CN105566920A - Low-oil-permeability super-soft thermally-conductive silica gel composition and thermally-conductive silica gel gasket and preparation method thereof - Google Patents
Low-oil-permeability super-soft thermally-conductive silica gel composition and thermally-conductive silica gel gasket and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The present invention relates to a low-oil-permeability super-soft thermally-conductive silica gel composition and a thermally-conductive silica gel gasket, the low-oil-permeability super-soft thermally-conductive silica gel composition comprising a first liquid silica gel, a second liquid silica gel and a thermally-conductive filler, the thermally-conductive silica gel gasket is prepared from the low-oil-permeability super-soft thermally-conductive silica gel composition, the low-oil-permeability super-soft thermally-conductive silica gel composition is prepared from the following components by mass: 7 to 11.9% of a first liquid silica gel and second liquid silica gel mixed liquid, 88 to 92.9% of the thermally-conductive filler, 0.05 to 0.5% of a catalyst and 0.05 to 0.5% of an inhibitor by the preparation method comprising stirring, rolling, vulcanizing and cutting; the low-oil-permeability super-soft thermally-conductive silica gel composition is prepared by mixing the first liquid silica gel, the second liquid silica gel and the thermally-conductive filler, vinyl silicone oil and a platinum catalyst in the first liquid silica gel and vinyl silicone oil and hydrogen-containing silicone oil in the second liquid silica gel can make the prepared plastic material characterized by being low in oil permeability and low in hardness, and the like, the viscosity of the first liquid silica gel and the second liquid silica gel are 3000mPa. s-10000mPa.s, uniform mixing of the material and the thermally-conductive filler during stirring can be guaranteed, and an appropriate crosslinking degree can be achieved during the vulcanizing.
Description
Technical field
The present invention relates to heat conductive silica gel field, particularly relate to low oil impregnate ultra-soft heat conductive silica gel composition and heat conductive silica gel pad and preparation method thereof.
Background technology
In electronic product, the electronic components such as central processing unit (CPU) (CPU), transistor and photodiode (LED) can generate heat at work in a large number, if the improper meeting of cooling measure makes component temperature too high, cause its serviceability to decline and even damage.Therefore, needing, on the element of heating, heat abstractor is installed, as radiator fan or copper billet etc., between heat abstractor and Heating element, usually filling plasticity heat conductor, as silica gel pad etc., for promoting the heat transmission between Heating element and heat abstractor; Usually, in order to obtain better heat-conducting effect, need the hardness reducing thermally conductive material, to obtain larger rate of compression, less thermally-conductive interface thickness and better infiltrate contact interface and fit.For silica-gel composition pad, silica gel that viscosity is little generally can be selected as matrix, to obtain softer pad product; Meanwhile, be also convenient to add a large amount of thermal conductivity inorganic powder wherein, to obtain stronger heat conductivility.
But softer its state of cure of silica-gel composition pad is also lower, be heated be easy to occur silicone oil ooze out, cause silicone oil migrates pollute components and parts.At present, on market, common heat-conducting pad oil impregnate rate is about 2.5% ~ 3.5%, and good product can control between 2.0% ~ 2.5%, and the product of oil impregnate rate below 2% does not have substantially.
Summary of the invention
The technical problem to be solved in the present invention is to provide low oil impregnate ultra-soft heat conductive silica gel composition and heat conductive silica gel pad and preparation method thereof, solves existing silica-gel composition pad and there is the problem that silicone oil oozes out.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions: low oil impregnate ultra-soft heat conductive silica gel composition, comprise first liquid silica gel, second liquid silica gel and heat conductive filler, the mass ratio of first liquid silica gel and second liquid silica gel is 1:0.6 ~ 1:1.4, and the viscosity of first liquid silica gel and second liquid silica gel is 3000mPa.s ~ 10000mPa.s;
First liquid silica gel includes vinyl silicone oil and platinum catalyst, and the mass percent of platinum catalyst in first liquid silica gel is 0.5% ~ 5%;
Second liquid silica gel includes vinyl silicone oil and containing hydrogen silicone oil, and the mass percent of containing hydrogen silicone oil in second liquid silica gel is 2 ~ 5%, and in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2 ~ 0.5%.
