CN101735619A - Halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive and preparation method thereof - Google Patents
Halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive and a preparation method thereof. The preparation method comprises: adding vinyl dimethicone, a reinforcing material, a heat-conducting filling material and a halogen-free flame retardant in a vacuum kneader, dehydrating and blending for 30-120 minutes at 100-150 DEG C and vacuum degree of 0.06-0.1MPa to obtain a base material, adding a cross-linking agent containing hydrogen silicone oil and a cross-linking inhibitor to the base material at the normal temperature, adequately agitating for 10-30 minutes to prepare a component A; adding a platinum catalyst to the base material, adequately agitating for 10-30 minutes to prepare a component B; taking the component A and the component B of the same parts by weight, blending uniformly, and deaerating for 5-10 minutes at the vacuum degree of 0.06-0.1MPa to obtain the halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive. The potting adhesive has good flow properties and convenient use and can be cured at the normal temperature or a high temperature, condensate has excellent flame retardant property and heat-conducting property, and the potting adhesive can be widely applied to the fields of electronic electric appliance, chip encapsulation and LED encapsulation, and the like.
Description
Technical field
The present invention relates to the electronic encapsulation material technical field, specifically, relate to a kind of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive and technology of preparing thereof.
Background technology
Along with high-tech areas such as electronic devices and components, power circuit module, large-scale surface-mounted integrated circuit, LED further realize high-performance, high reliability and miniaturization, and Working environment is harsh more, require the embedding part must be between low temperature and the high temperature, move under the condition such as high speed rotating, this just requires Embedding Material not only to have good high and low temperature resistance, mechanical mechanics property, electrical insulation capability etc., and need possess good heat-conducting and flame retardant properties.
Using more Embedding Material at present is various synthetic polymers, wherein more extensive with Resins, epoxy, urethane and elastomeric application.Silicon rubber can keep elasticity for a long time in very wide temperature range, and do not absorb heat during sulfuration, not heat release, and have good electric property and chemical stability, be the preferred material of electric assembly embedding.But the typical case is very poor without the heat conductivility of the silicon rubber of filling, and thermal conductivity has only 0.2W/mK, and flame retardant properties is relatively poor, just can perfect combustion once lighting.Therefore, in order to obtain to have the electronic encapsulation material of better heat conduction and flame retardant properties, often need to carry out filling-modified to silicon rubber.At present, though domestic in that some research reports are arranged aspect the halogen-free flame-retarded heat-conducting joint sealant, lay particular stress in single heat conduction or fire-retardant more.A kind of high heat conduction organosilicon filling and sealing gum is disclosed as Chinese patent application CN 101054057A, CN 101407635A discloses a kind of addition type heat conducting silicon rubber with excellent fluidity and high thermal conductivity, but these two patents flame retardant properties of not mentioned silicon rubber all.And Chinese patent application CN 101121820A discloses the halogen-free anti-flaming silicon rubber that a kind of flame retardant rating is the FV-0 level, but the heat conductivility of the not mentioned silicon rubber of this patent.Chinese patent application CN 101402798A discloses a kind of heat conduction flame-proof liquid silicon rubber for electron, though have high thermal and flame retardant properties, because its viscosity more than 10000mPas, lacks good flowing property, can not be used as electron pouring sealant.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive and preparation method thereof is provided, be characterized in that this halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive not only has good flame-retarded heat-conducting performance and excellent flowability energy, and Environmental Safety, easy handling.
The preparation method of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive of the present invention comprises the steps:
(1) preparation of base-material: vinyldimethicone, supporting material, heat conductive filler and halogen-free flame retardants are added in the vacuum kneader, at 100～150 ℃, under vacuum tightness 0.06～0.1MPa, 30～120 minutes acquisition base-materials of blend;
Raw materials in part by weight is as follows:
100 parts of vinyldimethicone
2～20 parts of supporting materials
100～300 parts of heat conductive fillers
50～100 parts of halogen-free flame retardantss;
(2) preparation of A component: at normal temperatures, in the base-material that step (1) makes, adding hydrogen content is containing hydrogen silicone oil linking agent and the cross-linked inhibitor of 0.3～1.6wt%, fully stirs and made the A component in 10～30 minutes,
Raw materials in part by weight is as follows:
100 parts of base-materials
0.2～45 part of containing hydrogen silicone oil
0.002～0.01 part of cross-linked inhibitor;
(3) preparation of B component: at normal temperatures, get the base-material that step (1) makes, adding platinum content is the platinum catalyst of 1000～5000ppm, fully stirs and makes the B component in 10～30 minutes; The weight ratio of described base-material and platinum catalyst is 100: 2.0～100: 0.01;
(4) preparation of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive: at normal temperatures, the B component that A component that the step (2) of weight makes and step (3) make such as getting mixes, deaeration is 5～10 minutes under vacuum tightness 0.06～0.1MPa, obtains halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive.
