WO2017020462A1 - 一种覆铜板用环氧树脂组合物及其应用 - Google Patents
一种覆铜板用环氧树脂组合物及其应用 Download PDFInfo
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- WO2017020462A1 WO2017020462A1 PCT/CN2015/096517 CN2015096517W WO2017020462A1 WO 2017020462 A1 WO2017020462 A1 WO 2017020462A1 CN 2015096517 W CN2015096517 W CN 2015096517W WO 2017020462 A1 WO2017020462 A1 WO 2017020462A1
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- epoxy resin
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- C08K2003/3045—Sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/01—Dielectrics
- H05K2201/0104—Properties and characteristics in general
- H05K2201/012—Flame-retardant; Preventing of inflammation
Definitions
- the present invention relates to the field of laminate technology, and in particular to an epoxy resin composition, and more particularly to an epoxy resin composition for a copper clad laminate and a prepreg, a laminate and a printed circuit board produced therefrom.
- bromine flame retardant Most of the traditional FR4 uses bromine flame retardant. Bromine has high flame retardant efficiency, and flame retardant materials such as tetrabromobisphenol A are inexpensive and easy to promote. However, if only bromine is flame retardant, the total bromine content in ordinary FR4 generally reaches 15% (the bromine content accounts for the mass ratio of the organic solids in the sheet) to reach the UL94V-0 level.
- the higher bromine content is not only environmentally friendly, but also because the C-Br bond is easily broken, which also causes the heat resistance of the material itself to be seriously degraded; and the organic matter with high bromine content is not conducive to high temperature, high pressure, humidity and easily polluted environment.
- phosphorus flame retardant can also achieve the purpose of flame retardant, because the phosphorus flame retardant system does not contain bromine, so the heat resistance is much better than the bromine flame retardant system.
- the phosphorus element is easy to absorb moisture, and the moisture absorption rate of the flame retardant plate is high, which is not conducive to the stability of the electrical properties of the plate; and the current price of the phosphorus-based flame retardant is generally high, and the cost pressure is large, so although The call for halogen-free is high, but it is not possible to abandon bromine flame retardation for cost reasons.
- Chinese patent CN102093670A discloses a method for achieving flame retardancy using a phosphorus-containing phenolic aldehyde containing a 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) structure, although the water absorption rate of DOPO is It is lower than phosphate, but because of its large amount, the phosphorus content is also above 2%, so the moisture absorption rate is not improved.
- DOPO 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide
- the bromine flame retardant system has a high bromine content, usually up to 15% to achieve flame retardancy, but higher bromine content leads to poor heat resistance and relative leakage.
- the tracking index (CTI) is also difficult to reach 600V.
- the use of phosphorus flame retardant has the disadvantage of increasing the moisture absorption rate due to the high phosphorus content.
- CN101892027 and CN101808466 disclose the sharing of bromine and phosphorus, but due to the use of a large amount of nitrile rubber, the acrylonitrile structure has a higher water absorption rate than the epoxy resin, and the voltage resistance of the composite substrate is lowered, and in addition, the nitrile rubber is used.
- the acrylonitrile structure accelerates the decomposition of bromine, which is detrimental to the CTI performance of the bromine-containing system.
- the present invention adopts the following technical solutions:
- the present invention provides an epoxy resin composition
- an epoxy resin composition comprising, by weight of the organic solids, the following components:
- the bromine content is 5 to 12% of the sum of the weights of the organic solids in the composition; and the phosphorus content is 0.2 to 1.5 of the sum of the weights of the organic solids in the composition. %.
- the invention adopts the method of simultaneously adding phosphorus-containing phenolic aldehyde and brominated bisphenol A in the manner of introducing the flame-retardant element, and adjusting the amount of the two, so that the bromine content is 5%-12%, and the phosphorus content is 0.2%-1.5%. It not only achieves UL94 V-0 flame retardancy, but also has higher heat resistance and higher CTI value than CCL with flame retardant bromine-containing epoxy resin. >600V), compared with the copper-clad board which is flame retardant with phosphorus-containing flame retardant alone, the moisture absorption rate is lower and the dipping resistance time is longer.