Preferably, heat conductive filler comprises the component of following mass percent: the spherical heat conductive filler 20 ~ 50% that the spherical heat conductive filler 40 ~ 70% that particle diameter is 40 μm ~ 50 μm, particle diameter are 3 μm ~ 10 μm, particle diameter are the aspherical heat conductive filler 5 ~ 20% of 0.2 μm ~ 5 μm, the heat conductive filler of different-grain diameter size can improve its filling ratio further, thus improves thermal conductivity further; To arrange in pairs or groups a certain amount of aspherical heat conductive filler simultaneously, utilize the feature that aspherical heat conductive filler specific surface area is large, oil absorption is strong, reduce oil impregnate rate further.
Heat conductive silica gel pad, comprises the component of following mass percent: the mixed solution 7 ~ 11.9% of first liquid silica gel and second liquid silica gel, heat conductive filler 88 ~ 92.9%, catalyzer 0.05 ~ 0.5%, inhibitor 0.05 ~ 0.5%; The mass ratio of first liquid silica gel and second liquid silica gel is 1:0.9 ~ 1:1.1, Silicon Containing Hydrogen oil viscosity is 200 ~ 500mPa.s, can not discharge lower-molecular substance, reduce oil impregnate, the mass ratio of first liquid silica gel and second liquid silica gel is that 1:0.9 ~ 1:1.1 can reduce oil impregnate further.
Preferably, heat conductive filler is the one in aluminum oxide, magnesium oxide, zinc oxide, aluminium powder, aluminium nitride or boron nitride, has sphericity high, filling ratio advantages of higher, with liquid silastic mixing process, has better dispersion effect.
Preferably, heat conductive filler is through coupling agent treatment, and the heat conductive filler after coupling agent surface modification, its dispersiveness and bounding force can improve, and the interface interaction between organic matrix improves, and can improve the capacity of heat transmission further.
Preferably, catalyzer is the one in platinum catalyst, ruthenium complex catalyst, using rhodium complex catalysts or organotin, inhibitor is 1-ethynyl-1-hexalin, catalyzer can promote being cross-linked between vinyl component and silicon hydrogen component, namely the sulfuration of silica gel is promoted, after inhibitor can make vinyl component and the mixing of silicon hydrogen component, under normal temperature, (20 DEG C) are long-time is not cross-linked or delay cross linking, and temperature Quick cross-linking when reaching curing temperature, can ensure before sulfuration, add enough heat conductive fillers in liquid silica gel and fully mixing.
A preparation method for heat conductive silica gel pad, comprises the following steps:
Step 1: first liquid silica gel, second liquid silica gel, inhibitor, heat conductive filler, catalyzer are added to stirring tank successively and stir, obtain sizing material, temperature in stirring tank is 20 ~ 35 DEG C, low vacuum in stirring tank is in-0.09MPa, stirring velocity is 25 ~ 45RPM, and the timed interval of adding between each component is 10min;
Step 2: the sizing material calendering formation process that step 1 is obtained;
Step 3: the product of step 2 calendering process is carried out sulfidizing, curing temperature 110 ~ 130 DEG C, curing time 25 ~ 35min;
Step 4: the product after step 3 sulfidizing is carried out cutting process.
In sum, advantage of the present invention: the low oil impregnate ultra-soft heat conductive silica gel composition be mixed by first liquid silica gel, second liquid silica gel and heat conductive filler, by the vinyl silicone oil in first liquid silica gel and platinum catalyst, vinyl silicone oil in second liquid silica gel and containing hydrogen silicone oil make the sizing material made have the feature of low oil impregnate and soft, the viscosity of first liquid silica gel and second liquid silica gel is 3000mPa.s ~ 10000mPa.s, can mix with heat conductive filler when can ensure material stirring, the crosslinking degree be mostly suitable for during sulfuration can be made.
By the mixed solution of first liquid silica gel and second liquid silica gel, heat conductive filler, catalyzer, the heat conductive silica gel pad that inhibitor is made, the hardness of its heat conductive silica gel pad is shore00<10, oil impregnate rate is less than 2%, substantially increase work-ing life, catalyzer can promote being cross-linked between vinyl component and silicon hydrogen component, namely the sulfuration of silica gel is promoted, after inhibitor can make vinyl component and the mixing of silicon hydrogen component, under normal temperature, (20 DEG C) are long-time is not cross-linked or delay cross linking, and temperature Quick cross-linking when reaching curing temperature, can ensure before sulfuration, enough heat conductive fillers are added and fully mixing in liquid silica gel.
