CN103834352B - Two component height heat conduction joint sealants of excellent in mechanical performance and preparation method thereof - Google Patents
Two component height heat conduction joint sealants of excellent in mechanical performance and preparation method thereof Download PDFInfo
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Abstract
The present invention is two component height heat conduction joint sealants of a kind of excellent in mechanical performance and preparation method thereof, and this joint sealant comprises A, B two components that mass mixing ratio is 1:1; Component A counts organopolysiloxane 100-120 part by weight; Single end-blocking vinyl silicone oil 15-45 part; Catalyzer 0.1-5 part; Heat conductive filler 200-1200 part; B component counts organopolysiloxane 100 parts by weight; Hydrogen containing siloxane 10-40 part; End hydrogen based polysiloxane 5-25 part; Inhibitor 0.05-1 part; Heat conductive filler 200-1200 part.The present invention selects spherical heat conductive filler, by adding the loading level of heat conductive filler under the composite prerequisite not affecting mobility of particle diameter, obtains higher heat conductivility; Single end-blocking vinyl silicone oil and end hydrogen based polysiloxane is added in system, by the content of both changes, can regulate mechanical property (hardness, elongation at break), and then improve the performance such as shock resistance, cracking resistance, finally can obtain a kind of high heat conduction joint sealant of excellent in mechanical performance.
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, ensure the mobility of joint sealant while improving thermal conductivity as far as possible, adding single end-blocking vinyl silicone oil and end hydrogen based polysiloxane on the other hand, obtaining 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.Simultaneously in order to prevent moisture, dust and obnoxious flavour to the intrusion of electronic devices and components, slow down vibrations, prevent external force damage components and parts, a kind of heat conductivility is good, the electron pouring sealant demand of excellent in mechanical performance is more and more very urgent.
Addition-type silicon rubber not only can room temperature vulcanization but also sulfuration of can heating, and sulfidation does not discharge low molecule by product, had that shrinking percentage is little, an advantage such as deep layer vulcanization and crosslinking structure are easily controlled simultaneously, was acknowledged as the preferred material of electron pouring sealant.Unfilled silicon rubber thermal conductivity only has about 0.2W/mK, the effective ways of current raising silicon rubber heat conductivility 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) needs 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.A kind of electronics heat conductive flame-retarding silicon rubber disclosed in 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.Disclosed in another patent of invention 201110237351.0 of China, a kind of additive high-thermal-conductivity organic silicon electronic pouring sealant thermal conductivity is greater than 1.0W/mK, and there is good mobility, can be used for embedding, but its mechanical property needs to improve, hardness can be caused to increase while being filled in of a large amount of heat conductive filler obtains good heat conductive performance and the remarkable reduction of elongation at break, can greatly affect like this performances, particularly high rigidity such as the shock resistance of joint sealant and cracking resistance and low elongation at break for opposing external shock power and vibrations, prevent cracking all very unfavorable.
Summary of the invention
The object of the invention is to overcome the mobility caused when using general heat conductive filler loading level larger and reduce problem, have selected spherical heat conductive filler, and by adding the loading level of heat conductive filler under the composite prerequisite not affecting mobility of particle diameter, obtain higher heat conductivility; Simultaneously by single end-blocking vinyl silicone oil and end hydrogen based polysiloxane with the use of, lifting is optimized to the body mechanical property of joint sealant.
In order to realize object of the present invention, propose a kind of two component height heat conduction joint sealants of excellent in mechanical performance, described joint sealant comprises A, B two components that mass mixing ratio is 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, when 25 DEG C, viscosity is 100-10000mpas, and 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
225 DEG C time, 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 at least one or several combinations in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide;
Described B component is as follows by weight:
B
1. organopolysiloxane 100 parts;
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, when 25 DEG C, viscosity is 100-10000mpas, and 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
225 DEG C time, 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, be positioned in the middle of molecular chain in structure;
Described B
325 DEG C time, viscosity is 5-50mpas, and hydrogen richness is 0.09%-0.19%.Described end hydrogen based polysiloxane uses as chainextender, containing two SiH groups in structure, is positioned at molecular chain two ends;
Described B
4select at least one in 1,3,5,7-tetravinyl-1,3,5,7-tetramethyl-ring tetrasiloxane, 1-ethynylcyclohexanol, 2-methylbutynol, DEF or diallyl maleate;
Described B
5select at least one or several combinations in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide.