- the bromine element and the phosphorus element are preferably derived from the phosphorus-containing phenolic aldehyde and bromine.
- Bisphenol A is a phosphorus-containing phenolic aldehyde and bromine.
- the invention adopts the combination of brominated bisphenol A as a source of bromine element and a phosphorus-containing phenolic aldehyde which provides phosphorus element, and the two can form a cross-linked interpenetrating network, thereby better synergistic effect, which requires only a low content.
- the bromine and phosphorus elements can achieve the flame retardancy of the substrate to UL94 V-0, and further reduce the water absorption of the substrate, high CTI, and good adhesion, processability and process operability. It reduces the dependence of flame retardant on bromine and is therefore more environmentally friendly.
- the epoxy resin is 50-100 parts by weight, and may be, for example, 50 parts by weight, 55 parts by weight, 60 parts by weight, 65 parts by weight, 70 parts by weight, 75 parts by weight, 80 parts by weight, and 85 parts by weight. Parts, 90 parts by weight, 95 parts by weight, 100 parts by weight.
- the phosphorus-containing phenolic aldehyde is 2-30 parts by weight, and may be, for example, 2 parts by weight, 5 parts by weight, 8 parts by weight, 10 parts by weight, 12 parts by weight, 15 parts by weight, 18 parts by weight, 20 parts by weight. Parts, 22 parts by weight, 25 parts by weight, 28 parts by weight, 30 parts by weight.
- the brominated bisphenol A is 1 to 40 parts by weight, and may be, for example, 1 part by weight, 2 parts by weight, 5 parts by weight, 8 parts by weight, 10 parts by weight, 12 parts by weight, 15 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 25 parts by weight, 28 parts by weight, 30 parts by weight, 32 parts by weight, 35 parts by weight, 38 parts by weight, and 40 parts by weight.
- the other curing agent is 10 to 60 parts by weight, for example, 10 parts by weight, 12 Parts by weight, 15 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 25 parts by weight, 28 parts by weight, 30 parts by weight, 32 parts by weight, 35 parts by weight, 38 parts by weight, 40 parts by weight, 42 parts by weight 45 parts by weight, 48 parts by weight, 50 parts by weight, 52 parts by weight, 55 parts by weight, 58 parts by weight, and 60 parts by weight.
- the curing accelerator is 0.05-1.0 parts by weight, for example, 0.05 parts by weight, 0.08 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight. Parts, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight, 1.0 parts by weight.
- the epoxy resin composition has a bromine content of 5-12% by weight of the organic solids in the composition, and may be, for example, 5%, 5.5%, 6%, 6.5%, or 7. %, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, preferably 5-10%, further preferably 5-8%.
- the epoxy resin composition has a phosphorus content of 0.2 to 1.5% by weight of the total of the organic solids in the composition, and may be, for example, 0.2%, 0.3%, 0.4%, 0.5%, 0.6. %, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, preferably 0.5-1.5%, further preferably 0.8-1.5%.
- the phosphorus-containing phenolic aldehyde is a phosphorus-containing phenanthrene-type compound, preferably a phenolic resin corresponding to dihydro-9-oxy-10-phosphaphenanthrene.
- the phosphorus-containing phenolic aldehyde is at least one of the following phenolic resins:
- the brominated bisphenol A has the following chemical structural formula:
- R 1 -R 4 is a Br atom
- R 1 -R 4 when R 1 -R 4 is not a Br atom, it is a H atom, for example, R 1 is a Br atom, R 1 - R 3 is a H atom, or R 1 and R 2 are a Br atom, R 3 - R 4 are a H atom and the like.
- the epoxy resin is bisphenol A epoxy resin, o-cresol novolac epoxy resin, bisphenol A novolac epoxy resin, phenol epoxy resin, dicyclopentadiene epoxy resin Resin, MDI epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, bisphenol F epoxy resin, tetrafunctional epoxy resin, naphthalene epoxy resin or biphenyl epoxy resin Any one or a mixture of at least two.