Vinyldimethicone described in the step (1) is one or more the mixture in straight chain type vinyldimethicone or the branched chain type vinyldimethicone, the contents of ethylene of vinyldimethicone is 0.3～3.0wt%, and the viscosity in the time of 25 ℃ is 200～3000mPas.
Supporting material described in the step (1) is that contents of ethylene is the methyl ethylene MvQ resin of 0.1～5wt%.Heat conductive filler described in the step (1) is that median size is one or more the mixture in the surface-treated aluminium sesquioxide of coupling agent, aluminium nitride, aluminum boride, silicon carbide or silicon nitride of 2～20 μ m.Halogen-free flame retardants described in the step (1) is that median size is one or more the mixture in the surface-treated aluminium hydroxide of coupling agent, magnesium hydroxide or zinc borate of 2～10 μ m.Described through the coupling agent surface treatment adopt technical field surface treatment method commonly used all can, the present invention preferably mixes coupling agent after with suitable solvent cut with heat conductive filler or halogen-free flame retardants after, the treatment process of heat drying.The present invention to the kind of coupling agent without limits, technical field coupling agent commonly used all can use, for example: sec.-propyl distearyl acyl-oxygen base aluminic acid ester and γ-methacryloxypropyl trimethoxy silane.
Described catalyzer is the alcoholic solution of Platinic chloride or the vinylsiloxane complex compound of Platinic chloride.
Described cross-linked inhibitor is 2-methyl-3-butynyl-2-alcohol, 2-methyl isophthalic acid-hexin base-3-alcohol, 3, and is at least a in 5-dimethyl-1-hexin base-3-alcohol, 1-ethynyl-1-hexalin, methyl (trimethylammonium fourth alkynyloxy group) silane, phenyl (trimethylammonium fourth alkynyloxy group) silane, vinyl (trimethylammonium fourth alkynyloxy group) silane and the phenylacetylene.
A kind of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive that makes by preparation method of the present invention.
With the halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive that aforesaid method makes, press GB/T 10247-2008 tested viscosity, press GB/T 531-2008 test Shore A hardness; Press GB/T 528-1998 test tensile strength and elongation at break; Press GB/T1408.1-2006 test dielectric strength; Press GB/T 1410-2006 test volume resistivity; Press GB/T11205-2009 test thermal conductivity; Press the fire-retardant rank of UL 94 tests.
Compared with prior art, the present invention has the following advantages:
1, adds good heat conductive filler of an amount of electrical property and halogen-free flame retardants in the halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive of the present invention, when making it have the excellent heat conductivity performance, also had higher flame retardant properties;
2, utilize band methyl ethylene MvQ resin to substitute white carbon black, not only reduced the viscosity of organic silicon potting adhesive, and helped the filling and the dispersion of heat conductive filler and fire retardant as supporting material;
3, the not halogen-containing and harmful heavy metal of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive of the present invention, and do not produce toxic substance or irritating smell in its production and the solidification process, there is not by product, Environmental Safety.
Embodiment
Embodiment 1:
Taking by weighing aluminium sesquioxide 200 weight parts adds in the high speed kneader, under the condition of high-speed stirring, slowly drip 1 weight part and use the consoluet sec.-propyl distearyl of white oil acyl-oxygen base aluminic acid ester in advance, be warming up to 120 ℃ after dropwising and continued high-speed stirring 2 hours, discharging, after placing vacuum drying oven to remove residual white oil the gained filler, sieve and promptly make the surface-treated aluminium sesquioxide of sec.-propyl distearyl acyl-oxygen base aluminic acid ester that median size is 5 μ m.
