CN103834352A - Double-component high heat-conducting pouring sealant with excellent mechanical properties and preparation method thereof - Google Patents
Double-component high heat-conducting pouring sealant with excellent mechanical properties and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a double-component high heat-conducting pouring sealant with excellent mechanical properties and a preparation method thereof. The pouring sealant comprises components A and B in a weight mixing ratio: 1:1, wherein the component A comprises 100-120 parts of polysiloxane, 15-45 parts of mono-blocked vinyl silicone oil, 0.1-5 parts of catalyst and 200-1200 parts of heat-conducting filler; the component B comprises 100 parts of polysiloxane, 10-40 parts of hydrogen-containing polysiloxane, 5-25 parts of hydrogen-terminated polysiloxane, 0.05-1 part of inhibitor and 200-1200 parts of heat-conducting filler. According to the sealant provided by the invention, spherical heat-conducting filler is selected, and the loading level of the heat-conducting filler is increased under the premise of not affecting the flowability through grain size compounding, so that a higher heat-conducting performance is obtained. The mono-blocked vinyl silicone oil and hydrogen-terminated polysiloxane are added into the system, and the mechanical properties (hardness and elongation at break) can be adjusted by changing the content of the mono-blocked vinyl silicone oil and hydrogen-terminated polysiloxane, so that performances such as impact resistance and crack resistance are further improved. Finally, the high heat-conducting pouring sealant with excellent mechanical can be obtained.
Description
Technical field
The present invention relates to a kind of high heat conduction joint sealant, this joint sealant is composite by the spherical heat conductive filler of different-grain diameter on the one hand, in improving thermal conductivity, ensure the mobility of joint sealant as far as possible, add on the other hand single end-blocking vinyl silicone oil and end hydrogen based polysiloxane, obtain excellent mechanical property by reducing hardness.
Background technology
Along with the development of integrated technology and package technique, electronic component, logical circuit are tending towards densification and miniaturization, and thermal value is corresponding increase also, if heat can not conduct in time, easily form localized hyperthermia, and then may damage components and parts, assembly.In order to prevent the intrusion to electronic devices and components of moisture, dust and obnoxious flavour, slow down vibrations simultaneously, prevent external force damage components and parts, the electron pouring sealant demand that a kind of heat conductivility is good, mechanical property is excellent is more and more very urgent.
Addition-type silicon rubber not only can room temperature vulcanization but also the sulfuration of can heating, and sulfidation do not discharge low molecule by product, had that shrinking percentage is little, an easily advantage such as control of deep layer vulcanization and crosslinking structure simultaneously, was acknowledged as the preferred material of electron pouring sealant.Unfilled silicon rubber thermal conductivity only has 0.2W/mK left and right, the effective ways that improve at present silicon rubber heat conductivility are to fill inorganic heat conductive filler (as aluminum oxide, silicon powder, aluminium nitride, boron nitride, silicon carbide etc.), but the silicon rubber of preparation high thermal conductivity (being greater than 1.0W/mK) need to add a large amount of fillers, and the increase of filler loading level can cause the reduction greatly of mobility, lose the meaning of embedding.The disclosed a kind of electronics heat conductive flame-retarding silicon rubber of Chinese invention patent 200810219101.2, although thermal conductivity can reach 1.5～2.5W/mK, viscosity is greater than 20000mPas, cannot use as joint sealant.The disclosed a kind of additive high-thermal-conductivity organic silicon electronic pouring sealant thermal conductivity of another patent of invention 201110237351.0 of China is greater than 1.0W/mK, and there is good mobility, can be used for embedding, but its mechanical property needs to improve, being filled in of a large amount of heat conductive fillers can cause hardness to increase when obtaining good heat conductive performance and the remarkable reduction of elongation at break, can greatly affect like this performance such as shock resistance and cracking resistance, particularly high rigidity of joint sealant and low elongation at break for opposing external shock power and vibrations, prevent that cracking is all very unfavorable.
Summary of the invention
The object of the invention is to overcome the mobility causing while using general heat conductive filler loading level larger and reduce problem, select spherical heat conductive filler, and by having increased the loading level of heat conductive filler under the composite prerequisite not affecting mobility of particle diameter, obtain higher heat conductivility; By being used in conjunction with of single end-blocking vinyl silicone oil and end hydrogen based polysiloxane, the body mechanical property of joint sealant is optimized to lifting simultaneously.