- the other curing agent is a mixture of any one or at least two of a phenol resin, an aromatic diamine curing agent, dicyandiamide, an aliphatic amine, an acid anhydride, an active polyester or a cyanate.
- the phenolic resin is a phenol type phenol resin, a bisphenol A type phenol resin, an o-cresol novolac resin, a trisphenol novolak resin, a naphthalene type phenol resin, a biphenyl type phenol resin or a dicyclopentadiene phenol resin. Any one or a mixture of at least two.
- the aromatic diamine curing agent has the following chemical structural formula:
- R 3 and R 4 are H, -CH 3 or -C 2 H 5
- R 2 is H, -CH 3 or -C 2 H 5 .
- the curing accelerator is any one or a mixture of at least two of an imidazole curing accelerator, an organic phosphine curing accelerator, or a tertiary amine curing accelerator.
- the imidazole curing accelerator is 2-methylimidazole, 2-methyl-4-ethylimidazole, 2- Any one or a mixture of at least two of undecylimidazole, 2-phenylimidazole or 1-cyanoethyl-2-ethyl-4-methylimidazole.
- the organophosphine curing accelerator is tributylphosphine and/or triphenylphosphine.
- the tertiary amine curing accelerator is benzyldimethylamine.
- the amount of the curing accelerator added is not excessive, and the reaction is rapid when the amount is too large, which is disadvantageous for the process operation and storage of the material.
- the epoxy resin composition further contains a filler, preferably an inorganic filler.
- the filler is boehmite, aluminum hydroxide, barium sulfate, calcium fluoride, magnesium hydroxide, silica, glass powder, kaolin, talc, mica powder, alumina, zinc oxide, magnesium oxide. Any one or a mixture of at least two of boron nitride, aluminum nitride or calcium carbonate.
- the filler has an average particle diameter of from 0.3 to 20 ⁇ m.
- the content of the filler is from 1 to 200 parts by weight, for example, 1 part by weight, 5 parts by weight, based on 100 parts by weight of the total of the organic solids of the components in the epoxy resin composition. 10 parts by weight, 20 parts by weight, 30 parts by weight, 50 parts by weight, 60 parts by weight, 80 parts by weight, 100 parts by weight, 120 parts by weight, 140 parts by weight, 150 parts by weight, 180 parts by weight, 200 parts by weight, preferably 50-100 parts by weight.
- the relative tracking index (CTI) of the substrate can be further increased, and the leakage tracking index (CTI) of the substrate can be made 600 V or more.
- the epoxy resin composition may also be appropriately added with an auxiliary agent, and the auxiliary agent used is an aminosilane coupling agent.
- an epoxy silane coupling agent such a coupling agent is free from heavy metals and has no adverse effect on human health, and is used in an amount of 0.5 to 2% by weight of the inorganic filler.
- the epoxy resin composition further contains a solvent, preferably an organic solvent.
- the solvent is any one or at least two of N,N'-dimethylformamide, ethylene glycol ethyl ether, propylene glycol methyl ether, acetone, methyl ethyl ketone, methanol, ethanol, benzene or toluene. mixing.
- the viscosity can be adjusted using a solvent, and by using the above solvent, the solid component content in the epoxy resin composition can be adjusted to 40 to 80%.
- the present invention provides a prepreg produced using the epoxy resin composition according to the first aspect of the invention, comprising a base material; and an epoxy resin adhered thereto by dipping and drying combination.
- the matrix material is a nonwoven or woven fiberglass cloth.
- the present invention also provides a laminate comprising the prepreg according to the second aspect of the invention.
- the invention provides a printed circuit board comprising the laminate of the third aspect of the invention.
- the present invention has the following beneficial effects:
- the epoxy resin composition of the present invention uses brominated bisphenol A and phosphorus-containing phenolic as a source of bromine and phosphorus, respectively, and combines a specific ratio of phosphorus to bromine, thereby effectively controlling cost while not only hindering
- the flammability is up to UL94 V-0, and the material's comparative tracking index (CTI) is improved, reaching CTI > 600V.