Embodiment
Low oil impregnate ultra-soft heat conductive silica gel composition, comprise first liquid silica gel, second liquid silica gel and heat conductive filler, the mass ratio of first liquid silica gel and second liquid silica gel is 1:0.6 ~ 1:1.4, and the viscosity of first liquid silica gel and second liquid silica gel is 3000mPa.s ~ 10000mPa.s;
First liquid silica gel includes vinyl silicone oil and platinum catalyst, and the mass percent of platinum catalyst in first liquid silica gel is 0.5% ~ 5%;
Second liquid silica gel includes vinyl silicone oil and containing hydrogen silicone oil, and the mass percent of containing hydrogen silicone oil in second liquid silica gel is 2 ~ 5%, and in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2 ~ 0.5%; Heat conductive filler comprises the component of following mass percent: the spherical heat conductive filler 20 ~ 50% that the spherical heat conductive filler 40 ~ 70% that particle diameter is 40 μm ~ 50 μm, particle diameter are 3 μm ~ 10 μm, particle diameter are the aspherical heat conductive filler 5 ~ 20% of 0.2 μm ~ 5 μm.
Embodiment one:
A kind of heat conductive silica gel pad, comprise the component of following mass percent: the mixed solution 11% of first liquid silica gel and second liquid silica gel, heat conductive filler 88.5%, platinum catalyst 0.2%, 1-ethynyl-1-hexalin 0.3%, the viscosity of first liquid silica gel and second liquid silica gel is 3000mPa.s;
Wherein: the mass ratio of first liquid silica gel and second liquid silica gel is 1:0.6, first liquid silica gel comprises vinyl silicone oil 99% and platinum catalyst 1%, second liquid silica gel comprises vinyl silicone oil 98% and containing hydrogen silicone oil 2%, in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2%, heat conductive filler is aluminum oxide, and the aspherical aluminum oxide 10% that the ball-aluminium oxide 30% that it be ball-aluminium oxide 60%, the particle diameter of 40 μm ~ 50 μm is 3 μm ~ 10 μm that heat conductive filler comprises particle diameter, particle diameter are 0.2 μm ~ 5 μm.
A preparation method for heat conductive silica gel pad, comprises the following steps:
Step 1: stir 10min add first liquid silica gel and second liquid silica gel in stirring tank after, then in stirring tank, add 1-ethynyl-1-hexalin inhibitor, and stir 10min, in stirring tank, add heat conductive filler again, stir 10min, in the most backward stirring tank, add platinum catalyst, sizing material is obtained after stirring 10min, whipping temp is 30 DEG C, and the vacuum tightness in stirring tank is-0.08MPa, and stirring velocity is 30RPM;
Step 2: the sizing material calendering formation process that step 1 is obtained;
Step 3: the product of step 2 calendering process is carried out sulfidizing, curing temperature 120 DEG C, curing time 30min;
Step 4: the product after step 3 sulfidizing is carried out cutting process.
Embodiment two:
A kind of heat conductive silica gel pad as described in embodiment one, the present embodiment has following difference: the component comprising following mass percent: the mixed solution 11% of first liquid silica gel and second liquid silica gel, heat conductive filler 88.5%, platinum catalyst 0.2%, 1-ethynyl-1-hexalin 0.3%, and the viscosity of first liquid silica gel and second liquid silica gel is 5000mPa.s;
Wherein: the mass ratio of first liquid silica gel and second liquid silica gel is 1:0.8, first liquid silica gel comprises vinyl silicone oil 99% and platinum catalyst 1%, second liquid silica gel comprises vinyl silicone oil 98% and containing hydrogen silicone oil 2%, in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2%, heat conductive filler is aluminum oxide, and the aspherical aluminum oxide 10% that the ball-aluminium oxide 30% that it be ball-aluminium oxide 60%, the particle diameter of 40 μm ~ 50 μm is 3 μm ~ 10 μm that heat conductive filler comprises particle diameter, particle diameter are 0.2 μm ~ 5 μm.
A preparation method for heat conductive silica gel pad, comprises the following steps:
Step 1: stir 10min add first liquid silica gel and second liquid silica gel in stirring tank after, then in stirring tank, add 1-ethynyl-1-hexalin inhibitor, and stir 10min, in stirring tank, add heat conductive filler again, stir 10min, in the most backward stirring tank, add platinum catalyst, sizing material is obtained after stirring 10min, whipping temp is 30 DEG C, and the vacuum tightness in stirring tank is-0.08MPa, and stirring velocity is 30RPM;
Step 2: the sizing material calendering formation process that step 1 is obtained;
Step 3: the product of step 2 calendering process is carried out sulfidizing, curing temperature 120 DEG C, curing time 30min;
Step 4: the product after step 3 sulfidizing is carried out cutting process.