In order to realize object of the present invention, a kind of high heat conduction joint sealant of two components of mechanical property excellence is proposed, described joint sealant comprises that mass mixing ratio is two components of A, B of 1:1;
Described component A is as follows by weight:
A
1. organopolysiloxane 100-120 part;
A
2. single end-blocking vinyl silicone oil 15-45 part;
A
3. catalyzer 0.1-5 part;
A
4. heat conductive filler 200-1200 part;
Described A
1structure in have at least two vinyl to be connected with Siliciumatom, 25 DEG C time, viscosity is 100-10000mpas, contents of ethylene is 0.1%-8.0%.Described vinyl can be positioned at molecule chain end, molecular chain centre or molecule chain end and centre exists simultaneously;
Described A
2in the time of 25 DEG C, viscosity is 100-5000mpas, and contents of ethylene is 0.05%-0.8%.Described vinyl is positioned at an end of molecular chain, and another end is methyl or hydroxyl;
Described A
3component is Pt complex compound, and part is 1,3-divinyl tetramethyl disiloxane, and the content of Pt is 5-2000ppm;
Described A
4select in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide at least one or several combinations;
Described B component is as follows by weight:
B
1. 100 parts of organopolysiloxane;
B
2. hydrogen containing siloxane 10-40 part;
B
3. end hydrogen based polysiloxane 5-25 part;
B
4. inhibitor 0.05-1 part;
B
5. heat conductive filler 200-1200 part;
Described B
1structure in have at least two vinyl to be connected with Siliciumatom, 25 DEG C time, viscosity is 100-10000mpas, contents of ethylene is 0.1%-8.0%.Described vinyl can be positioned at molecule chain end, molecular chain centre or molecule chain end and centre exists simultaneously;
Described B
2in the time of 25 DEG C, viscosity is 10-100mpas, and hydrogen richness is 0.15%-1.6%.Described hydrogen containing siloxane uses as linking agent, at least will contain three SiH groups in structure, is positioned in the middle of molecular chain;
Described B
3in the time of 25 DEG C, viscosity is 5-50mpas, and hydrogen richness is 0.09%-0.19%.Described end hydrogen based polysiloxane uses as chainextender, contains two SiH groups in structure, is positioned at molecular chain two ends;
Described B
4select 1,3,5,7-tetrem thiazolinyl-1, at least one in 3,5,7-tetramethyl-ring tetrasiloxane, 1-ethynylcyclohexanol, 2-methylbutynol, DEF or diallyl maleate;
Described B
5select in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide at least one or several combinations.
Described heat conductive filler A
4and B
5form is spherical, adopts two kinds of particle diameters to carry out composite, and wherein small particle size scope is at 0.2-20 μ m, and large particle size range is at 20-50 μ m, and the compound proportion of large small particle size is 0.25-4:1.
The present invention also proposes to prepare the method for the described pair of high heat conduction joint sealant of component, wherein,
The preparation method of described component A is: by the A of described proportioning
1, A
2, A
3join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min and mix de-bubbled, then by A
4component joins in stirring tank, is greater than under the condition of 0.095MPa stirs 60-90min in vacuum tightness;
The preparation method of described B component is: by the B of described proportioning
1, B
2, B
3, B
4join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min and mix de-bubbled, then by B
5component joins in stirring tank, is greater than under the condition of 0.095MPa stirs 60-90min in vacuum tightness.
Beneficial effect of the present invention: first the present invention selects spherical heat conductive filler, by having increased the loading level of heat conductive filler under the composite prerequisite not affecting mobility of particle diameter, obtains higher heat conductivility; Secondly in system, add single end-blocking vinyl silicone oil and end hydrogen based polysiloxane, by changing the content of the two, can regulate mechanical property (hardness, elongation at break), and then improve the performances such as shock resistance, cracking resistance, finally can obtain a kind of high heat conduction joint sealant of mechanical property excellence.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, the present invention is described in more detail.