Described heat conductive filler A
4and B
5form is spherical, and adopt two kinds of particle diameters to carry out composite, wherein small particle size scope is at 0.2-20 μm, and Large stone scope is at 20-50 μm, and the compound proportion of large small particle size is 0.25-4:1.
The present invention also proposes the method preparing described pair of component height heat conduction joint sealant, 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, stir 20min under temperature control 50-60 DEG C condition and mix de-bubbled, then by A
4component joins in stirring tank, stirs 60-90min under being greater than the condition of 0.095MPa 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, stir 20min under temperature control 50-60 DEG C condition and mix de-bubbled, then by B
5component joins in stirring tank, stirs 60-90min under being greater than the condition of 0.095MPa in vacuum tightness.
Beneficial effect of the present invention: first the present invention selects spherical heat conductive filler, by adding 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 the content of both changes, can regulate mechanical property (hardness, elongation at break), and then improve the performance such as shock resistance, cracking resistance, finally can obtain a kind of high heat conduction joint sealant of excellent in mechanical performance.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, the present invention is described in more detail.
Implement comparative example:
The preparation method of component A is: be the organopolysiloxane 145 parts of 200mpas by viscosity when 25 DEG C, the Pt complex compound catalyst 1 part of 2000ppm joins in planet stirring still, 0.095MPa is greater than in vacuum tightness, stir 20min under temperature control 50-60 DEG C condition, mix de-bubbled; Be that 30 μm and 7 μm of mixing ball-aluminium oxides 300 parts that 1:1 is composite in proportion join in stirring tank by median size, stir 60min be greater than the condition of 0.095MPa in vacuum tightness under, finally can obtain component A.
The preparation method of B component is: be the organopolysiloxane 135 parts of 200mpas by viscosity when 25 DEG C, hydrogen richness be 0.25% hydrogen containing siloxane 10 parts, 1,3,5,7-tetravinyl-1,3,5,0.1 part, 7-tetramethyl-ring tetrasiloxane inhibitor joins in planet stirring still, be greater than 0.095MPa in vacuum tightness, stir 20min under temperature control 50-60 DEG C condition, mix de-bubbled; Be that 30 μm and 7 μm of mixing ball-aluminium oxides 300 parts that 1:1 is composite in proportion join in stirring tank by median size, stir 60min be greater than the condition of 0.095MPa in vacuum tightness under, finally can obtain B component.
Embodiment 1:
The preparation method of component A is: by viscosity when 25 DEG C be the organopolysiloxane 120 parts of 200mpas, 25 DEG C time viscosity be single end-blocking vinyl silicone oil 25 parts of 1000mpas, the Pt complex compound catalyst 1 part of 2000ppm joins in planet stirring still, 0.095MPa is greater than in vacuum tightness, stir 20min under temperature control 50-60 DEG C condition, mix de-bubbled; Be that 30 μm and 7 μm of mixing ball-aluminium oxides 300 parts that 1:1 is composite in proportion join in stirring tank by median size, stir 60min be greater than the condition of 0.095MPa in vacuum tightness under, finally can obtain component A.
The preparation method of B component is: be the organopolysiloxane 100 parts of 200mpas by viscosity when 25 DEG C, the hydrogen richness hydrogen containing siloxane 30 parts that is 0.25%, the hydrogen richness end hydrogen based polysiloxane 15 parts, 1 that is 0.18%, 3,5,7-tetravinyl-1,3,5,0.1 part, 7-tetramethyl-ring tetrasiloxane inhibitor joins in planet stirring still, be greater than 0.095MPa in vacuum tightness, stir 20min under temperature control 50-60 DEG C condition, mix de-bubbled; Be that 30 μm and 7 μm of mixing ball-aluminium oxides 300 parts that 1:1 is composite in proportion join in stirring tank by median size, stir 60min be greater than the condition of 0.095MPa in vacuum tightness under, finally can obtain B component.
