CN106280282B - A kind of moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant and the preparation method and application thereof - Google Patents

A kind of moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant and the preparation method and application thereof Download PDF

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Publication number
CN106280282B
CN106280282B CN201610667748.6A CN201610667748A CN106280282B CN 106280282 B CN106280282 B CN 106280282B CN 201610667748 A CN201610667748 A CN 201610667748A CN 106280282 B CN106280282 B CN 106280282B
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fire retardant
type epoxy
nitrogen
moulding type
containing phosphorus
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CN106280282A (en
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封其立
单玉来
张德伟
孙波
张国
王松松
葛笑笑
周佃香
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Jiangsu Xuyuan New Materials Co ltd
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JIANGSU ZHONGPENG NEW MATERIAL CO Ltd
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Abstract

The components such as a kind of the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant, including epoxy resin, phenolic curing agent, inorganic filler, curing accelerator, " phosphorus-nitrogen " synergistic fire retardant, coupling agent, release agent, colorant.Due to having used completely new phosphorus nitrogen synergistic fire retardant, compared with prior art, flame retarding efficiency with higher, and fire retardant is good with resin system compatibility, efficiently solves its dispersion, and simple process, it is low in cost, it is a kind of novel halogen-free flame-retardant green epoxy composite.

Description

A kind of moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant and preparation method thereof with Using
Technical field
The present invention relates to a kind of polymer-electronics encapsulating material technical field, especially a kind of mould of containing phosphorus-nitrogen fire retardant Plastotype epoxy bottom filler.
Background technique
In recent years, moulding type epoxy bottom filler (MUF) is widely used in the encapsulation of advanced flip chip type. MUF is usually to be made of components such as epoxy resin, phenolic curing agent, inorganic filler, curing accelerator and additives.With numerous High-molecular organic material is the same, and plain edition epoxy resin, phenolic resin are also easy to burn, and the electronics member of above-mentioned plastic packaging material encapsulation Part is often exposed in air at high temperature to be used, therefore it is required that it must have good flame-retarding characteristic.That applies earliest contains Bromine flame retardant, thermal decomposition product can remove fuel gas in conjunction with fuel gas.But brominated flame-retardant generates toxic in a fire Gas makes one to be poisoned, and in addition waste needs recovery processing of classifying, and has been prohibited from using substantially in plastic packaging material at present.It is big at present Inorganic fire retardants has been used in the plastic packaging material of part, has done fire retardant using magnesium hydroxide as CN1984960A is reported, they are by dividing Solution absorbs a large amount of combustions heat to prevent combustion thermal cycle from acting on polymer.But its additive amount is big, can largely sacrifice MUF Mobility.Some middle and high end plastic packaging materials use intrinsic flame retardant resin systems, as US6242110 report uses biphenyl or naphthalene type tree Rouge resin system advantageously forms foam layer of charcoal and assigns epoxy-plastic packaging material good anti-flammability in combustion process.But it is above-mentioned This body structure of resin leads to material at high temperature poor fluidity, may cause encapsulating structure lead in molding process and is destroyed, this Outer this kind of intrinsic flame retardant type epoxy and phenolic resin system often cost with higher.It therefore is to meet wanting for Advanced Packaging It asks, the new fire retardant of research and probe or fire-retardant mode are imperative.
Phosphorus-containing matter is considered as most possibly replacing brominated flame-retardant, realizes the fire retardant of halogen-free flameproof.Based on containing The research of phosphorus fire retardant has very much, but its application in plastic packaging material is not much and sees.US7544727 is reported using containing mostly fragrant Electronic package material of the cyclic phosphate as fire retardant.Nitrogenated flame retardant is also a kind of common flame-retardant system, fire-retardant mode Mainly to form the non-flammable compressive gases such as ammonia in decomposable process, flammable group is diluted and watered down.Its major advantage is Halogen, low cigarette, Be conducive to environmental protection.But its exclusive use is inefficient, and effect is more preferable in conjunction with other flame-retardant systems.It is released dependent on its pyrolysis The feature of non-flammable compressive gas is put, there is good frothing function, can be used as the foaming agent of Intumescent Retardant System.