Taking by weighing aluminium hydroxide 200 weight parts adds in the high speed kneader, under the condition of high-speed stirring, slowly drip the γ-methacryloxypropyl trimethoxy silane of the ethanol alcoholic solution dilution of the prior water of 1 weight part, be warming up to 120 ℃ after dropwising and continued high-speed stirring 2 hours, discharging, after placing vacuum drying oven to remove residual water and ethanol the gained filler, sieve and promptly make the surface-treated aluminium hydroxide of γ-methacryloxypropyl trimethoxy silane that median size is 2.7 μ m.
With viscosity is that 500mPas, contents of ethylene are straight chain type vinyldimethicone 100 weight parts of 0.45wt%, contents of ethylene is 3.5% methyl ethylene MvQ resin 7.14 weight parts, aluminium sesquioxide 140 weight parts of above-mentioned processing, aluminium hydroxide 60 weight parts of above-mentioned processing add in the vacuum kneader, in 120 ℃ of temperature, vacuum tightness is 0.08MPa, 60 minutes acquisition base-materials of dehydration blend.
With hydrogen content is 0.5% containing hydrogen silicone oil linking agent 4.1 weight parts, and cross-linked inhibitor 1-ethynyl-1-hexalin 0.0065 weight part and 100 weight part base-materials fully mixed 20 minutes, obtains the A component.Vinylsiloxane complex compound 0.25 weight part and the 100 weight part base-materials that with platinum content are the Platinic chloride of 2600ppm mixed under stirrer 20 minutes, obtained the B component.
After the A component and B component blend at room temperature evenly of weight part such as getting, be deaeration 8 minutes under the 0.1MPa in vacuum tightness, obtain halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive, The performance test results is as shown in table 1.As can be seen, this joint sealant has good flame-retarded heat-conducting performance, flowing property, electrical property and mechanical property.
Embodiment 2:
The preparation method of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive of the present invention and condition such as embodiment 1, to change into through the surface-treated median size of coupling agent sec.-propyl distearyl acyl-oxygen base aluminic acid ester be aluminium sesquioxide 105 weight parts of 5 μ m with median size through coupling agent sec.-propyl distearyl acyl-oxygen base aluminic acid ester surface-treated (adopting the surface treatment method identical with embodiment 1) with heat conductive filler is aluminium sesquioxide 35 weight parts of 19 μ m, make halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive, The performance test results is as shown in table 1.As can be seen, compare with embodiment 1, its thermal conductivity rises to 0.75W/mK from 0.65W/mK, and other performance variation is little, this shows, the composite heat conductivility that helps improving joint sealant of different-grain diameter filler.
Embodiment 3:
The preparation method of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive of the present invention and condition such as embodiment 1, it is 300mPas that vinyldimethicone is changed into viscosity, contents of ethylene is the straight chain type vinyldimethicone of 0.72wt%, corresponding is that 0.5% containing hydrogen silicone oil linking agent is brought up to 5.6 weight parts with hydrogen content, make halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive, The performance test results is as shown in table 1.As can be seen, compare with embodiment 1,2, though the heat conductivility of this joint sealant decreases, its flowing property is significantly improved, and its viscosity only is 2600mPas.
Embodiment 4:
The preparation method of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive of the present invention and condition such as embodiment 1, with the reinforced filling contents of ethylene is that 3.5% methyl ethylene MvQ resin is increased to 14.28 weight parts, corresponding is that 0.5% containing hydrogen silicone oil linking agent is brought up to 5.5 weight parts with hydrogen content, make halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive, The performance test results is as shown in table 1.As can be seen, the content that increases methyl ethylene MvQ resin in proper range helps the raising of the tensile strength of joint sealant, and less to other performance impact.
Embodiment 5
Taking by weighing silicon carbide 200 weight parts adds in the high speed kneader, under the condition of high-speed stirring, slowly drip 1 weight part and use the consoluet sec.-propyl distearyl of white oil acyl-oxygen base aluminic acid ester in advance, be warming up to 120 ℃ after dropwising and continued high-speed stirring 2 hours, discharging, after placing vacuum drying oven to remove residual white oil the gained filler, sieve and promptly make the surface-treated silicon carbide of sec.-propyl distearyl acyl-oxygen base aluminic acid ester that median size is 2 μ m.
Taking by weighing zinc borate 200 weight parts adds in the high speed kneader, under the condition of high-speed stirring, slowly drip the γ-methacryloxypropyl trimethoxy silane of the ethanol alcoholic solution dilution of the prior water of 1 weight part, be warming up to 120 ℃ after dropwising and continued high-speed stirring 2 hours, discharging, after placing vacuum drying oven to remove residual water and ethanol the gained filler, sieve and promptly make the surface-treated zinc borate of γ-methacryloxypropyl trimethoxy silane that median size is 10 μ m.
