CN105419723B - A kind of crosslinkable one pack system heat conduction can dispensing - Google Patents
A kind of crosslinkable one pack system heat conduction can dispensing Download PDFInfo
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- CN105419723B CN105419723B CN201510988369.2A CN201510988369A CN105419723B CN 105419723 B CN105419723 B CN 105419723B CN 201510988369 A CN201510988369 A CN 201510988369A CN 105419723 B CN105419723 B CN 105419723B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of crosslinkable one pack system heat conduction can dispensing, include following mass percent component composition:The liquid silica gel 5~15% of epoxy-functional, the liquid silica gel 0.5~2% of vinyl-functional, containing hydrogen silicone oil 0.5~2%, catalyst 0.05~0.5%, remaining be heat filling；The viscosity of the liquid silica gel of epoxy-functional is 50~5000mPas, and the viscosity of the liquid silica gel of vinyl-functional is 200~5000mPas；Advantages of the present invention：A kind of crosslinkable one pack system heat conduction provided by the invention can dispensing, the components such as liquid silica gel, containing hydrogen silicone oil and the heat filling of liquid silica gel, vinyl-functional including epoxy-functional, addition reaction can occur for the liquid silica gel and containing hydrogen silicone oil of vinyl-functional, by adjusting its viscosity and component ratio, the product with Suitable flow rate can be obtained, and it can for a long time keep turnover rate constant at normal temperatures, it is ensured that product remains able to normally extrude dispensing after long-term storage.
Description
Technical field
The present invention relates to heat-conducting interface material technical field, more particularly to a kind of crosslinkable one pack system heat conduction can dispensing.
Background technology
In heat-conducting interface material field, Heat Conduction Material has can dispensing form and solid shim form etc..Solid gasket type
Heat Conduction Material is mostly sheet form, is pressed between heater members surface and radiating element surface；Can dispensing form heat conduction
Material has certain mobility, and storage in a reservoir, is extruded and is applied on thermally-conductive interface by pipe or syringe.Can dispensing shape
The Heat Conduction Material of formula has many advantages, such as e.g., there is certain mobility, be suitable for different compared with the Heat Conduction Material of solid shim form
Shape and gap, reduce waste of material；And for example, well, lower interface resistance can be achieved in the infiltration to device surface；For another example, easily
In the production for realizing automation, production efficiency is improved.Thus, can dispensing form Heat Conduction Material have be widely applied very much.
But can the Heat Conduction Material of dispensing form also have the shortcomings that certain, i.e. when this kind of Heat Conduction Material be filled in it is larger
When between gap (1.0~2.0mm or more), easily occur creep, Heat Conduction Material, which can not hold its shape, shape and to be held in place
Put.Particularly when the gap between heater members and radiating element surface in vertical direction when, it is easier to creep occurs.In addition,
Variation of ambient temperature and vibration can also have an impact to Heat Conduction Material from shape retention, can make Heat Conduction Material along vertical
Direction is slided and leaves original position, causes its heat conduction disabler, causes heater members temperature to raise, and may finally lead
Cause its damage.
In view of the above-mentioned problems, prior art has a variety of settling modes, basic thinking be all make can dispensing have at certain
Under the conditions of the characteristic that solidifies, after dispensing operation terminates, colloid solidifies under certain condition, so as to avoid that creep and position occurs
Move.
Such as Chinese patent application CN201110414862.5, a kind of high temperature curing monocomponent heat-conduction flame-retardation electronic pouring sealant and
Its preparation method, by catalyst as in microcapsule-type, capsule will not discharge catalyst under normal temperature, make colloid can be at normal temperatures
Preserve；And at high temperature, the housing of microcapsules can melt and discharge catalyst, be catalyzed embedding adhesive curing, and such a scheme lacks
Putting is：First, because the material of capsule shells can not be dissolved in silica gel, and the capsule shell material performance melted under high temperature can change,
Influence the performance of heat conductive silica gel.2nd, due to being filled with the ceramic powders of a large amount of high rigidity in heat conductive silica gel, the broken of capsule is easily caused
Split, capsules break may occur during processing or mixing or catalyst oozes out, cause silica gel premature cure, influence
Normal production and use.3rd, it is the cost of platinum catalyst microencapsulation is higher.