Implement comparative example:
The preparation method of component A is: 1 part of 145 parts of the organopolysiloxane that during by 25 DEG C, viscosity is 200mpas, the Pt complex compound catalyst of 2000ppm join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min, mix de-bubbled; By median size be 30 μ m and 7 μ m in proportion 300 parts of composite mixing ball-aluminium oxides of 1:1 join in stirring tank, be greater than in vacuum tightness under the condition of 0.095MPa and stir 60min, finally can make component A.
The preparation method of B component is: 10 parts of 135 parts of the organopolysiloxane that during by 25 DEG C, viscosity is 200mpas, the hydrogen containing siloxane that hydrogen richness is 0.25%, 1,3,5,7-tetrem thiazolinyl-1,3,5,0.1 part, 7-tetramethyl-ring tetrasiloxane inhibitor joins in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min, mix de-bubbled; By median size be 30 μ m and 7 μ m in proportion 300 parts of composite mixing ball-aluminium oxides of 1:1 join in stirring tank, be greater than in vacuum tightness under the condition of 0.095MPa and stir 60min, finally can make B component.
Embodiment 1:
The preparation method of component A is: 1 part of 25 parts of single end-blocking vinyl silicone oil that when 120 parts, 25 DEG C of organopolysiloxane that during by 25 DEG C, viscosity is 200mpas, viscosity is 1000mpas, the Pt complex compound catalyst of 2000ppm join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min, mix de-bubbled; By median size be 30 μ m and 7 μ m in proportion 300 parts of composite mixing ball-aluminium oxides of 1:1 join in stirring tank, be greater than in vacuum tightness under the condition of 0.095MPa and stir 60min, finally can make component A.
The preparation method of B component is: 15 parts of 100 parts of the organopolysiloxane that during by 25 DEG C, viscosity is 200mpas, 30 parts of the hydrogen containing siloxanes that hydrogen richness is 0.25%, end hydrogen based polysiloxanes that hydrogen richness is 0.18%, 1,3,5,7-tetrem thiazolinyl-1,3,5,0.1 part, 7-tetramethyl-ring tetrasiloxane inhibitor joins in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min, mix de-bubbled; By median size be 30 μ m and 7 μ m in proportion 300 parts of composite mixing ball-aluminium oxides of 1:1 join in stirring tank, be greater than in vacuum tightness under the condition of 0.095MPa and stir 60min, finally can make B component.
Embodiment 2:
The preparation method of component A is: 1 part of 40 parts of single end-blocking vinyl silicone oil that when 105 parts, 25 DEG C of organopolysiloxane that during by 25 DEG C, viscosity is 200mpas, viscosity is 1000mpas, the Pt complex compound catalyst of 2000ppm join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min, mix de-bubbled; By median size be 30 μ m and 7 μ m in proportion 1000 parts of composite mixing ball-aluminium oxides of 1:1 join in stirring tank, be greater than in vacuum tightness under the condition of 0.095MPa and stir 90min, finally can make component A.
The preparation method of B component is: 30 parts of 100 parts of the organopolysiloxane that during by 25 DEG C, viscosity is 200mpas, 15 parts of the hydrogen containing siloxanes that hydrogen richness is 0.25%, end hydrogen based polysiloxanes that hydrogen richness is 0.18%, 1,3,5,7-tetrem thiazolinyl-1,3,5,0.1 part, 7-tetramethyl-ring tetrasiloxane inhibitor joins in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min, mix de-bubbled; By median size be 30 μ m and 7 μ m in proportion 1000 parts of composite mixing ball-aluminium oxides of 1:1 join in stirring tank, be greater than in vacuum tightness under the condition of 0.095MPa and stir 90min, finally can make B component.
By embodiment 1, embodiment 2, implement the A component prepared in comparative example and B component respectively in mass ratio 1:1 mix, press GB/T2794 test mixing viscosity, utilize the mould of the about 2mm of thickness left and right to prepare the print of the about 2mm of thickness, under 120 DEG C of conditions, solidify 10min, be cooled to the special cut-off knife of room temperature and be cut into dumbbell shape, by GB/T531 tested for hardness, by GB/T528 test tensile strength and elongation at break, press GB/T3399 test thermal conductivity, every test data is in table 1.
