CN104151777A - Thermosetting resin composition - Google Patents
Thermosetting resin composition Download PDFInfo
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- CN104151777A CN104151777A CN201410387041.0A CN201410387041A CN104151777A CN 104151777 A CN104151777 A CN 104151777A CN 201410387041 A CN201410387041 A CN 201410387041A CN 104151777 A CN104151777 A CN 104151777A
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Abstract
The invention relates to a thermosetting resin composition which comprises the following components by mass percent: 20%-70% of thermosetting resin, 1%-30% of a curing agent, 0%-10% of an accelerator and 1%-70% of high comparative tracking index (CTI) filler with average particle size of 0.5-15 microns. The invention further relates to a copper-clad plate prepared from the thermosetting resin composition. A composite material prepared from the thermosetting resin composition can have high CTI, the highest CTI of the copper-clad plate prepared from the thermosetting resin composition can reach more than 600 V, and meanwhile, the alkali resistance of plates cannot be influenced. Therefore, the thermosetting resin composition has important economic meaning.
Description
Technical field
The present invention relates to copper-clad plate technical field, be specifically related to a kind of resin combination, relate in particular to a kind of compositions of thermosetting resin and utilize the copper-clad plate of its making.
Background technology
Along with electronics is towards light, thin, short and small and multifunctional direction development, as the tellite of electronic components main support, also constantly move towards thin type, miniaturization and densification; Along with the densification of circuit, requirements at the higher level, particularly environmental facies can be proposed to all the more so under severe condition to the insulating reliability between circuit.
When the insulating substrate surface of circuit card is subject to the pollution of dust, moisture, dewfall or moisture erosion and ionic contamination, under impressed voltage effect, because its surperficial leakage current will increase greatly than clean surface, the moist pollutent of heat of vaporization that leakage current produces, the surface of insulating substrate is played pendulum, easily produce spark, insulativity is reduced, can puncture short when serious or open circuit.
Common epoxy resin copper-clad plate, its relative anti creepage trace index is lower, is generally difficult to reach 240V, therefore, improving phase ratio creepage tracking index (CTI, Comparative Tracking Index) has become the emphasis direction of electronic technology field research and development.
CN101578010A discloses a kind of high phase ratio electric leakage resistant tracking index leadless compatible CEM-3 copper-clad laminate preparation method, and it adopts filling aluminium hydrate to prepare high CTI CEM-3 plate.Although aluminium hydroxide has higher CTI, aluminium hydroxide chemical resistant properties is not good, while adding too high levels, can in the processing of PCB, occur the defect that chemical resistant properties is bad.
CN102093670A discloses a kind of method that adopts barium sulfate to prepare high CTI copper-clad plate.But in the method, barium sulfate is than great, and in veneer sheet glue, easily sedimentation, has increased veneer sheet manufacture difficulty.
Therefore, how to produce a kind of high phase ratio creepage tracking index (CTI), ensure that the copper-clad plate that its chemical resistant properties is good is problem demanding prompt solution simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of resin combination, particularly a kind of compositions of thermosetting resin and utilize said composition make copper-clad plate.
For reaching this goal of the invention, the present invention by the following technical solutions:
First aspect, the invention provides a kind of compositions of thermosetting resin, said composition comprise component and weight percent as follows: thermosetting resin 20-70 quality %, solidifying agent 1-30 quality %, promotor 0-10 quality %, high CTI filler 1-70 quality %; Described high CTI filler at least comprises Calcium Fluoride (Fluorspan).
As optimal technical scheme, described high CTI filler is through surface treatment.
Preferably, described surface treatment is used tensio-active agent processing.
Preferably, described tensio-active agent is the mixture of cationic, anionic, both sexes or neutral surface active agent's any one or at least two kinds.
Preferably, described tensio-active agent is the mixture of any one or at least two kinds of silane coupling agent, titanate ester treatment agent, aluminate, zirconate, stearic acid, oleic acid, lauric acid and their metallic salt, resol, organic silicone oil or polyoxyethylene glycol.
As optimal technical scheme, described high CTI filler, except comprising Calcium Fluoride (Fluorspan), can also be selected from the mixture of any one or at least two kinds of aluminium hydroxide, barium sulfate, barium titanate, strontium titanate, talcum powder or titanium dioxide.