And for example, Chinese patent application CN201210575815.3, a kind of one-component are heating and curing liquid silastic and its system
Preparation Method.The technical scheme of this application is that, using alkynes alcohol-based mixtures as polymerization inhibitor, the one-component that can be stored at normal temperatures adds
Heat cure liquid silastic, treat that polymerization inhibitor volatilization is i.e. curable after dispensing.The shortcomings that such a scheme is：First, only in polymerization inhibitor
Silica gel could solidify after volatilization, be only suitable for being applied to shallow layer, coating thicker (0.5mm and more than) or applied in closure means
When, because polymerization inhibitor is not volatile, cause silica gel to be difficult to solidify.2nd, the polymerization inhibitor of volatilization has an impact to the performance of electronic device.
3rd, excessive polymerization inhibitor can cause the change of the color and performance of silica gel.4th, the one-component add-on type liquid of polymerization inhibitor is used merely
Body silica gel, its storage stability are also influenceed by polymerization inhibitor stability, and reliability is bad.
For another example, Chinese patent application CN201310398140.4, a kind of one-component heat conductive flame-retarding type RTV silicon rubber and its system
Preparation Method, give the technical scheme using moisture-curable.The shortcomings that such a scheme is：First, there is small molecule thing during moisture-curable
Matter discharges, and the small-molecule substance discharged has large effect to the performance of device and silica gel, and some materials can also cause device
Metal portion is corroded in part.2nd, silica gel needs that preservation is fully sealed before solidifying, and if contacted with moisture, also can at normal temperatures
Solidify and rotten.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of crosslinkable one pack system heat conduction can dispensing, solve it is existing can point
The problem of creep be present in the Heat Conduction Material of glue form.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions：A kind of crosslinkable single group
Point heat conduction can dispensing, include the component composition of following mass percent:Liquid silica gel 5~15%, the vinyl of epoxy-functional
The liquid silica gel 0.5~2% of functionalization, containing hydrogen silicone oil 0.5~2%, catalyst 0.05~0.5%, remaining be heat filling；Ring
The viscosity of the liquid silica gel of oxygen functionalization is 50~5000mPas, the viscosity of the liquid silica gel of vinyl-functional for 200~
5000mPa·s。
Preferably, the mass percent of the liquid silica gel of epoxy-functional is 8~12%.
Preferably, the particle diameter of heat filling has at least two particle diameters.
Preferably, the particle diameter of heat filling is 0.1~300 μm.
Preferably, heat filling is through coupling agent treatment mistake.
Preferably, heat filling is at least one of aluminum oxide, zinc oxide, aluminium nitride and boron nitride.
Preferably, catalyst is platinum catalyst.
In summary, advantages of the present invention：A kind of crosslinkable one pack system heat conduction provided by the invention can dispensing, including ring
The components such as the liquid silica gel of oxygen functionalization, the liquid silica gel of vinyl-functional, containing hydrogen silicone oil and heat filling, vinyl functional
Addition reaction can occur for the liquid silica gel and containing hydrogen silicone oil of change, by adjusting its viscosity and component ratio, can obtain with suitable
The product of suitable turnover rate, and can for a long time keep turnover rate constant at normal temperatures, it is ensured that product remains able to after long-term storage
Normal extrusion dispensing, after tested, with made from technical solution of the present invention can dispensing sample, be made after being stored 1 day under rear normal temperature
Turnover rate is 29g/min, and still has 26.7g/min turnover rate after being stored 30 days under normal temperature；And when temperature is more than 85
DEG C when, the liquid silica gel of epoxy-functional is because its thermosetting solidifies, and matrix can be cured as no stream after certain time
The heat-conducting pad of dynamic property.After tested, with made from technical solution of the present invention can dispensing, solidify 2 hours its turnover rates at 100 DEG C
4.9g/min can be dropped to, solidification solidifies completely after 2 days, after 1000-40~85 DEG C of temperature cycling tests, still may be used
State is fully cured in holding, and position is unchanged in vertical frock.