- the epoxy resin composition of the present invention has better heat resistance than the pure bromine flame retardant system, and has a lower moisture absorption rate than the pure phosphorus flame retardant system, that is, the pure bromine is solved.
- the flame retardant heat resistance is poor and the pure phosphorus flame retardant moisture absorption rate is high, and the comprehensive performance is excellent.
- the present invention can further reduce the dependence of the flame retardant on the bromine element, thereby making it more environmentally friendly.
- the epoxy resin, the phosphorus-containing phenolic aldehyde, the brominated bisphenol A, the other curing agent, the filler and the curing accelerator are mixed with an organic solvent, uniformly mixed by a stirring and dispersing device, and the epoxy resin composition is pre-prepared. It is immersed in a non-woven or woven glass fiber cloth and dried in a gluing machine (120-180 ° C) to prepare a prepreg for a printed circuit board in a semi-cured state.
- the prepreg is laminated several times, and the copper foil is laminated on one side or both sides of the laminate, and then placed on a 120-200 ° C laminator, and hot-pressed to form a printed circuit board.
- a copper clad laminate; the copper foil may also be replaced with an aluminum foil, a silver foil or a stainless steel foil.
- the glass transition temperature, the tracking tracking index (CTI), the flame retardancy, the dipping time, the PCT water absorption rate, the 5% thermal weight loss and the drilling process were tested.
- the properties and the like are further described and described as in the following Examples 1-4 and Comparative Examples 1-7.
- the measurement was carried out according to the DSC method specified in IPC-TM-650 2.4.25 according to differential scanning calorimetry (DSC).
- a double-sided copper foil sheet having a size of 100 ⁇ 100 mm was immersed in a solder bath heated to 288 ° C, and the time from the immersion to the occurrence of the delamination of the sheet was calculated.
- the pre-dried sample was weighed and then placed in an autoclave for 4 hours to see the rate of change in mass.
- the temperature was raised to 500 ° C in a nitrogen atmosphere at a heating rate of 5 ° C / min, and the temperature at which the sample mass loss was 5% was recorded.
- the two plates with a thickness of 1.6mm are stacked together, drilled with a 0.3mm drill bit, the drilling speed is 110krpm, the falling speed is 33mm/s, and 5000 holes are continuously drilled. Whenever the 1000 holes, the tip wear of the drill bit is observed. The size of the wear determines the processability of the drill.
- Comparative Example 6 Synthetic rubber (commercial brand No. Nipol 1072CGX, produced by ZEON Corporation, USA) 23 parts by weight, brominated epoxy (manufactured by DER530A80, manufactured by DOW), 25 parts by weight, high bromine epoxy (commercial brand number EPICLON 153-60M, Large Japanese ink production) 21 parts by weight, biphenyl epoxy (NC3000H, manufactured by Nippon Kayaku Co., Ltd.) 25 parts by weight, 2E4MI (produced by Japan Shikoku Chemicals Co., Ltd.) 0.2 parts by weight, aromatic diamine 4,4-DDS (produced by Taiwan Hygiene) 10.1 Parts by weight, phenoxyphosphazene (SPB-100, phosphorus content 13.4%, produced by Yabao, USA) 20 parts by weight, aluminum hydroxide (manufactured by Yabao, USA) 15 parts by weight, boehmite ( ⁇ ) Company) 31 parts by weight, barium sulfate (Guizhou Red Star Co.,
- Comparative Example 7 33 parts by weight of a nitrile rubber-modified epoxy (SC-024, manufactured by SHIN-A), 67 parts by weight of a brominated epoxy resin (DEBR 530A80, manufactured by The Dow Chemical Co., Ltd.), 3 parts of dicyandiamide, 2 - 0.02 parts of methylimidazole, 6 parts by weight of tetrabromobisphenol A, 31 parts by weight of phosphorus phenolic aldehyde (LC950, produced by SHIN-A), 17 parts by weight of aluminum hydroxide (manufactured by Yabao, USA), boehmite Source quartz material Co., Ltd.) 34 parts by weight, barium sulfate (Guizhou Red Star Co., Ltd.) 9 parts by weight, solvent MEK adjusted solid content to 66%.