Test result shows: single end-blocking vinyl silicone oil and end hydrogen based polysiloxane are very obvious to the improvement of mechanical property, and lower hardness simultaneously elongation at break significantly increases.Select ball-aluminium oxide filler to have higher loading level, when thering is high heat conduction, still keep good mobility, coordinate single end-blocking vinyl silicone oil of suitable proportion and end hydrogen based polysiloxane can obtain all very excellent joint sealants of mechanical property and heat conductivility.
Table 1
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect have been carried out to further detailed description; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. the high heat conduction joint sealant of two components of mechanical property excellence, is characterized in that, described joint sealant comprises that mass mixing ratio is two components of A, B of 1:1;
Described component A is as follows by weight:
A
1. organopolysiloxane 100-120 part;
A
2. single end-blocking vinyl silicone oil 15-45 part;
A
3. catalyzer 0.1-5 part;
A
4. heat conductive filler 200-1200 part;
Described A
1structure in have at least two vinyl to be connected with Siliciumatom, 25 DEG C time, viscosity is 100-10000mpas, contents of ethylene is 0.1%-8.0%;
Described vinyl can be positioned at molecule chain end, molecular chain centre or molecule chain end and centre exists simultaneously;
Described A
2in the time of 25 DEG C, viscosity is 100-5000mpas, and contents of ethylene is 0.05%-0.8%;
Described vinyl is positioned at an end of molecular chain, and another end is methyl or hydroxyl;
Described A
3component is Pt complex compound, and part is 1,3-divinyl tetramethyl disiloxane, and the content of Pt is 5-2000ppm;
Described A
4select in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide at least one or several combinations;
Described B component is as follows by weight:
B
1. 100 parts of organopolysiloxane;
B
2. hydrogen containing siloxane 10-40 part;
B
3. end hydrogen based polysiloxane 5-25 part;
B
4. inhibitor 0.05-1 part;
B
5. heat conductive filler 200-1200 part;
Described B
1structure in have at least two vinyl to be connected with Siliciumatom, 25 DEG C time, viscosity is 100-10000mpas, contents of ethylene is 0.1%-8.0%;
Described vinyl can be positioned at molecule chain end, molecular chain centre or molecule chain end and centre exists simultaneously;
Described B
2in the time of 25 DEG C, viscosity is 10-100mpas, and hydrogen richness is 0.15%-1.6%;
Described hydrogen containing siloxane uses as linking agent, at least will contain three SiH groups in structure, is positioned in the middle of molecular chain;
Described B
3in the time of 25 DEG C, viscosity is 5-50mpas, and hydrogen richness is 0.09%-0.19%;
Described end hydrogen based polysiloxane uses as chainextender, contains two SiH groups in structure, is positioned at molecular chain two ends;
Described B
4select 1,3,5,7-tetrem thiazolinyl-1, at least one in 3,5,7-tetramethyl-ring tetrasiloxane, 1-ethynylcyclohexanol, 2-methylbutynol, DEF or diallyl maleate;
Described B
5select in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide at least one or several combinations.
2. the high heat conduction joint sealant of two components of mechanical property excellence as claimed in claim 1, is characterized in that, described heat conductive filler A
4and B
5form is spherical, adopts two kinds of particle diameters to carry out composite, and wherein small particle size scope is at 0.2-20 μ m, and large particle size range is at 20-50 μ m, and the compound proportion of large small particle size is 0.25-4:1.
3. the preparation method of two high heat conduction joint sealants of component as claimed in claim 1 or 2, is characterized in that:
The preparation method of described component A is: by the A of described proportioning
1, A
2, A
3join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min and mix de-bubbled, then by A
4component joins in stirring tank, is greater than under the condition of 0.095MPa stirs 60-90min in vacuum tightness;
The preparation method of described B component is: by the B of described proportioning
1, B
2, B
3, B
4join in planet stirring still, be greater than 0.095MPa in vacuum tightness, under temperature control 50-60 DEG C condition, stir 20min and mix de-bubbled, then by B
5component joins in stirring tank, is greater than under the condition of 0.095MPa stirs 60-90min in vacuum tightness.
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