Embodiment
A kind of crosslinkable one pack system heat conduction can dispensing, include following mass percent component composition:Epoxy-functional
Liquid silica gel 5~15%, liquid silica gel 0.5~2%, containing hydrogen silicone oil 0.5~2%, the platinum catalyst of vinyl-functional
0.05~0.5%, remaining is heat filling；The viscosity of the liquid silica gel of epoxy-functional is 50~5000mPas, vinyl
The viscosity of the liquid silica gel of functionalization is 200~5000mPas.
In the present invention, the liquid silica gel of epoxy-functional has thermosetting.The viscosity that whole component includes 5~15% is 50
The liquid silica gel of~5000mPas epoxy-functional so that the product as made from the present invention program can under normal temperature state
Original viscosity is kept, so as to ensure with mobility and the property put, and after being extruded and being applied on working face, heat
Solidification, so as to prevent creep, the best in quality percentage of the liquid silica gel of epoxy-functional is 8~12%, in this scope
Interior, product has more preferable thermosetting, it is only necessary to which 2 hours its turnover rates are heated at 100 DEG C can be down to 5g/min or so, separately
Outside, the liquid silica gel viscosity of epoxy-functional is 50~5000mPas, can make to be mixed into enough heat fillings in raw material, side
Just it is well mixed.
In the present invention, the liquid silica gel and containing hydrogen silicone oil of vinyl-functional can adjust the product as made from the present invention program
Finished product viscosity.Addition reaction can occur for the liquid silica gel and containing hydrogen silicone oil of vinyl-functional, occur between its product component
A certain degree of crosslinking, the degree of cross linking is higher, and its viscosity is bigger, by adjusting its viscosity and component ratio, can obtain with suitable
The product of turnover rate.Scheme provided by the present invention, comprising 0.5~2% viscosity it is 200m~5000mPas's in component
The liquid silica gel of vinyl-functional, 0.5~2% containing hydrogen silicone oil and 0.05~0.5% platinum catalyst, in this condition
Under, by each component can be obtained after well mixed turnover rate be 10~40g/min can dispensing product.
In the present invention, heat filling is mixed with matrix material, to transmit heat, the form of heat filling has spherical
With aspherical two kinds of forms, the particle diameter of heat filling also has two kinds of different sizes, and aspherical heat filling specific surface area is big, and heat passes
It is higher to lead ability；The heat filling of small particle can be filled into the space between big particle diameter heat filling, can obtain higher
Filling rate, so as to improve thermal conductivity, in of the invention, preferably average grain diameter is 1~5 μm and 40~60 μm of heat filling；Heat conduction
One or more in the optional aluminum oxide of wire feeding, zinc oxide, aluminium nitride and boron nitride etc., preferably aluminum oxide.
Wherein, heat filling can be undressed or through coupling agent treatment mistake, preferably through coupling agent treatment
The heat filling crossed.The heat filling crossed through coupling agent treatment can be coated more fully, and heat conductivility is more preferable.By the present invention
Product made from the technical scheme of offer, thermal conductivity reach 2.5~4W/k.m.
Embodiment one：
A kind of crosslinkable one pack system heat conduction can dispensing, include following mass percent component composition:Epoxy-functional
Liquid silica gel 5%, the liquid silica gel 1% of vinyl-functional, containing hydrogen silicone oil 1%, platinum catalyst 0.5%, particle diameter be 1 μm
Zinc oxide 11.9%, the aluminum oxide 29.9% that particle diameter is 5 μm, the alumina particle 48.7% that particle diameter is 40 μm, particle diameter 60
μm boron nitride particle 2%.
The liquid silica gel of the liquid silica gel of vinyl-functional, containing hydrogen silicone oil, epoxy-functional is added to planet together
Stirred in mixer；Sequentially add the zinc oxide, the aluminum oxide that particle diameter is 5 μm, the oxygen that particle diameter is 40 μm that particle diameter is 1 μm
Change aluminium and particle diameter to mix for 60 μm of boron nitride, all should be first uniformly mixed after every kind of filler addition, then add lower one kind and fill out
Material；Platinum catalyst is added to be sufficiently mixed；Vacuumize process, sample is made.