Embodiment three:
A kind of heat conductive silica gel pad as described in embodiment one, two, the present embodiment has following difference: the component comprising following mass percent: the mixed solution 10% of first liquid silica gel and second liquid silica gel, heat conductive filler 89.5%, platinum catalyst 0.2%, 1-ethynyl-1-hexalin 0.3%, and the viscosity of first liquid silica gel and second liquid silica gel is 8000mPa.s;
Wherein: the mass ratio of first liquid silica gel and second liquid silica gel is 1:1, first liquid silica gel comprises vinyl silicone oil 99% and platinum catalyst 1%, second liquid silica gel comprises vinyl silicone oil 98% and containing hydrogen silicone oil 2%, in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2%, heat conductive filler is aluminum oxide, and the aspherical aluminum oxide 20% that the ball-aluminium oxide 20% that it be ball-aluminium oxide 60%, the particle diameter of 40 μm ~ 50 μm is 3 μm ~ 10 μm that heat conductive filler comprises particle diameter, particle diameter are 0.2 μm ~ 5 μm.
A preparation method for heat conductive silica gel pad, comprises the following steps:
Step 1: stir 10min add first liquid silica gel and second liquid silica gel in stirring tank after, then in stirring tank, add 1-ethynyl-1-hexalin inhibitor, and stir 10min, in stirring tank, add heat conductive filler again, stir 10min, in the most backward stirring tank, add platinum catalyst, sizing material is obtained after stirring 10min, whipping temp is 30 DEG C, and the vacuum tightness in stirring tank is-0.08MPa, and stirring velocity is 30RPM;
Step 2: the sizing material calendering formation process that step 1 is obtained;
Step 3: the product of step 2 calendering process is carried out sulfidizing, curing temperature 120 DEG C, curing time 30min;
Step 4: the product after step 3 sulfidizing is carried out cutting process.
Embodiment four:
A kind of heat conductive silica gel pad as described in embodiment one, two, three, the present embodiment has following difference: the component comprising following mass percent: the mixed solution 10% of first liquid silica gel and second liquid silica gel, heat conductive filler 89.5%, platinum catalyst 0.2%, 1-ethynyl-1-hexalin 0.3%, and the viscosity of first liquid silica gel and second liquid silica gel is 10000mPa.s;
Wherein: the mass ratio of first liquid silica gel and second liquid silica gel is 1:1.2, first liquid silica gel comprises vinyl silicone oil 99% and platinum catalyst 1%, second liquid silica gel comprises vinyl silicone oil 98% and containing hydrogen silicone oil 2%, in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2%, heat conductive filler is aluminum oxide, and the aspherical aluminum oxide 20% that the ball-aluminium oxide 20% that it be ball-aluminium oxide 60%, the particle diameter of 40 μm ~ 50 μm is 3 μm ~ 10 μm that heat conductive filler comprises particle diameter, particle diameter are 0.2 μm ~ 5 μm.
A preparation method for heat conductive silica gel pad, comprises the following steps:
Step 1: stir 10min add first liquid silica gel and second liquid silica gel in stirring tank after, then in stirring tank, add 1-ethynyl-1-hexalin inhibitor, and stir 10min, in stirring tank, add heat conductive filler again, stir 10min, in the most backward stirring tank, add platinum catalyst, sizing material is obtained after stirring 10min, whipping temp is 30 DEG C, and the vacuum tightness in stirring tank is-0.08MPa, and stirring velocity is 30RPM;
Step 2: the sizing material calendering formation process that step 1 is obtained;
Step 3: the product of step 2 calendering process is carried out sulfidizing, curing temperature 120 DEG C, curing time 30min;
Step 4: the product after step 3 sulfidizing is carried out cutting process.
Oil impregnate rate and hardness test are carried out to the heat conductive silica gel pad that embodiment one, embodiment two, embodiment three, embodiment four obtain, test result as shown in Table 1:
| Embodiment one | Embodiment two | Embodiment three | Embodiment four | |
| Oil impregnate rate | 1.42％ | 1.31％ | 1.14％ | 0.98％ |
| Shore hardness | 5shore 00 | 6shore 00 | 7shore 00 | 9shore 00 |
| Thermal conductivity | 1.22w/m.k | 1.21w/m.k | 1.33w/m.k | 1.35w/m.k |
Table one
Oil impregnate rate in above-described embodiment and hardness data are tested by following methods and are obtained.