Embodiment 2:
The preparation method of component A is: by viscosity when 25 DEG C be the organopolysiloxane 105 parts of 200mpas, 25 DEG C time viscosity be single end-blocking vinyl silicone oil 40 parts of 1000mpas, the Pt complex compound catalyst 1 part of 2000ppm joins in planet stirring still, 0.095MPa is greater than in vacuum tightness, stir 20min under temperature control 50-60 DEG C condition, mix de-bubbled; Be that 30 μm and 7 μm of mixing ball-aluminium oxides 1000 parts that 1:1 is composite in proportion join in stirring tank by median size, stir 90min be greater than the condition of 0.095MPa in vacuum tightness under, finally can obtain component A.
The preparation method of B component is: be the organopolysiloxane 100 parts of 200mpas by viscosity when 25 DEG C, the hydrogen richness hydrogen containing siloxane 15 parts that is 0.25%, the hydrogen richness end hydrogen based polysiloxane 30 parts, 1 that is 0.18%, 3,5,7-tetravinyl-1,3,5,0.1 part, 7-tetramethyl-ring tetrasiloxane inhibitor joins in planet stirring still, be greater than 0.095MPa in vacuum tightness, stir 20min under temperature control 50-60 DEG C condition, mix de-bubbled; Be that 30 μm and 7 μm of mixing ball-aluminium oxides 1000 parts that 1:1 is composite in proportion join in stirring tank by median size, stir 90min be greater than the condition of 0.095MPa in vacuum tightness under, finally can obtain B component.
By embodiment 1, embodiment 2, implement the component A prepared in comparative example and B component respectively in mass ratio 1:1 mix, by GB/T2794 test mixing viscosity, the print that thickness is about 2mm prepared by the mould utilizing thickness to be about about 2mm, 10min is solidified under 120 DEG C of conditions, 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, test thermal conductivity by GB/T3399, every test data is in table 1.
Test result shows: to the improvement of mechanical property clearly, hardness reduces elongation at break simultaneously and significantly increases for single end-blocking vinyl silicone oil and end hydrogen based polysiloxane.Spherical alumina Al filler is selected to have higher loading level, still keep good mobility while there is high heat conduction, coordinate single end-blocking vinyl silicone oil of suitable proportion and end hydrogen based polysiloxane can obtain mechanical property and all very excellent joint sealant of heat conductivility.
Table 1.
Above-described specific embodiment; further detailed description has been carried out to object of the present invention, technical scheme and beneficial effect; be 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 made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. two component height heat conduction joint sealants for excellent in mechanical performance, is characterized in that: described joint sealant comprises A, B two components that mass mixing ratio is 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, when 25 DEG C, viscosity is 100-10000mPas, and contents of ethylene is 0.1%-8.0%;
Described vinyl is positioned at molecule chain end, molecular chain centre or molecule chain end and centre exists simultaneously;
Described A
225 DEG C time, 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 at least one or several combinations in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide;
Described B component is as follows by weight:
B
1. organopolysiloxane 100 parts;
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, when 25 DEG C, viscosity is 100-10000mPas, and contents of ethylene is 0.1%-8.0%;
Described vinyl is positioned at molecule chain end, molecular chain centre or molecule chain end and centre exists simultaneously;
Described B
225 DEG C time, 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, be positioned in the middle of molecular chain in structure;
Described B
325 DEG C time, viscosity is 5-50mPas, and hydrogen richness is 0.09%-0.19%;
Described end hydrogen based polysiloxane uses as chainextender, containing two SiH groups in structure, is positioned at molecular chain two ends;
Described B
4select at least one in 1,3,5,7-tetravinyl-1,3,5,7-tetramethyl-ring tetrasiloxane, 1-ethynylcyclohexanol, 2-methylbutynol, DEF or diallyl maleate;
Described B
5select at least one or several combinations in aluminum oxide, silicon powder, aluminium nitride, boron nitride and silicon carbide;
Described heat conductive filler A
4and B
5form is spherical, and adopt two kinds of particle diameters to carry out composite, wherein small particle size scope is at 0.2-20 μm, and Large stone scope is at 20-50 μm, and the compound proportion of large small particle size is 0.25-4:1.
2. prepare the method for two component height heat conduction joint sealant as claimed in claim 1, it 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, stir 20min under temperature control 50-60 DEG C condition and mix de-bubbled, then by A
4component joins in stirring tank, stirs 60-90min under being greater than the condition of 0.095MPa 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, stir 20min under temperature control 50-60 DEG C condition and mix de-bubbled, then by B
5component joins in stirring tank, stirs 60-90min under being greater than the condition of 0.095MPa in vacuum tightness.
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