Embodiment two：
A kind of crosslinkable one pack system heat conduction as described in embodiment one can dispensing, the present embodiment has following difference
Place：Component composition including following mass percent:Liquid silica gel 8.9%, the liquid of vinyl-functional of epoxy-functional
Silica gel 1%, containing hydrogen silicone oil 1%, platinum catalyst 0.5%, the zinc oxide 11.9% that particle diameter is 1 μm, the aluminum oxide that particle diameter is 5 μm
29.9%th, particle diameter is 40 μm alumina particle 44.8%, the boron nitride particle 2% that particle diameter is 60 μm.
The liquid silica gel of the liquid silica gel of vinyl-functional, containing hydrogen silicone oil, epoxy-functional is first added to row together
Stirred 10 minutes in star mixer；It is 40 μm to sequentially add zinc oxide, the aluminum oxide that particle diameter is 5 μm, particle diameter that particle diameter is 1 μm
Aluminum oxide and boron nitride that particle diameter is 60 μm mix, all should be first uniformly mixed after the addition of every kind of filler, then add next
Kind filler；Platinum catalyst is added to be sufficiently mixed；Vacuumize process, sample is made.
Embodiment three：
A kind of crosslinkable one pack system heat conduction as described in embodiment one, two can dispensing, the present embodiment has following difference
Part：Component composition including following mass percent:Liquid silica gel 15%, the liquid of vinyl-functional of epoxy-functional
Body silica gel 1%, containing hydrogen silicone oil 1%, platinum catalyst 0.5%, the zinc oxide 11.9% that particle diameter is 1 μm, the oxidation that particle diameter is 5 μm
Alumina particle 38.7% that aluminium 29.9%, particle diameter are 40 μm, the boron nitride particle 2% that particle diameter is 60 μm.
The liquid silica gel of the liquid silica gel of vinyl-functional, containing hydrogen silicone oil, epoxy-functional is first added to row together
Stirred 10 minutes in star mixer；Sequentially add zinc oxide, the aluminum oxide that average grain diameter is 5 μm that average grain diameter is 1 μm, flat
The boron nitride mixing that particle diameter is 40 μm of aluminum oxide and average grain diameter is 60 μm, all should first it be stirred after every kind of filler addition
Uniformly, then a kind of filler is added down；Platinum catalyst is added to be sufficiently mixed；Vacuumize process, sample is made.
Comparative example：
A kind of crosslinkable one pack system heat conduction can dispensing, include following mass percent component composition:Epoxy-functional
Liquid silica gel 2%, the liquid silica gel 10% of vinyl-functional, containing hydrogen silicone oil 1%, particle diameter is 1 μm of zinc oxide 11.9%,
Particle diameter is 5 μm of aluminum oxide 29.9%, and particle diameter is 40 μm of alumina particle 42.7%, and particle diameter is 60 μm of boron nitride particle
2%, platinum catalyst 0.5%.
The liquid silica gel of the liquid silica gel of vinyl-functional, containing hydrogen silicone oil, epoxy-functional is first added to row together
Stirred 10 minutes in star mixer；Sequentially add zinc oxide, the aluminum oxide that average grain diameter is 5 μm that average grain diameter is 1 μm, flat
The boron nitride mixing that particle diameter is 40 μm of aluminum oxide and average grain diameter is 60 μm, all should first it be stirred after every kind of filler addition
Uniformly, then a kind of filler is added down；Platinum catalyst is added to be sufficiently mixed；Vacuumize process, sample is made.
Thermal conductivity test is carried out to embodiment one, embodiment two, embodiment three, comparative example, places one at different temperatures
Turnover rate measurement is carried out after fixing time, measurement result data are as shown in Table 1：
Table one
Wherein：
In table one, thermal conductivity is according to standard ASTM D-5470, by LW-9389 boundary materials thermal resistance and the coefficient of heat conduction
Measuring equipment test gained；
Turnover rate is that the colloid extruded by promise letter Nordson EFD Relius1100 point gum machines under 90psi pressure is surveyed
Examination gained, length of testing speech 1min；
Temperature cycle range is -40 DEG C~85 DEG C.
In order to more intuitively show the advantage of technical solution of the present invention, inventor is to the sample as made from technical solution of the present invention
The creep resistant test in vertical gap has been carried out, and has been contrasted with the test result of other technologies scheme.Method of testing is specific
It is：Tested colloid is applied between the aluminum substrate surface and smooth glass surface that surface roughness is Ra3.2, put vertically
Put, after temperature cycles change 1000 times between -40 DEG C~60 DEG C, the position for recording colloid keeps situation.
