosensitive solder resist ink is required also more and more higher. Aluminium base has tow sides, one side welding LED pin, and another side presents aluminium true qualities, and the ink that the one side of welding LED pin is used is exactly LED photosensitive solder resist ink. The brightness of LED is reduced owing to solder mask plane of reflection easily deteriorates variable color. Therefore in order to brightness raising and the long lifetime of LED, it is necessary to selection has high whiteness, high reflectance and is difficult to cause the material of variable color as LED photosensitive solder resist ink.
By the development of nearly 20 years, China's domestic solder mask brand obtained certain city's field-effect in this field, had part right of speech. Up to the present, China market has the solder mask of more than 50 brand. Produce part solder mask in performance substantially close to the performance of import ink. But, domestic solder mask mainly occupies market, low and middle-end field, and market, high-end field is still occupied by foreign brand name. As: high quality LED photosensitive solder resist ink needs import Japan, Taiwan, and price is very high, seriously governs the development of domestic LED industry. At present, there is a fatal problem in the development of domestic LED photosensitive solder resist ink: core technology still rests in foreign country's staff. Especially high reflectance, the LED photosensitive solder resist ink that endurance is good, good heat resistance, pliability are good. Traditional LED photosensitive solder resist ink whiteness of current domestic production is general, and endurance, poor heat resistance, can not meet the service requirements of LED at all. Seriously govern the development of China's LED Project Technical.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of LED color inhibition photosensitive solder resist ink.
It is a further object to provide the preparation method of above-mentioned ink.
Technical problem to be solved by this invention is achieved by the following technical programs:
A kind of color inhibition photosensitive solder resist ink, is made up of the component of following mass fraction:
��-Hydroxyethyl acrylate modified melamine-formaldehyde resin 50 ~ 150 parts; Reaction diluent 40 ~ 120 parts; Poly-silazane resin 5 ~ 15 parts; Epoxy resin 15 ~ 50 parts; Light-initiated dose 4 ~ 12 parts; Pigment 120 ~ 200 parts; Filler 4 ~ 10 parts; Auxiliary agent 4 ~ 10 parts.
Described ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin is according to documentation & info recording materials, and the 5th phase in 2008, the method preparation described in 9 ~ 15 pages, the present invention no longer describes.
Further, poly-silazane resin is the DURAZANE1800 type height functional resin of An Zhi electronic material company of Britain, and described poly-silazane resin has following structure:
Wherein, R1��R2Can be H, CH3��C2H5, 20��n��30;
Further, described reaction diluent is at least one in Viscoat 295, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, double pentaerythritol methacrylate, the third oxidation tetramethylol methane tetraacrylate.
The present invention is except using modified resins and reactive diluent composite as except matrix resin, also introduce a kind of novel high functional resin organopolysilazane resin, poly-silazane resin is the polymkeric substance alternately forming basic framework by silicon and nitrogen-atoms, and side chain is with carbon-carbon double bond; The introducing of this resin, substantially improves the performance of solder mask. This resin not only has good light-cured performance, material of most of ends is had excellent sticking power, but also there is extremely strong thermotolerance (being up to 900 DEG C), excellent weathering resistance, this resin can also form fine and close polymeric film simultaneously, whole solder mask coating all being had good shade effect, effectively solves the solder mask high temperature easily yellow problem become, its coating formed has excellent weathering resistance, high thermal resistance and extremely good resistance to acids and bases.
Epoxy resin of the present invention is that the bisphenol-A liquid epoxy resin that the art is commonly used all can realize the present invention.
In the present invention, filler is at least one in aerosil, silica flour silicon-dioxide, kaolin, pure aluminium silicate, talcum powder.
Further; described light-initiated dose is 2; 4; 6-trimethyl benzoyl diphenyl base phosphine oxide, 2; 4; at least one in 6-trimethylbenzoyl ethoxyl phenenyl phosphine oxide, two (2,4,6-trimethylbenzoyl) phenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-acetone, 1-hydroxy-cyclohexyl benzophenone.
Further, described pigment is that Rutile type Titanium Dioxide, lithopone powder, ultramarine, phthalocyanine blue, phthalocyanine are green, at least one in titanium chrome green, carbon black.
Further, described auxiliary agent is at least one in defoamer and dispersion agent.