With viscosity is that 3000mPas, contents of ethylene are branched chain type vinyldimethicone 20 weight parts of 3wt%, viscosity is that 300mPas, contents of ethylene are straight chain type vinyldimethicone 80 weight parts of 0.72wt%, contents of ethylene is methyl ethylene MvQ resin 2 weight parts of 5wt%, silicon carbide 100 weight parts of above-mentioned processing, zinc borate 100 weight parts of above-mentioned processing add in the vacuum kneader, in 100 ℃ of temperature, vacuum tightness is 0.06MPa, 30 minutes acquisition base-materials of dehydration blend.
With hydrogen content is 0.3% containing hydrogen silicone oil linking agent 12.6 weight parts, and cross-linked inhibitor vinyl (trimethylammonium fourth alkynyloxy group) silane 0.002 weight part and 100 weight part base-materials fully mixed 10 minutes, obtains the A component.Aqueous isopropanol 2 weight parts and the 100 weight part base-materials that with platinum content are the Platinic chloride of 1000ppm mixed under stirrer 10 minutes, obtained the B component.
After the A component and B component blend at room temperature evenly of weight part such as getting, be deaeration 5 minutes under the 0.06MPa in vacuum tightness, obtain halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive, The performance test results is as shown in table 1.As can be seen, this joint sealant has good comprehensive performances, and the vinyl silicone oil that adds an amount of side chain helps the raising of the tensile strength of joint sealant.
Embodiment 6
Taking by weighing aluminium nitride 200 weight parts adds in the high speed kneader, under the condition of high-speed stirring, slowly drip 1 weight part and use the consoluet sec.-propyl distearyl of white oil acyl-oxygen base aluminic acid ester in advance, be warming up to 120 ℃ after dropwising and continued high-speed stirring 2 hours, discharging, after placing vacuum drying oven to remove residual white oil the gained filler, sieve and promptly make the surface-treated aluminium nitride of sec.-propyl distearyl acyl-oxygen base aluminic acid ester that median size is 2 μ m.
Taking by weighing magnesium hydroxide zinc 200 weight parts adds in the high speed kneader, under the condition of high-speed stirring, slowly drip the γ-methacryloxypropyl trimethoxy silane of the ethanol alcoholic solution dilution of the prior water of 1 weight part, be warming up to 120 ℃ after dropwising and continued high-speed stirring 2 hours, discharging, after placing vacuum drying oven to remove residual water and ethanol the gained filler, sieve and promptly make the surface-treated magnesium hydroxide of γ-methacryloxypropyl trimethoxy silane that median size is 10 μ m.
With viscosity is that 200mPas, contents of ethylene are straight chain type vinyldimethicone 100 weight parts of 0.8wt%, contents of ethylene is methyl ethylene MvQ resin 20 weight parts of 0.1wt%, above-mentioned processing aluminium nitride 300 weight parts, above-mentioned processing magnesium hydroxide 50 weight parts add in the vacuum kneader, in 150 ℃ of temperature, vacuum tightness is 0.1MPa, 120 minutes acquisition base-materials of dehydration blend.
With hydrogen content is containing hydrogen silicone oil linking agent 1.0 weight parts of 1.6wt%, and cross-linked inhibitor phenylacetylene 0.01 weight part and 100 weight part base-materials fully mixed 30 minutes, obtains the A component.Vinylsiloxane complex compound 0.01 weight part and the 100 weight part base-materials that with platinum content are the Platinic chloride of 5000ppm mixed under stirrer 30 minutes, obtained the B component.
After the A component and B component blend at room temperature evenly of weight part such as getting, be deaeration 10 minutes under the 0.1MPa in vacuum tightness, obtain halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive, The performance test results is as shown in table 1.As can be seen, add relatively large aluminium nitride with high thermal conductivity after, the heat conductivility of joint sealant is significantly improved, and has reached 1.12W/mK, and joint sealant has still kept good flame-retardance energy, flowing property, electrical property and mechanical property.