Preferably, the median size of described Calcium Fluoride (Fluorspan) is 0.5-15 μ m, is preferably 1-10 μ m, more preferably 1-5 μ m.
Preferably, described Calcium Fluoride Content is 1-70 quality %, is preferably 5-50 quality %, more preferably 10-40 quality %.
As optimal technical scheme, described thermosetting resin is the mixture of any one or at least two kinds of epoxy resin, cyanate, bismaleimides, polyimide or polybutadiene.
The present invention adds the phase ratio creepage tracking index (CTI) that Calcium Fluoride (Fluorspan) improves substrate, has been applicable to halogen system or Halogen system, can have significant effect.
Preferably, described thermosetting resin is that number-average molecular weight is the mixture of any one or at least two kinds of bisphenol A epoxide resin, aliphatic epoxy resin or the cycloaliphatic epoxy resin of 500-4000.
As optimal technical scheme, described solidifying agent is amine and/or anhydrides.
Preferably, described solidifying agent is the mixture of any one or at least two kinds of Dyhard RU 100, diaminodiphenylsulfone(DDS) or two amido ditanes.
As optimal technical scheme, resin combination of the present invention also comprises fire retardant.
Preferably, described fire retardant is compound in triazine class and/or trimeric cyanamide and salt thereof.
The present invention can also add non-high CTI filler, such as silicon-dioxide etc.
Second aspect, the present invention also provides a kind of veneer sheet that adopts compositions of thermosetting resin of the present invention to make, and it comprises prepreg.
Preferably, described prepreg comprises that strongthener core is by impregnation drying postadhesion compositions of thermosetting resin of the present invention thereon.
As optimal technical scheme, described strongthener is the mixture of any one or at least two kinds of natural fiber, organic synthetic fibers, organic fabric or inorganic fibre.
The third aspect, the present invention further provides the method for a kind of raising veneer sheet phase ratio creepage tracking index (CTI), and the method adopts compositions of thermosetting resin of the present invention.
Preferably, described compositions of thermosetting resin comprises high CTI filler, and described high CTI filler at least comprises Calcium Fluoride (Fluorspan).
The present invention adopts direct interpolation Calcium Fluoride (Fluorspan) to improve the phase ratio creepage tracking index of substrate (CTI), successful, and side effect is little.Calcium is with the fluorochemical of gang, and as beryllium fluoride, magnesium fluoride, strontium fluoride and barium fluoride have toxicity, are not suitable for the application of electronic product; Fluorine, with the halogenide of gang, as calcium chloride, Calcium Bromide, calcium iodide and astatine calcium water soluble, discharges ion, can affect the insulativity of electronic material, is not suitable for equally applying in electronic material.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention adopts the filler of direct interpolation high phase ratio creepage tracking index can improve the phase ratio creepage tracking index of copper-clad plate, can make more than its CTI value reaches 300V, wherein, while adopting separately Calcium Fluoride (Fluorspan) filler, can make CTI value reach maximum value, more than realizing 600V.
(2) the present invention adds separately after the filler Calcium Fluoride (Fluorspan) of high phase ratio creepage tracking index, solve filling aluminium hydrate alkali resistance poor, the problem of barium sulfate free settling, prepared copper-clad plate alkali resistance strengthens, at 10%NaOH, at 80 DEG C two hours, all, without the appearance of white point, finally obtain the copper-clad plate of excellent combination property.
(3) the present invention adopts the high CTI filler of Calcium Fluoride (Fluorspan) and other to mix while use, reach identical CTI, can reduce the consumption of other high CTI filler, improve some problems that the interpolation of other filler brings, for example improve filling aluminium hydrate alkali resistance poor, the problem of barium sulfate free settling, has finally obtained the copper-clad plate of excellent combination property.
Embodiment
Further illustrate technical scheme of the present invention below by embodiment.
Those skilled in the art should understand, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Each code name and composition thereof used in embodiment and comparative example are as follows:
Thermosetting resin A: represent the epoxy resin that LG-DOW is produced, commodity are called DER530, its epoxy equivalent (weight) 435g/eq, bromine content is 19wt%.
Thermosetting resin B: represent the novolac epoxy that Hexion Specialty Chemicals company (Bowden chemical company of the former U.S. and German Berlet company) produces, commodity are called EPR627-MEK80, and its epoxy equivalent (weight) is between 160～250g/eq.