While exploring synthesizing new efficient flame-retarding agent, people are used cooperatively also by different flame retardant, are reducing Flame retarding efficiency is improved while amount of flame-retardant agent.During different flame retardant is used cooperatively, since different flame retardant is fire-retardant The synergistic effect of mechanism, in the identical situation of additive amount, the flame retarding efficiency of cooperative flame retardant system is apparently higher than two kinds of fire retardants Flame retarding efficiency when exclusive use, here it is so-called fire retardant " synergistic effects ".Phosphorus-nitrogen cooperative flame retardant system is to apply at present Compare extensive cooperative flame retardant system, for example, Japan's volt is shown in that Co., Ltd., pharmacy institute develops efficient " phosphorus-nitrogen " synergistic fire retardant Polyphosphazene (trade name: Rabitle FP-100).The fire retardant has excellent flame-retarding characteristic to epoxy-plastic packaging material.Patent CN102617640 reports a kind of " phosphorus-silicon " synergistic fire retardant, and CN103073585 reports a kind of " phosphorus-silicon-nitrogen " ternary association Same fire retardant has used expensive end-vinyl silicon compound in above-mentioned fire retardant, such as 1,1,3,3- tetramethyl -1,3- Divinyl disiloxane, 1,1,3,3- tetramethyl -1,3- divinyl disilazane, diphenyl -1 1,3- dimethyl -1,3-, 3- divinyl disiloxane, 1,1,3,3- tetraphenyl -1,3- divinyl disiloxane, four silicon oxygen of tetramethyl tetravinyl ring Alkane, eight ethylene basic rings, eight silsesquioxane etc..The expensive cost of raw material causes the high cost of final fire retardant, makes it in MUF Application in equal epoxy composites is extremely restricted.In addition, be mostly fatty chain structure in above-mentioned synergistic fire retardant, It is unfavorable for improving the heat-resistant stability of MUF.
Summary of the invention
The technical problems to be solved in view of the defects of the present invention is to propose a kind of fire-retardant effects with higher The moulding type epoxy bottom filler of rate and fire retardant and the good containing phosphorus-nitrogen fire retardant of resin system compatibility.The present invention is another to be solved Certainly the technical issues of, is to provide the preparation method of the moulding type epoxy bottom filler of the containing phosphorus-nitrogen fire retardant, and its in flip-chip Application in type encapsulation.
The technical problem to be solved by the present invention is to what is be achieved through the following technical solutions, a kind of containing phosphorus-nitrogen fire retardant Moulding type epoxy bottom filler, its main feature is that, the component containing following parts by weight:
100 parts of epoxy resin;
1-200 parts of phenolic curing agent;
100-3000 parts of inorganic filler;
1-10 parts of curing accelerator;
1-50 parts of synergistic fire retardant of " phosphorus-nitrogen ";
1-20 parts of coupling agent;
1-10 parts of release agent;
1-10 parts of colorant.
In the filler of moulding type epoxy bottom, epoxy resin include linear phenolic epoxy resin, biphenyl type epoxy resin or One or more of mixtures of dicyclopentadiene type epoxy resin.
In the filler of moulding type epoxy bottom, curing agent can be amine, anhydride, imidazoles and phenolic epoxy acrylate One or more of mixtures.It is preferred that linear phenolic resin and biphenyl linear phenolic resin etc..
In the filler of moulding type epoxy bottom, inorganic filler has silica (unformed, crystallinity), alumina, aluminium nitride Deng preferred spherical junctions crystal form SiO 2 powder.
In the filler of moulding type epoxy bottom, curing accelerator has imidazoles, tertiary amine, phosphorus series compound, preferably 2- ethyl -4- Methylimidazole and triphenylphosphine.
In the filler of moulding type epoxy bottom, " phosphorus-nitrogen " synergistic fire retardant, structure respectively as shown in Formulas I or Formula II,
(Formulas I)
(Formula II).
In the filler of moulding type epoxy bottom, the coupling agent is selected from γ-(2,3- the third oxygen of epoxy) propyl trimethoxy Silane (KH-560), γ aminopropyltriethoxy silane (KH-550), γ-mercaptan aminopropyl trimethoxysilane (KH- 580) at least one of or a variety of mixtures in any ratio composition applicatory, preferably KH-580.
In the filler of moulding type epoxy bottom, the release agent is selected from native paraffin (bar wax etc.), synthetic wax (polyethylene wax Deng), stearic acid, palmitinic acid, zinc stearate, calcium stearate, at least one of lithium stearate and magnesium stearate or a variety of by appointing The mixture of what ratio composition applicatory, preferably bar wax and polyethylene wax.