Defoamer is that the defoamer that the art is commonly used all can realize the present invention, in the present invention preferably containing organic siloxane group or the defoamer containing silicone group.
Further, described dispersion agent selects at least one in methyl amyl alcohol, oleyl amine acetate, alkyl quaternary ammonium salts, amino propylamine dioleate, quaternary amine, modification polyamino amidophosphoric acid salt.
A kind of color inhibition photosensitive solder resist ink preparation method, comprises the steps:
(1) by ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin, poly-silazane resin, pigment, light-initiated dose, dispersion agent, filler mixing, with high speed dispersor, speed is adjusted to 800 ~ 1200rpm, dispersed with stirring 20 ~ 40min, then grind 3 ~ 5 times with three-roller, obtained host;
(2) by reactive diluent, epoxy resin, the mixing of residue pigment, with high speed dispersor, speed is adjusted to 800 ~ 1200rpm, dispersed with stirring 20 ~ 40min, then grinds 3 ~ 5 times with three-roller, obtained solidifying agent;
(3) host and solidifying agent being mixed according to the ratio of 2:1 ~ 6:1, add auxiliary agent, dispersed with stirring is even, obtained photosensitive solder resist ink.
The present invention has following useful effect:
Reactive diluent used in the present invention is all have multi-functional reactive monomer, there is higher reactive behavior, the modified resin that the present invention simultaneously is used and reactive monomer resin all have good ultraviolet light polymerization performance, and solder mask prepared by the present invention has higher glossiness.
The present invention provides a kind of LED color inhibition photosensitive solder resist ink, this solder mask is compared with traditional LED photosensitive solder resist ink of domestic production, solder mask prepared by the present invention has high reflectance, excellent thermotolerance, soldering resistance, yellowing resistance, is specially adapted to LED photosensitive solder resist ink.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention, is not limitation of the invention.
Embodiment 1
150g ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin, the poly-silazane resin of 5g, 118g titanium dioxide, 5g oleyl amine acetate dispersion agent, light-initiated dose of 5gTEPO, light-initiated dose of 5g1173,10g aerosil, 2g ultramarine are mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained host.
50g Viscoat 295,50g tetramethylol methane tetraacrylate, 80g titanium dioxide, 50g epoxy resin being mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained solidifying agent.
Host being mixed according to the ratio of 6:1 with solidifying agent, add 5g silicone defoamer, dispersed with stirring is even, i.e. the LED color inhibition photosensitive solder resist ink of obtained the present invention.
Performance test methods and result are as follows:
Taking epoxy resin being the LED board material of base material in through pre-treatment by the solder mask 110 object silk screen printing of above-mentioned preparation, ink thickness is 20 ~ 30 ��m.
Prebake conditions (75 DEG C): 25min. After prebake conditions, ink is tack-free.
Exposure machine exposes: exposure energy 550mJ/cm2, levels of exposure: 11 grades.
Developing machine develops: 1%Na2CO3The aqueous solution, development 60s, development is clean.
Rear baking (150 DEG C): 60min. After rear baking, ink non yellowing.
Sticking power (GB/T9286-1998): 1 grade.
Hardness (GB/T6739-2006): 6H.
Glossiness (GB/T1743-1979): 77.
Welding resistance performance (288 DEG C of solder furnace dipping 10s, three times): ink becomes without Huang, nothing bursts, nothing comes off, non-soldering tin enters phenomenon.
Embodiment 2
100g ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin, the poly-silazane resin of 10g, 100g titanium dioxide, 3g oleyl amine acetate dispersion agent, light-initiated dose of 3gTEPO, light-initiated dose of 3g1173,6g talcum powder, 1.5g ultramarine are mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained host.
30g Viscoat 295,40g tetramethylol methane tetraacrylate, 60g titanium dioxide, 40g epoxy resin being mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained solidifying agent.
Host being mixed according to the ratio of 4:1 with solidifying agent, add 4g silicone defoamer, dispersed with stirring is even, i.e. the LED color inhibition photosensitive solder resist ink of obtained the present invention.
Performance test methods and result are as follows:
Taking epoxy resin being the LED board material of base material in through pre-treatment by the solder mask 110 object silk screen printing of above-mentioned preparation, ink thickness is 20 ~ 30 ��m.