Table 1
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Viscosity (mPas) | ??4500 | ??4400 | ??2600 | ??4650 | ??3900 | ??5060 |
| Density (g/cm 3) | ??1.86 | ??1.86 | ??1.85 | ??1.85 | ??1.81 | ??2.1 |
| Hardness (Shore A) | ??55 | ??56 | ??60 | ??59 | ??58 | ??75 |
| Tensile strength (MPa) | ??2.76 | ??2.70 | ??2.8 | ??2.94 | ??2.88 | ??3.3 |
| Elongation at break (%) | ??45 | ??40 | ??30 | ??38 | ??28 | ??20 |
| Dielectric strength (KV/mm) | ??20 | ??20 | ??22 | ??21 | ??22 | ??18 |
| Volume specific resistance (Ω cm) | ??1.1×10 15 | ??1.1×10 15 | ??1.2×10 15 | ??1.2×10 15 | ??1.3×10 15 | ??9.8×10 14 |
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Thermal conductivity (W/mK) | ??0.65 | ??0.75 | ??0.62 | ??0.67 | ??0.54 | ??1.12 |
| Fire-retardant rank (UL 94) | ??V-0 | ??V-0 | ??V-0 | ??V-0 | ??V-0 | ??V-0 |
Claims (8)
1. the preparation method of a halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive is characterized in that specifically may further comprise the steps:
(1) preparation of base-material: vinyldimethicone, supporting material, heat conductive filler and halogen-free flame retardants are added in the vacuum kneader, at 100～150 ℃, under vacuum tightness 0.06～0.1MPa, 30～120 minutes acquisition base-materials of blend;
Raw materials in part by weight is as follows:
100 parts of vinyldimethicone
2～20 parts of supporting materials
100～300 parts of heat conductive fillers
50～100 parts of halogen-free flame retardantss;
(2) preparation of A component: at normal temperatures, in the base-material that step (1) makes, adding hydrogen content is containing hydrogen silicone oil linking agent and the cross-linked inhibitor of 0.3～1.6wt%, fully stirs and made the A component in 10～30 minutes,
Raw materials in part by weight is as follows:
100 parts of base-materials
0.2～45 part of containing hydrogen silicone oil
0.002～0.01 part of cross-linked inhibitor;
(3) preparation of B component: at normal temperatures, get the base-material that step (1) makes, adding platinum content is the platinum catalyst of 1000～5000ppm, fully stirs and makes the B component in 10～30 minutes; The weight ratio of described base-material and platinum catalyst is 100: 2.0～100: 0.01;
(4) preparation of halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive: at normal temperatures, the B component that A component that the step (2) of weight makes and step (3) make such as getting mixes, deaeration is 5～10 minutes under vacuum tightness 0.06～0.1MPa, obtains halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive.
2. preparation method according to claim 1, it is characterized in that vinyldimethicone described in the step (1) is one or more the mixture in straight chain type vinyldimethicone or the branched chain type vinyldimethicone, the contents of ethylene of vinyldimethicone is 0.3～3.0wt%, and the viscosity in the time of 25 ℃ is 200～3000mPas.
3. preparation method according to claim 1 is characterized in that supporting material described in the step (1) is that contents of ethylene is the methyl ethylene MvQ resin of 0.1～5wt%.
4. preparation method according to claim 1 is characterized in that heat conductive filler described in the step (1) is that median size is one or more the mixture in the surface-treated aluminium sesquioxide of coupling agent, aluminium nitride, aluminum boride, silicon carbide or silicon nitride of 2～20 μ m.
5. preparation method according to claim 1, it is characterized in that halogen-free flame retardants described in the step (1) be median size be 2～10 μ m through coupling agent surface-treated aluminium hydroxide, magnesium hydroxide or zinc borate in one or more mixture.
6. preparation method according to claim 1 is characterized in that described catalyzer is the alcoholic solution of Platinic chloride or the vinylsiloxane complex compound of Platinic chloride.
7. preparation method according to claim 1, it is characterized in that described cross-linked inhibitor is 2-methyl-3-butynyl-2-alcohol, 2-methyl isophthalic acid-hexin base-3-alcohol, 3, one or more mixture in 5-dimethyl-1-hexin base-3-alcohol, 1-ethynyl-1-hexalin, methyl (trimethylammonium fourth alkynyloxy group) silane, phenyl (trimethylammonium fourth alkynyloxy group) silane, vinyl (trimethylammonium fourth alkynyloxy group) silane or the phenylacetylene.
8. halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive that makes by the described preparation method of claim 1.
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