In the filler of moulding type epoxy bottom, the colorant is selected from carbon black.
The method provided by the invention for preparing above-mentioned moulding type epoxy bottom filler, includes the following steps:
By the epoxy resin, the phenolic curing agent, the promotor, the coupling agent, the release agent, described disappear Infusion, the inorganic filler are kneaded after mixing, and obtain the MUF material.In the mixing step, temperature is 20-120 DEG C, tool Body can be 20-30 DEG C, 50-80 DEG C, 90-110 DEG C or 90-120 DEG C, preferably 60-90 DEG C;Time is 0.5-3 hours, concretely 0.5-1.5 hours or 1-1.5 hours, preferably 0.5-1 hours.
In concrete operations, above-mentioned each component can be uniformly mixed in required ratio, in common various three rollers of material or It heats and is kneaded on two roller kneading machines, obtain evenly dispersed mixture and buy cake on pancake making machine after cooling, crushing, needed for obtaining The moulding type epoxy bottom filler of size.
In addition, application of the moulding type epoxy bottom filler of aforementioned present invention offer in the encapsulation of various flip chip types, It belongs to the scope of protection of the present invention.
Epoxy composite provided by the present invention, due to having used completely new phosphorus nitrogen synergistic fire retardant, with prior art phase Than, flame retarding efficiency with higher, and fire retardant is good with resin system compatibility, efficiently solves its dispersion, and technique Simply, low in cost, it is a kind of novel halogen-free flame-retardant green epoxy composite.
Detailed description of the invention
Fig. 1 is the infared spectrum of fire retardant shown in preparation formula I in embodiment 1;
Fig. 2 is the MOLDI-TOF map of fire retardant shown in preparation formula I in embodiment 1;
Fig. 3 is the infared spectrum of fire retardant shown in preparation formula II in embodiment 2;
Fig. 4 is the MOLDI-TOF map of fire retardant shown in preparation formula II in embodiment 2.
Specific embodiment
A kind of moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant, the component containing following parts by weight:
100 parts of epoxy resin;
1-200 parts of phenolic curing agent;
100-3000 parts of inorganic filler;
1-10 parts of curing accelerator;
1-50 parts of synergistic fire retardant of " phosphorus-nitrogen ";
1-20 parts of coupling agent;
1-10 parts of release agent;
1-10 parts of colorant.
In the filler of moulding type epoxy bottom, epoxy resin include linear phenolic epoxy resin, biphenyl type epoxy resin or One or more of mixtures of dicyclopentadiene type epoxy resin.
In the filler of moulding type epoxy bottom, curing agent can be amine, anhydride, imidazoles and phenolic epoxy acrylate One or more of mixtures.It is preferred that linear phenolic resin and biphenyl linear phenolic resin etc..
In the filler of moulding type epoxy bottom, inorganic filler has silica (unformed, crystallinity), alumina, aluminium nitride Deng preferred spherical junctions crystal form SiO 2 powder.
In the filler of moulding type epoxy bottom, curing accelerator has imidazoles, tertiary amine, phosphorus series compound, preferably 2- ethyl -4- Methylimidazole and triphenylphosphine.
In the filler of moulding type epoxy bottom, fire retardant is " phosphorus-nitrogen " synergistic fire retardant, and structure is respectively such as Formulas I or formula Shown in II,
(Formulas I)
(Formula II).
In the filler of moulding type epoxy bottom, the coupling agent is selected from γ-(2,3- the third oxygen of epoxy) propyl trimethoxy Silane (KH-560), γ aminopropyltriethoxy silane (KH-550), γ-mercaptan aminopropyl trimethoxysilane (KH- 580) at least one of or a variety of mixtures in any ratio composition applicatory, preferably KH-580.
In the filler of moulding type epoxy bottom, the release agent is selected from native paraffin (bar wax etc.), synthetic wax (polyethylene wax Deng), stearic acid, palmitinic acid, zinc stearate, calcium stearate, at least one of lithium stearate and magnesium stearate or a variety of by appointing The mixture of what ratio composition applicatory, preferably bar wax and polyethylene wax.
In the filler of moulding type epoxy bottom, the colorant is selected from carbon black.