Solidifying agent is Dyhard RU 100, and Ningxia Daiei is produced.
Promotor represents that Japanese four countries change into the 2MI that company produces.
Filler A represents Calcium Fluoride (Fluorspan), and median size is 3 μ m.
Filler B represents the aluminium hydroxide of SUMITOMO CHEMICAL, and commodity are called C-302A, and median size is 2-3 μ m.
Filler C represents the barium sulfate of Guizhou Red Star, and commodity are called BM/E.
Filler D represents the barium titanate of Shandong state porcelain, and commodity are called BT-300.
Filler E represents the strontium titanate that Shanghai allusion quotation is raised, and commodity are called strontium titanate.
Embodiment 1-8
Embodiment 1-8 solids component formula composition refers to table 1, wherein, embodiment 1 has added the Calcium Fluoride (Fluorspan) of 10g, and embodiment 2 has added the Calcium Fluoride (Fluorspan) of 50g, the barium sulfate of 50g, embodiment 3 has added the Calcium Fluoride (Fluorspan) of 100g and the barium sulfate of 50g, embodiment 4 has added 150g Calcium Fluoride (Fluorspan), and embodiment 5 has added 50g Calcium Fluoride (Fluorspan) and 50g barium titanate, and embodiment 6 has added 50g Calcium Fluoride (Fluorspan) and 50g strontium titanate, embodiment 7 has added the Calcium Fluoride (Fluorspan) of 50 g, and embodiment 8 has added the Calcium Fluoride (Fluorspan) of 100g.
Utilize butanone to be modulated into and manufacture the thermosetting epoxy resin varnish that veneer sheet uses, wherein solids component accounts for 65%.
Copper clad foil substrate according to following preparation technology's Preparation Example 1-8:
(1) glue: solvent is added in proportion container, add respectively the solution of thermosetting resin, curing agent solution and promotor when stirring; Stir after 2 hours, add filler, continue to stir after 4-8 hour, the gel time (170 DEG C of constant temperature hot plates) of sampling and testing glue is 200～300 seconds.
(2) impregnation: by the layers of reinforcement of soaking glue by vertical or horizontal type impregnation machine, push the conditions such as wheel speed, linear speed, wind-warm syndrome and furnace temperature by control, specifically taking vertical impregnation machine demonstration example as: extruding wheel speed :-1.3～-2.5 ± 0.1M/min; Main line speed: 4～18m/min; Wind-warm syndrome: 120～170 DEG C; Furnace temperature: 130～220 DEG C, make prepreg by above condition.
(3) compacting: after the prepreg of having reduced and Copper Foil are combined, put into vacuum hotpressing machine, by certain temperature, time and pressure also finally make copper coated foil plate, and specifically demonstration example is:
Temperature formula: 130 DEG C/30min+155 DEG C/30min+190 DEG C/90min+220 DEG C/60min;
Pressure formula: 25Kgf.cm
-2/ 30min+50Kgf.cm
-2/ 30min+90Kgf.cm
-2/ 120min+30Kgf.cm
-2/ 90min;
Vacuum formula: 30mmHg/130min+800mmHg/130min.
By said procedure, adopt layer of prepreg that 8 thickness are 0.2mm to be stacked between the thick Copper Foil of 35 μ m, after hot pressing, can make the veneer sheet that 1.6mm is thick.Obtain, after copper coated foil plate, plate property being tested, table 2 is depicted as copper clad foil substrate performance comparison.
Comparative example 1-3
Comparative example 1-3 solids component formula composition refers to table 1, and wherein, comparative example 1 does not add filler, and comparative example 2 has added 100g barium sulfate, and comparative example 3 has added 100g aluminium hydroxide.
Utilize butanone to be modulated into and manufacture the thermosetting resin glue that veneer sheet uses, wherein solids component accounts for 65%.The preparation method of comparative example 1-3 is as embodiment 1-8.
Table 1
Adopt the copper clad foil substrate that following methods is prepared embodiment 1-8 and comparative example 1-3 to measure phase ratio creepage tracking index and alkali resistance, test result is as shown in table 2.