Test result shows, with sample made from technical scheme provided by the present invention, can protect for a long time at normal temperatures
Deposit, and its turnover rate can decline to a great extent after short time high temperature solidifies, the basic energy after the hot setting of long period
Enough it is fully cured, and stable solid state can be still kept after temperature cycling test.
Therefore, technical scheme provided by the invention can solve the problem that it is existing it is curable can gluing process be complicated, solidification effect
The problem of difference and side effect are larger, has good normal temperature storage stability and solidification effect, industrial production is highly profitable.
In addition to above preferred embodiment, the present invention also has other embodiments, and those skilled in the art can be according to this
Invention is variously modified and deformed, and without departing from the spirit of the present invention, all should belong to appended claims of the present invention and determine
The scope of justice.
Claims (5)
1. a kind of crosslinkable one pack system heat conduction can dispensing, it is characterised in that：Component composition including following mass percent:Ring
The liquid silica gel 5~15% of oxygen functionalization, the liquid silica gel 0.5~2% of vinyl-functional, containing hydrogen silicone oil 0.5~2%, urge
Agent 0.05~0.5%, remaining be heat filling；
The viscosity of the liquid silica gel of epoxy-functional is 50~5000mPas, and the viscosity of the liquid silica gel of vinyl-functional is
200~5000mPas；
The mass percent of the liquid silica gel of epoxy-functional is 8~12%；
The particle diameter of heat filling has at least two particle diameters, and the form of heat filling has spherical and aspherical two kinds of forms.
2. a kind of crosslinkable one pack system heat conduction according to claim 1 can dispensing, it is characterised in that：The grain of heat filling
Footpath is 0.1~300 μm.
3. a kind of crosslinkable one pack system heat conduction according to claim 2 can dispensing, it is characterised in that：Heat filling is through idol
Connection agent treats.
4. a kind of crosslinkable one pack system heat conduction according to claim 3 can dispensing, it is characterised in that：Heat filling is oxygen
Change at least one of aluminium, zinc oxide, aluminium nitride and boron nitride.
5. a kind of crosslinkable one pack system heat conduction according to claim 1 can dispensing, it is characterised in that：Catalyst is platinum
Catalyst.
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| CN201510988369.2A CN105419723B (en) | 2015-12-24 | 2015-12-24 | A kind of crosslinkable one pack system heat conduction can dispensing |
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| CN201510988369.2A CN105419723B (en) | 2015-12-24 | 2015-12-24 | A kind of crosslinkable one pack system heat conduction can dispensing |
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| CN105419723B true CN105419723B (en) | 2018-04-10 |
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| CN106753205B (en) * | 2017-01-11 | 2020-05-22 | 湖南博翔新材料有限公司 | Epoxy modified organic silicon pouring sealant with low viscosity and high heat conductivity and application thereof |
| CN106633909B (en) * | 2017-01-13 | 2018-09-25 | 深圳市汉华热管理科技有限公司 | The method of insulation paste and insulation processing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962528A (en) * | 2010-09-30 | 2011-02-02 | 烟台德邦科技有限公司 | Two-component sealing silica gel with low viscosity and high thermal conductivity and preparation method theref |
| CN102002346A (en) * | 2010-10-15 | 2011-04-06 | 深圳市安品有机硅材料有限公司 | Organic silicon heat conduction composition and organic silicon heat conduction patch |
| CN102898999A (en) * | 2012-11-06 | 2013-01-30 | 江苏科技大学 | Sealant for electrical heating tubes |
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- 2015-12-24 CN CN201510988369.2A patent/CN105419723B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962528A (en) * | 2010-09-30 | 2011-02-02 | 烟台德邦科技有限公司 | Two-component sealing silica gel with low viscosity and high thermal conductivity and preparation method theref |
| CN102002346A (en) * | 2010-10-15 | 2011-04-06 | 深圳市安品有机硅材料有限公司 | Organic silicon heat conduction composition and organic silicon heat conduction patch |
| CN102898999A (en) * | 2012-11-06 | 2013-01-30 | 江苏科技大学 | Sealant for electrical heating tubes |
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