The method provided by the invention for preparing above-mentioned moulding type epoxy bottom filler, includes the following steps:
By the epoxy resin, the phenolic curing agent, the promotor, the coupling agent, the release agent, described disappear Infusion, the inorganic filler are kneaded after mixing, and obtain the MUF material.In the mixing step, temperature is 20-120 DEG C, tool Body can be 20-30 DEG C, 50-80 DEG C, 90-110 DEG C or 90-120 DEG C, preferably 60-90 DEG C;Time is 0.5-3 hours, concretely 0.5-1.5 hours or 1-1.5 hours, preferably 0.5-1 hours.
In concrete operations, above-mentioned each component can be uniformly mixed in required ratio, in common various three rollers of material or It heats and is kneaded on two roller kneading machines, obtain evenly dispersed mixture and buy cake on pancake making machine after cooling, crushing, needed for obtaining The moulding type epoxy bottom filler of size.
In addition, application of the moulding type epoxy bottom filler of aforementioned present invention offer in the encapsulation of various flip chip types, It belongs to the scope of protection of the present invention.
The present invention is further elaborated combined with specific embodiments below, but the present invention is not limited to following embodiments.Institute State method is conventional method unless otherwise instructed.The raw material can be gotten from open business unless otherwise instructed. " phosphorus-nitrogen " fire retardant shown in Formulas I of the present invention and Formula II can refer to CN102617640 and CN103073585 the method system It is standby.The preparation process includes the following steps: after dissolving vinyl itrogenous organic substance and diphenyl phosphine oxide in reaction dissolvent, Again into the system be added organic boron solution, at a certain temperature reaction a period of time, obtain after completion of the reaction the Formulas I or Compound shown in Formula II.
In the above method, the reaction dissolvent is selected from least one of alcohol compound, saturated hydrocarbons compound;Its In, the alcohol compound is in methanol, ethyl alcohol, propyl alcohol, amylalcohol, n-butanol, isopropanol, isobutanol, isoamyl alcohol, ethylene glycol At least one, specially at least one of methanol, ethyl alcohol, propyl alcohol and isopropanol;Wherein saturated hydrocarbons compound is selected from penta At least one of alkane, hexane, heptane, octane, nonane, decane, pentamethylene, hexamethylene and cycloheptane, specially pentane, oneself At least one of alkane, heptane, pentamethylene and hexamethylene.
In the method, organic boron be selected from trimethyl borine, boron triethyl, tripropylborane, triisopropyl boron, tri butyl boron and At least one of triphenyl borine;In the solution of the organic boron, solvent in ether, tetrahydrofuran and n-hexane at least It is a kind of.
In the reaction step, temperature is 0 ~ 50 DEG C, specially 10 ~ 45 DEG C;Reaction time is 0.5 ~ 40 hour, specially 1 ~ 35 hour.The reaction step carries out in an inert atmosphere;The inert atmosphere is in nitrogen atmosphere and argon atmosphere At least one, specially nitrogen atmosphere.
The performance of preparation gained composition epoxy resin is measured as follows in following embodiments (described Measuring method is conventional method unless otherwise instructed):
FTIR spectrum (FT IR) is measured using 2000 type Fourier infrared spectrograph of Perkin-Elmer, sample preparation Method uses KBr pressed disc method, range 4000-400 cm-1, 4 cm of resolution ratio-1.Mass spectrum (MALDI-TOF-MS) test uses The measurement of Biflex type III MALDI-TOF-MS mass spectrograph.LOI test: GB/T 2406-93 according to national standards, sample size 100×6.5×3.0 mm3.Vertical burn test: GB/T 2408-1996 according to national standards, sample size 125 × 13 ×3.0 mm3
Spiral flow length is measured by transmitting injection press and according to the helical flow metal die of EMM-I-66.Gelation Time uses iron plate method, by plastic packaging material as 175oIt in the thermal station of C, flattens, starts timing and obtained solidifying after plastic packaging material gel Gel time.Calorimetric inspects scanning (DSC) test and uses TA Q-100 type Instrument measuring, tests in a nitrogen environment, vitrifying It is 20 that transition temperature, which tests heating rate,oC/min.Mechanical performance is tested on 5567 type universal testing machine of Instron.Bending Measurement (GB/T 1040.1-2006 and GB/T9341-2000) the extrusion speed of performance is 2.0 mm/min.Test temperature: often Temperature.