Prebake conditions (75 DEG C): 25min. After prebake conditions, ink is tack-free.
Exposure machine exposes: exposure energy 550mJ/cm2, levels of exposure: 10 grades.
Developing machine develops: 1%Na2CO3The aqueous solution, development 60s, development is clean.
Rear baking (150 DEG C): 60min. After rear baking, ink non yellowing.
Sticking power (GB/T9286-1998): 1 grade.
Hardness (GB/T6739-2006): 6H.
Glossiness (GB/T1743-1979): 79.
Welding resistance performance (288 DEG C of solder furnace dipping 10s, three times): ink becomes without Huang, nothing bursts, nothing comes off, non-soldering tin enters phenomenon.
Embodiment 3
50g ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin, the poly-silazane resin of 15g, 79g titanium dioxide, 2g oleyl amine acetate dispersion agent, light-initiated dose of 2gTEPO, light-initiated dose of 2g1173,4g kaolin, 1g ultramarine are mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained host.
15g Viscoat 295,20g tetramethylol methane tetraacrylate, 40g titanium dioxide, 15g epoxy resin being mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained solidifying agent.
Host being mixed according to the ratio of 2:1 with solidifying agent, add 2g silicone defoamer, dispersed with stirring is even, i.e. the LED color inhibition photosensitive solder resist ink of obtained the present invention.
Performance test methods and result are as follows:
Taking epoxy resin being the LED board material of base material in through pre-treatment by the solder mask 110 object silk screen printing of above-mentioned preparation, ink thickness is 20 ~ 30 ��m.
Prebake conditions (75 DEG C): 25min. After prebake conditions, ink is tack-free.
Exposure machine exposes: exposure energy 550mJ/cm2, levels of exposure: 11 grades.
Developing machine develops: 1%Na2CO3The aqueous solution, development 60s, development is clean.
Rear baking (150 DEG C): 60min. After rear baking, ink non yellowing.
Sticking power (GB/T9286-1998): 1 grade.
Hardness (GB/T6739-2006): 7H.
Glossiness (GB/T1743-1979): 83.
Welding resistance performance (288 DEG C of solder furnace dipping 10s, three times): ink becomes without Huang, nothing bursts, nothing comes off, non-soldering tin enters phenomenon.
Embodiment 4
Green to 100g ��-Hydroxyethyl acrylate modified melamine-formaldehyde resin, the poly-silazane resin of 8g, 90g phthalocyanine, 3g oleyl amine acetate dispersion agent, light-initiated dose of 3gTEPO, light-initiated dose of 3g1173,6g talcum powder are mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained host.
Green to 30g Viscoat 295,45g tetramethylol methane tetraacrylate, 50g phthalocyanine, 40g epoxy resin being mixed, with high speed dispersor, speed is adjusted to 1100rpm, dispersed with stirring 30min, then 5 times are ground with three-roller, to fineness below 20 ��m, obtained solidifying agent.
Host being mixed according to the ratio of 3:1 with solidifying agent, add 4g silicone defoamer, dispersed with stirring is even, i.e. the LED color inhibition photosensitive solder resist ink of obtained the present invention.
Performance test methods and result are as follows:
Taking epoxy resin being the LED board material of base material in through pre-treatment by the solder mask 110 object silk screen printing of above-mentioned preparation, ink thickness is 20 ~ 30 ��m.
Prebake conditions (75 DEG C): 25min. After prebake conditions, ink is tack-free.
Exposure machine exposes: exposure energy 550mJ/cm2, levels of exposure: 10 grades.
Developing machine develops: 1%Na2CO3The aqueous solution, development 60s, development is clean.
Rear baking (150 DEG C): 60min. After rear baking, ink non yellowing.
Sticking power (GB/T9286-1998): 1 grade.
Hardness (GB/T6739-2006): 6H.
Glossiness (GB/T1743-1979): 81.
Welding resistance performance (288 DEG C of solder furnace dipping 10s, three times): ink becomes without Huang, nothing bursts, nothing comes off, non-soldering tin enters phenomenon.