Table 2
As shown in Table 2, for the CTI value of copper clad foil substrate, the CTI value of embodiment 1-8 is all higher than comparative example 1-2, the CTI value of embodiment 5-7 is identical with embodiment 3, and embodiment 3-4 and 8 CTI value are all higher than embodiment 3, wherein, the CTI value of embodiment 4 is the highest, more than reaching 600V; For the alkali resistance of copper clad foil substrate, after tested, all without the generation of white point, and there is white point in comparative example 3 to embodiment 1-8.
From embodiment 1-8 and comparative example 1-3 can find out following some:
(1) embodiment 1,4,7 is with 8 compared with comparative example 1, and it is high that CTI value is obviously wanted, and the interpolation due to Calcium Fluoride (Fluorspan) filler is described, improved the CTI value of copper clad foil substrate;
(2) embodiment 2 is compared with comparative example 2, although equally all added 100g filler, but it is high that the CTI value of embodiment 2 is wanted, illustrate that the selected Calcium Fluoride (Fluorspan) of the present invention and barium sulfate collocation are used higher than the CTI value of the copper clad foil substrate that uses separately barium sulfate filler to prepare;
(3) embodiment 8 is compared with comparative example 3, and CTI value obviously increases, and alkali resistance strengthens, and illustrates that selected Calcium Fluoride (Fluorspan) can corresponding raising its CTI value and alkali resistance;
(4) embodiment 3 compares with embodiment 4, has equally all added 150g filler, but in the time that filler is all Calcium Fluoride (Fluorspan), its CTI value is higher.
In general, copper clad foil substrate of the present invention is adding after Calcium Fluoride (Fluorspan) filler, can improve its CTI value; When filler selects Calcium Fluoride (Fluorspan) and other high CTI filler collocation to use, compare other high CTI filler of independent use, can promote the CTI value of copper clad foil substrate, and improve the other problem that other CTI filler excessive use brings, have good over-all properties; Adopt high level and can make the CTI value of copper clad foil substrate obviously improve during for the Calcium Fluoride (Fluorspan) of one-component, more than reaching 600V, and also over-all properties optimum, there is stronger alkali resistance, be suitable for large-scale industrialization production.
Applicant's statement, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the selected raw material of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. a compositions of thermosetting resin, is characterized in that, comprises by weight percentage following component: thermosetting resin 20-70 quality %, solidifying agent 1-30 quality %, promotor 0-10 quality % and high CTI filler 1-70 quality %; Described high CTI filler at least comprises Calcium Fluoride (Fluorspan).
2. compositions of thermosetting resin as claimed in claim 1, is characterized in that, described high CTI filler is through surface treatment;
Preferably, described surface treatment is used tensio-active agent processing;
Preferably, described tensio-active agent is the mixture of cationic, anionic, both sexes or neutral surface active agent's any one or at least two kinds;
Preferably, described tensio-active agent is the mixture of any one or at least two kinds of silane coupling agent, titanate ester treatment agent, aluminate, zirconate, stearic acid, oleic acid, lauric acid and metallic salt, resol, organic silicone oil or polyoxyethylene glycol.
3. compositions of thermosetting resin as claimed in claim 1, it is characterized in that, described high CTI filler, except comprising Calcium Fluoride (Fluorspan), is also selected from the mixture of any one or at least two kinds of aluminium hydroxide, barium sulfate, barium titanate, strontium titanate, talcum powder or titanium dioxide.
4. compositions of thermosetting resin as claimed in claim 3, is characterized in that,
The median size of described Calcium Fluoride (Fluorspan) is 0.5-15 μ m, is preferably 1-10 μ m, more preferably 1-5 μ m;
Preferably, described Calcium Fluoride Content is 1-70 quality %, is preferably 5-50 quality %, more preferably 10-40 quality %.
5. the compositions of thermosetting resin as described in claim 1-4 any one, is characterized in that, described thermosetting resin is the mixture of any one or at least two kinds of epoxy resin, cyanate, bismaleimides, polyimide or polybutadiene;
Preferably, described thermosetting resin is that number-average molecular weight is the mixture of any one or at least two kinds of bisphenol A epoxide resin, aliphatic epoxy resin or the cycloaliphatic epoxy resin of 500-4000.
6. the compositions of thermosetting resin as described in claim 1-5 any one, is characterized in that, described solidifying agent is amine and/or anhydrides;
Preferably, described solidifying agent is the mixture of any one or at least two kinds of Dyhard RU 100, diaminodiphenylsulfone(DDS) or two amido ditanes.