Embodiment 1
In a reactor equipped with nitrogen inlet, condenser pipe and thermometer, by 6.06 g(0.02 mol) diphenyl Phosphine oxygen (DPPO) and 2.49 g(0.01 mol) iso-cyanuric acid triallyl ester sequentially adds in 10 ml acetone, at 15 DEG C Stir to clarify it is transparent, under nitrogen protection, control temperature at 15 DEG C, be added dropwise in 0.5 hour 4 ml concentration be 0.5M 3 third The tetrahydrofuran solution of base boron;After being added dropwise, stops reaction after keeping 15 DEG C of reactions 1 hour, steam solvent, repeatedly washed with water Wash, dry, obtain 6.75 g(fire retardant 1 of white solid), yield 79%.It is as follows to prepare reaction equation:
The structure detection data of flame retardant compound shown in Formulas I, including infrared spectrum, mass spectrum (MALDI-TOF) are respectively such as Shown in attached drawing 1 and 2.
Embodiment 2
In a reactor equipped with nitrogen inlet, condenser pipe and thermometer, by 6.06 g(0.03 mol) diphenyl Phosphine oxygen (DPPO) and 2.49 g(0.01 mol) triallyl cyanurate sequentially adds in 10 ml tetrahydrofurans, at 15 DEG C Stir to clarify it is transparent, under nitrogen protection, control temperature at 15 DEG C, in 0.5 hour be added dropwise 5ml concentration be 0.5M tributyl The hexane solution of boron;After being added dropwise, stops reaction after keeping 15 DEG C of reactions 2 hours, steam solvent, repeatedly washed with ether Wash, dry, obtain 6.32 g(fire retardant 2 of white solid), yield 74%.It is as follows to prepare reaction equation:
The structure detection data of flame retardant compound shown in Formula II, including infrared spectrum, mass spectrum (MALDI-TOF) are respectively such as Shown in attached drawing 3 and 4.
Embodiment 3
By 15 g of fire retardant shown in Formulas I prepared by embodiment 1,29.8 g of line style phenolic aldehyde, linear phenolic epoxy resin 55.2 g are heated to 150 DEG C, and melting mixing is uniform, later in 120 DEG C of 10 min of heat preservation, add triphenylphosphine (TPP) 0.4 G carries out deaeration after being quickly stirred, is finally cast in mold, 150 DEG C of solidifications 3h, 180 DEG C of solidification 6h, obtain sample into Limit by row oxygen index (OI) and vertical burn test, gained sample LOI are 33.5, and flame retardant rating is UL 94 V-0 grade.
Embodiment 4
By 15 g of fire retardant shown in Formula II prepared by embodiment 2,29.8 g of line style phenolic aldehyde, linear phenolic epoxy resin 55.2 g are heated to 150 DEG C, and melting mixing is uniform, later in 120 DEG C of 10 min of heat preservation, add triphenylphosphine (TPP) 0.4 G carries out deaeration after being quickly stirred, is finally cast in mold, 150 DEG C of solidifications 3h, 180 DEG C of solidification 6h, obtain sample into Limit by row oxygen index (OI) and vertical burn test, gained sample LOI are 33.8, and flame retardant rating is UL 94 V-0 grade.
Comparative example 1
35 g of line style phenolic aldehyde, 65 g of linear phenolic epoxy resin are heated to 150 DEG C, melting mixing is uniform, Zhi Hou 120 DEG C of 10 min of heat preservation, add 0.4 g of triphenylphosphine (TPP), carry out deaeration after being quickly stirred, be finally cast to mould In tool, 150 DEG C of solidifications 3h, 180 DEG C of solidification 6h obtain sample and carry out limit oxygen index and vertical burn test, gained sample LOI It is 21, flame retardant rating is not up to UL 94 V-2 grade.
Comparative example 3, embodiment 4 and comparative example 1 are as can be seen that be applied to ring for fire retardant shown in Formulas I and Formula II In oxygen composition, epoxy composite can be made to reach UL 94 V-0 grade fire-retardant.
Embodiment 5
Other components of removing silicon powder, coupling agent and curing accelerator are put into kneading machine first in MUF preparation process, It is kneaded 2 minutes;Silicon powder and coupling agent are added later, is kneaded 10 minutes, material is uniformly mixed;It is eventually adding curing accelerator, is mixed Refining 3 minutes.The composition mixed carries out crushing material after object to be combined is cooling, rear portion sample for flowing Property test and gelation time test;Another part sample breaks into pie, the preparation for batten.In batten preparation process, Using molded method, so that composition is softened and is molded into molding die under the conditions of 180 DEG C, goes out after solidification two minutes Mould, it is rear at 220 DEG C later to solidify 4h.