- SC-024, manufactured by SHIN-A 67 parts by weight of a brominated epoxy resin
- DEBR 530A80 brominated epoxy resin
- LC950 phosphorus
- Example 1-4 Compared with Comparative Example 3, the PCT water absorption rate of Example 1-4 is superior to that of Comparative Example 3, since only phosphorus-containing phenolic aldehyde is used in Comparative Example 3, and its phosphorus content is as high as 2.5%, so that its moisture absorption is increased. And Examples 1-4 use both phosphorus-containing phenolic and brominated bisphenol A, which can achieve low moisture absorption at a phosphorus content of only 0.2% to 1.5%, indicating the use of phosphorus-containing phenolic aldehydes and brominated bisphenols. After the A compounding technique, the substrate can achieve low water absorption.
- Example 2-4 phosphorus-bromine synergistic flame-retardant requires only 10% or less of bromine to achieve flame retardant UL94 V-0, while Comparative Example 2 only introduces bromine resistance. Although the bromine content reached 9.5%, it still could not reach the UL94 V-0 level of flame retardant.
- Example 1 Compared with Comparative Example 1, Examples 1-4 were similarly used due to the phosphorus-bromine synergistic flame retardant route. In the case of the flame retardant UL94 V-0 grade, only 12% or less of bromine element is required, so that Examples 1-4 have higher chemical heat resistance than Comparative Example 1, that is, 5% weight loss temperature ratio is compared. In Example 1, it is higher than 9 ° C and the dipping time is longer.
- Comparative Example 6 and Comparative Example 7 The resin compositions invented by the patents CN 101808466A and CN 101892027A, respectively, have failed to reach CTI 600V under the same bromine content and phosphorus content as in the present invention and the same filler system. And the water absorption rate is remarkably higher than the present invention, and the pressure resistance of the present invention is superior.
- the epoxy resin composition of the present invention has a much higher heat resistance than the pure bromine flame retardant system, and the CTI is above 600 V after adding a filler such as boehmite; compared to pure phosphorus
- the flame retardant system has lower water absorption rate, good drilling processability and good flame retardancy.
- the prepreg and the copper clad laminate prepared by using the above epoxy resin composition have excellent CTI characteristics, so that the PCB can obviously improve the adaptability of the PCB in a harsh environment; at the same time, the relatively high heat resistance and the long dipping time can be Suitable for the needs of lead-free soldering. And the invention can further reduce the dependence of the flame retardant on the bromine element, thereby making it more environmentally friendly.
- the present invention illustrates the process of the present invention by the above-described embodiments, but the present invention is not limited to the above process steps, that is, it does not mean that the present invention must rely on the above process steps to be implemented. It will be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of the materials selected for the present invention, and the addition of the auxiliary ingredients, the selection of the specific means, etc., are all within the scope of the present invention.