The above embodiment only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to patent scope of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (5)
1. a color inhibition photosensitive solder resist ink, it is characterised in that be made up of the component of following mass fraction:
��-Hydroxyethyl acrylate modified melamine-formaldehyde resin 50��150 parts;
Reaction diluent 40��120 parts;
Poly-silazane resin 5��15 parts;
Epoxy resin 15��50 parts;
Light-initiated dose 4��12 parts;
Pigment 120��200 parts;
Filler 4��10 parts;
Auxiliary agent 4��10 parts;
Described reaction diluent is the mixture of Viscoat 295 and tetramethylol methane tetraacrylate;
Described poly-silazane resin has following structure:
Wherein, R1, R2 are H, CH3��C2H5, 20��n��30.
2. a kind of color inhibition photosensitive solder resist ink according to claim 1; it is characterized in that; described light-initiated dose is 2; 4; 6-trimethyl benzoyl diphenyl base phosphine oxide, 2,4,6-trimethylbenzoyl ethoxyl phenenyl phosphine oxide, two (2; 4,6-trimethylbenzoyl) phenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-acetone, at least one in 1-hydroxy-cyclohexyl benzophenone.
3. a kind of color inhibition photosensitive solder resist ink according to claim 1, it is characterised in that, described pigment is that Rutile type Titanium Dioxide, lithopone powder, ultramarine, phthalocyanine blue, phthalocyanine are green, at least one in titanium chrome green, carbon black.
4. a kind of color inhibition photosensitive solder resist ink according to claim 1, it is characterised in that, described auxiliary agent is at least one in defoamer and dispersion agent.
5. a kind of color inhibition photosensitive solder resist ink according to claim 4, it is characterised in that, described dispersion agent selects at least one in methyl amyl alcohol, oleyl amine acetate, amino propylamine dioleate, quaternary amine, modification polyamino amidophosphoric acid salt.
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| US9835944B2 (en) | 2014-12-10 | 2017-12-05 | Goo Chemical Co., Ltd. | Liquid solder resist composition and covered-printed wiring board |
| CN104516205B (en) * | 2014-12-20 | 2018-08-14 | 江门市阪桥电子材料有限公司 | A kind of liquid photosensitive moldeed depth color solder resist material and preparation method thereof |
| CN105199560A (en) * | 2015-10-23 | 2015-12-30 | 李沾云 | Separation device of lead block of waste storage battery |
| CN105331186B (en) * | 2015-10-23 | 2017-12-19 | 重庆智菱油墨科技有限公司 | A kind of heat resistance solder mask |
| CN105199480B (en) * | 2015-10-23 | 2019-05-17 | 永胜泰油墨(深圳)有限公司 | A kind of photocuring solder mask ink composition |
| CN109828435A (en) * | 2018-12-27 | 2019-05-31 | 江门市阪桥电子材料有限公司 | A kind of non-discolouring photosensitive white solder resist material and preparation method thereof of resistance to turmeric |
| CN109699644A (en) * | 2018-12-28 | 2019-05-03 | 东南大学苏州医疗器械研究院 | Non-releasing micro anti-biotic material and its application |
| CN110105867A (en) * | 2019-04-20 | 2019-08-09 | 无锡天杨电子有限公司 | A kind of formula and preparation method thereof of ceramic copper-clad plate high-temperature resistant welding resistance |
| CN114656833B (en) * | 2022-04-13 | 2023-02-28 | 江苏广信感光新材料股份有限公司 | Yellowing-resistant non-dry-net thermosetting ink and preparation method thereof |
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| US4975512A (en) * | 1987-08-13 | 1990-12-04 | Petroleum Energy Center | Reformed polysilazane and method of producing same |
| JP2010241976A (en) * | 2009-04-07 | 2010-10-28 | Seiko Epson Corp | Method for producing water-repellent treated aluminum pigment dispersion, water-repellent treated aluminum pigment, and aqueous ink composition containing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102286228A (en) * | 2011-06-20 | 2011-12-21 | 无锡广信感光科技有限公司 | Preparation method of high temperature resistant non-halogen fire resistant ultraviolet curing solder resist ink |
| CN103642318A (en) * | 2013-12-20 | 2014-03-19 | 何彦萱 | Boiling-resistant UV (Ultraviolet) curing jet-ink for non-absorbent substrate and preparation method of jet-ink |
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