Oil impregnate rate testing method is:
Heat conductive silica gel pad is cut into the size of 30mm × 30mm × 1.0mm, weighs and record data m1;
At the equal placement of multiple layers oil-Absorbing Sheets in heat conductive silica gel pad two sides, ensure that the silicone oil oozed out can be completely absorbed, then heat conductive silica gel pad and oil-Absorbing Sheets are clamped as between two blocks of aluminium sheets, by heat conductive silica gel spacer thickness compression 30%, put into 120 DEG C of baking boxs and toast 48H continuously;
Heat conductive silica gel pad through previous step process is taken out and weighs, record data m2;
Oil impregnate rate=(m1-m2)/m1, calculates the oil impregnate rate of this silica gel heat-conducting pad.
Hardness measuring method: ASTM-D2240 standard.
Except above preferred embodiment, the present invention also has other embodiment, and those skilled in the art can make various change and distortion according to the present invention, only otherwise depart from spirit of the present invention, all should belong to the scope that claims of the present invention define.
Claims (7)
1. low oil impregnate ultra-soft heat conductive silica gel composition, it is characterized in that: comprise first liquid silica gel, second liquid silica gel and heat conductive filler, the mass ratio of first liquid silica gel and second liquid silica gel is 1:0.6 ~ 1:1.4, and the viscosity of first liquid silica gel and second liquid silica gel is 3000mPa.s ~ 10000mPa.s;
First liquid silica gel includes vinyl silicone oil and platinum catalyst, and the mass percent of platinum catalyst in first liquid silica gel is 0.5% ~ 5%;
Second liquid silica gel includes vinyl silicone oil and containing hydrogen silicone oil, and the mass percent of containing hydrogen silicone oil in second liquid silica gel is 2 ~ 5%, and in containing hydrogen silicone oil, the molar percentage of reactive hydrogen is 0.2 ~ 0.5%.
2. low oil impregnate ultra-soft heat conductive silica gel composition according to claim 1, is characterized in that: heat conductive filler comprises the component of following mass percent: the spherical heat conductive filler 20 ~ 50% that the spherical heat conductive filler 40 ~ 70% that particle diameter is 40 μm ~ 50 μm, particle diameter are 3 μm ~ 10 μm, particle diameter are the aspherical heat conductive filler 5 ~ 20% of 0.2 μm ~ 5 μm.
3. the heat conductive silica gel pad made of low oil impregnate ultra-soft heat conductive silica gel composition as defined in claim 1, is characterized in that: the component comprising following mass percent: the mixed solution 7 ~ 11.9% of first liquid silica gel and second liquid silica gel, heat conductive filler 88 ~ 92.9%, catalyzer 0.05 ~ 0.5%, inhibitor 0.05 ~ 0.5%;
The mass ratio of first liquid silica gel and second liquid silica gel is 1:0.9 ~ 1:1.1, and Silicon Containing Hydrogen oil viscosity is 200 ~ 500mPa.s.
4. heat conductive silica gel pad according to claim 3, is characterized in that: heat conductive filler is the one in aluminum oxide, magnesium oxide, zinc oxide, aluminium powder, aluminium nitride or boron nitride.
5. heat conductive silica gel pad according to claim 3, is characterized in that: heat conductive filler is through coupling agent treatment.
6. heat conductive silica gel pad according to claim 3, is characterized in that: catalyzer is the one in platinum catalyst, ruthenium complex catalyst, using rhodium complex catalysts or organotin, and inhibitor is 1-ethynyl-1-hexalin.
7. the preparation method that adopts of heat conductive silica gel pad as claimed in claim 3, is characterized in that: comprise the following steps:
Step 1: stir 10min add first liquid silica gel and second liquid silica gel in stirring tank after, then in stirring tank, add 1-ethynyl-1-hexalin inhibitor, and stir 10min, in stirring tank, add heat conductive filler again, stir 10min, in the most backward stirring tank, add platinum catalyst, sizing material is obtained after stirring 10min, temperature in stirring tank is 20 ~ 35 DEG C, and the low vacuum in stirring tank is in-0.09MPa, and stirring velocity is 25 ~ 45RPM;
Step 2: the sizing material calendering formation process that step 1 is obtained;
Step 3: the product of step 2 calendering process is carried out sulfidizing, curing temperature 110 ~ 130 DEG C, curing time 25 ~ 35min;
Step 4: the product after step 3 sulfidizing is carried out cutting process.
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