7. the compositions of thermosetting resin as described in claim 1-6 any one, is characterized in that, described composition also comprises fire retardant;
Preferably, described fire retardant is compound in triazine class and/or trimeric cyanamide and salt thereof.
8. the veneer sheet that the compositions of thermosetting resin of employing as described in one of claim 1-7 made, is characterized in that, it comprises prepreg;
Preferably, described prepreg comprises strongthener; With by impregnation drying postadhesion compositions of thermosetting resin thereon.
9. veneer sheet as claimed in claim 8, is characterized in that, described strongthener is the mixture of any one or at least two kinds of natural fiber, organic synthetic fibers, organic fabric or inorganic fibre.
10. a method that improves veneer sheet phase ratio creepage tracking index, is characterized in that, adopts the compositions of thermosetting resin described in claim 1-7 any one.
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| CN201410387041.0A CN104151777B (en) | 2014-08-07 | 2014-08-07 | Thermosetting resin composition |
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| CN201410387041.0A CN104151777B (en) | 2014-08-07 | 2014-08-07 | Thermosetting resin composition |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016019547A1 (en) * | 2014-08-07 | 2016-02-11 | 广东生益科技股份有限公司 | Thermosetting resin composition |
| JP2017088828A (en) * | 2015-11-17 | 2017-05-25 | 住友ベークライト株式会社 | Semiconductor sealing resin composition, semiconductor device and structure |
| CN107406672A (en) * | 2015-02-23 | 2017-11-28 | 沙特基础工业全球技术有限公司 | Anti creepage trace composition, the product formed by it and its manufacture method |
| CN110154486A (en) * | 2019-06-10 | 2019-08-23 | 铜陵华科电子材料有限公司 | The copper-clad plate of high proof tracking |
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| JPH0770411A (en) * | 1993-09-03 | 1995-03-14 | Hitachi Cable Ltd | Epoxide cast articles for sulfur hexafluoride insulator |
| JPH08199044A (en) * | 1995-01-27 | 1996-08-06 | Hitachi Cable Ltd | Epoxy resin composition for equipment insulated with sulfur hexafluoride gas |
| CN102093670A (en) * | 2010-12-23 | 2011-06-15 | 广东生益科技股份有限公司 | Halogen-free flame retardant epoxy resin composition and copper clad plate prepared from same |
| CN102173131A (en) * | 2010-12-30 | 2011-09-07 | 上海南亚覆铜箔板有限公司 | Copper foil-coated plate with high electricity leakage tracking index and preparation method thereof |
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2014
- 2014-08-07 CN CN201410387041.0A patent/CN104151777B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0770411A (en) * | 1993-09-03 | 1995-03-14 | Hitachi Cable Ltd | Epoxide cast articles for sulfur hexafluoride insulator |
| JPH08199044A (en) * | 1995-01-27 | 1996-08-06 | Hitachi Cable Ltd | Epoxy resin composition for equipment insulated with sulfur hexafluoride gas |
| CN102093670A (en) * | 2010-12-23 | 2011-06-15 | 广东生益科技股份有限公司 | Halogen-free flame retardant epoxy resin composition and copper clad plate prepared from same |
| CN102173131A (en) * | 2010-12-30 | 2011-09-07 | 上海南亚覆铜箔板有限公司 | Copper foil-coated plate with high electricity leakage tracking index and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016019547A1 (en) * | 2014-08-07 | 2016-02-11 | 广东生益科技股份有限公司 | Thermosetting resin composition |
| CN107406672A (en) * | 2015-02-23 | 2017-11-28 | 沙特基础工业全球技术有限公司 | Anti creepage trace composition, the product formed by it and its manufacture method |
| CN107406672B (en) * | 2015-02-23 | 2020-01-10 | 沙特基础工业全球技术有限公司 | Tracking resistant compositions, articles formed therefrom, and methods of making the same |
| JP2017088828A (en) * | 2015-11-17 | 2017-05-25 | 住友ベークライト株式会社 | Semiconductor sealing resin composition, semiconductor device and structure |
| CN110154486A (en) * | 2019-06-10 | 2019-08-23 | 铜陵华科电子材料有限公司 | The copper-clad plate of high proof tracking |
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| CN104151777B (en) | 2017-01-25 |
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