Each component shown in table 1 is proportionally weighed, material mixing is carried out by the above process later, one after the completion of mixing Sample is divided to test for mobile performance and gelation time, another part sample prepares batten by molded, and tests it Performance.Properties of product are shown in Table 2.
Embodiment 6
MUF preparation process is same as Example 5.Each component shown in table 1 is proportionally weighed, later by the above process into The mixing of row material, mixing are completed rear portion sample and are tested for mobile performance and gelation time, and another part sample passes through It is molded to prepare batten, and test its performance.Properties of product are shown in Table 2.
Comparative example 2
MUF preparation process is same as Example 5.Each component shown in table 1 is proportionally weighed, the above process is pressed later Material mixing is carried out, mixing is completed rear portion sample and tested for mobile performance and gelation time, and another part sample is logical Cross it is molded prepare batten, and test its performance, properties of product are shown in Table 2.
1 epoxy composite sample composition of table
2 MUF epoxy composite properties of product of table
Comparative example 5, embodiment 6 and comparative example 2 are as can be seen that use the MUF ring of fire retardant shown in Formulas I and Formula II The more traditional MUF composition of oxygen composition has higher fire-retardant rank.The heat resistance and mechanical property of its solidfied material simultaneously Also it increases, this is mainly due to caused by the good heat-resistant stability of fire retardant and toughening effect.

Claims (11)

1. a kind of moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant, which is characterized in that include the component of following parts by weight:
Epoxy resin: 100 parts;
Phenolic curing agent: 1-200 parts;
Inorganic filler: 100-3000 parts;
Curing accelerator: 1-10 parts;
" phosphorus-nitrogen " synergistic fire retardant: 1-50 parts;
Coupling agent: 1-20 parts;
Release agent: 1-10 parts;
Colorant: 1-10 parts,
Above-mentioned " phosphorus-nitrogen " synergistic fire retardant, structure respectively as shown in Formulas I or Formula II,
(Formulas I)
(Formula II).
2. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 1, it is characterised in that: the epoxy Resin is selected from the mixed of the one or more including linear phenolic epoxy resin, biphenyl epoxy resin or DCPD-containing epoxy resin Close object.
3. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 1, it is characterised in that: the phenolic aldehyde Curing agent selects novolac or biphenyl novolac.
4. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 1, it is characterised in that: inorganic filler Selected from silica, alumina or aluminium nitride.
5. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 4, it is characterised in that: inorganic filler Selected from spherical junctions crystal form SiO 2 powder.
6. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 1, it is characterised in that: solidification promotes Agent is selected from imidazoles, tertiary amine or phosphorus series compound.
7. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 6, it is characterised in that: solidification promotes Agent is selected from 2-ethyl-4-methylimidazole or triphenylphosphine.
8. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 1, it is characterised in that: the idol Join agent and is selected from γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane (KH-560), γ aminopropyltriethoxy silane (KH- Or at least one of γ-mercaptan aminopropyl trimethoxysilane (KH-580) or a variety of in any ratio group applicatory 550) At mixture.
9. the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant according to claim 1, it is characterised in that: described is de- Mould agent is in native paraffin, synthetic wax, stearic acid, palmitinic acid, zinc stearate, calcium stearate, lithium stearate or magnesium stearate At least one or more of mixture in any ratio composition applicatory.
10. the preparation method of the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant as described in claim 1, it is characterised in that: The component raw material is passed through into rubber mixing machine or extruder, is squeezed out at 50-150 DEG C, the pre-molding after cooling crush.
11. a kind of purposes of the moulding type epoxy bottom filler of containing phosphorus-nitrogen fire retardant as described in claim 1, it is characterised in that: The moulding type epoxy bottom filler of the containing phosphorus-nitrogen fire retardant is in flip chip type BGA Package, chip size packages, wafer scale Application in encapsulation.
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CN108276538A (en) * 2018-02-11 2018-07-13 南京远淑医药科技有限公司 A kind of preparation process of phosphorus containing phenolic resin and its application
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