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Abstract
Description
Claims (10)
- 一种环氧树脂组合物,其特征在于,以有机固形物重量份计,包括如下组分:(A)环氧树脂:50-100重量份;(B)含磷酚醛:2-30重量份;(C)溴化双酚A:1-40重量份;(D)其他固化剂:10-60重量份;(E)固化促进剂:0.05-1.0重量份;其中,所述的环氧树脂组合物中,溴含量占所述组合物中有机固形物重量之和的5-12%;磷含量占所述组合物中有机固形物重量之和的0.2-1.5%。
- 如权利要求1所述的环氧树脂组合物,其特征在于,所述的环氧树脂组合物中,溴含量占所述组合物中有机固形物重量之和的5-10%,优选为5-8%;磷含量占所述组合物中有机固形物重量之和的0.5-1.5%,优选为0.8-1.5%。
- 如权利要求1-4任一项所述的环氧树脂组合物,其特征在于,所述的环氧树脂为双酚A型环氧树脂、邻甲酚型酚醛环氧树脂、双酚A型酚醛环氧树脂、苯酚型环氧树脂、双环戊二烯型环氧树脂、MDI环氧树脂、双酚F型环氧树脂、双酚S型环氧树脂、双酚F型环氧树脂、四官能环氧树脂、萘型环氧树脂或联苯型环氧树脂中的任意一种或至少两种的混合。
- 如权利要求1-5任一项所述的环氧树脂组合物,其特征在于,所述的其他固化剂为酚醛树脂、芳香二胺类固化剂、双氰胺、脂肪族胺、酸酐、活性聚酯或氰酸酯中的任意一种或至少两种的混合;优选地,所述的酚醛树脂为苯酚型酚醛树脂、双酚A型酚醛树脂、邻甲酚酚醛树脂、三酚酚醛树脂、萘型酚醛树脂、联苯型酚醛树脂或双环戊二烯酚醛树脂中的任意一种或至少两种的混合;优选地,所述的芳香二胺类固化剂具有如下化学结构式:优选地,所述的固化促进剂为咪唑类固化促进剂、有机膦固化促进剂或三级胺固化促进剂中的任意一种或至少两种的混合;优选地,所述的咪唑类固化促进剂为2-甲基咪唑、2-甲基-4-乙基咪唑、2-十一烷基咪唑、2-苯基咪唑或1-氰乙基-2-乙基-4-甲基咪唑中的任意一种或至少两种的混合;优选地,所述的有机膦固化促进剂为三丁基膦和/或三苯基膦;优选地,所述的三级胺固化促进剂为苄基二甲基胺。
- 如权利要求1-6任一项所述的环氧树脂组合物,其特征在于,所述的环氧树脂组合物还含有填料,优选为无机填料;优选地,所述的填料为勃姆石、氢氧化铝、硫酸钡、氟化钙、氢氧化镁、二氧化硅、玻璃粉、高岭土、滑石粉、云母粉、氧化铝、氧化锌、氧化镁、氮 化硼、氮化铝或碳酸钙中的任意一种或至少两种的混合;优选地,所述填料的平均粒径为0.3-20μm;优选地,按所述环氧树脂组合物中各组分的有机固形物之和为100重量份计,所述填料的含量为1-200重量份,优选为50-100重量份;优选地,所述的环氧树脂组合物还含有溶剂,优选为有机溶剂;优选地,所述的溶剂为N,N’-二甲基甲酰胺、乙二醇***、丙二醇甲醚、丙酮、丁酮、甲醇、乙醇、苯或甲苯中的任意一种或至少两种的混合。
- 一种使用如权利要求1-7任一项所述的环氧树脂组合物制作的预浸料,其特征在于,其包括基体材料;和通过浸渍干燥后附着在其上的环氧树脂组合物;优选地,所述的基体材料为无纺或有纺玻璃纤维布。
- 一种层压板,其特征在于,其包含如权利要求8所述的预浸料。
- 一种印刷电路板,其特征在于,其包含如权利要求9所述的层压板。
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CN107383776A (zh) * | 2016-05-16 | 2017-11-24 | 广东广山新材料股份有限公司 | 一种溴磷协效阻燃树脂组合物、热固性树脂组合物、预浸板及复合金属基板 |
CN107383774A (zh) * | 2016-05-16 | 2017-11-24 | 广东广山新材料股份有限公司 | 一种溴硫协效阻燃树脂组合物、热固性树脂组合物、预浸板及复合金属基板 |
CN107383775A (zh) * | 2016-05-16 | 2017-11-24 | 广东广山新材料股份有限公司 | 一种溴磷硫协效阻燃树脂组合物、热固性树脂组合物、预浸板及复合金属基板 |
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US20180201761A1 (en) | 2018-07-19 |
CN105175995B (zh) | 2018-05-04 |
CN105175995A (zh) | 2015-12-23 |
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