CN105273680A - Double-component heat conduction silica gel sheet and preparation method and device thereof - Google Patents
Double-component heat conduction silica gel sheet and preparation method and device thereof Download PDFInfo
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- CN105273680A CN105273680A CN201510799056.2A CN201510799056A CN105273680A CN 105273680 A CN105273680 A CN 105273680A CN 201510799056 A CN201510799056 A CN 201510799056A CN 105273680 A CN105273680 A CN 105273680A
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Abstract
The invention provides a double-component heat conduction silica gel sheet which comprises two components. The component A comprises two-alkenyl end-capped dimethyl polysiloxane, double-hydroxyalkyl end-capped polysiloxane, double-hydroxy end-capped dimethyl siloxane, methyl vinyl siloxane copolymers, methyl vinyl cyclosiloxane, heat conduction fillers and epoxy modified silane coupling agents. The component B comprises phenyl hydrogen-contained silicone oil or a mixture of phenyl hydrogen-contained silicone oil and hydrogen-contained silicone oil, methyl vinyl cyclosiloxane and platinum catalysts. The component A and the component B are mixed according to the weight ratio of 1 to (0.7-1). The double-component heat conduction silica gel sheet can meet the demand for heat conduction of small and integrated equipment and has a higher heat conductivity coefficient on the premise of maintaining good comprehensive performance.
Description
Technical field
The invention relates to heat-conducting interface material synthesis preparing technical field, and particularly a kind of have silicone based heat conduction film of two component composition and preparation method thereof and equipment, is applicable to transmission and the heat dissipation of heat between Heating element, heat dissipation element.
Background technology
Along with the development of electronic equipment small and functional diversities, by integrated increasing element and function in small component, in use procedure, temperature will raise fast, easily causes the degradation of electronic component, equipment travelling speed slows down, the many-sided problem of lamp is broken down in equipment operation.Therefore, how fast and effeciently the more heats produced in miniaturization, integrated equipment to be taken away one of discharge important content becoming Design of Temperature Control.
Heat-conducting organic silica gel sheet material is the mainstay material for transferring heat between heating position and heat radiation position in prior art, there is good snappiness, electrical insulating property, compressibility, ductility, fully can fill the surface of irregular components and parts, eliminate air, enlarge active surface, the effect of spacing insulation, antidetonation, sealing is the ideal chose of heat transfer material in electronics.
In prior art, organosilicon thermally conductive material is base material mainly with organic silica gel, adds heat conductive filler and be aided with the one-component mixture material that various auxiliary agent obtains greatly, obtains after repressed shaping, cross cutting, infrared or vulcanizable cures.But organosilicon thermally conductive material of the prior art has following defect: (1) due to mixture material be one-component material, the addition of heat conductive filler is restricted, in unit volume, heat conductive filler makes the heat conductivility of heat conductive silica gel sheet material be restricted containing quantitative limitation, be difficult to the discharge requirement adapting to more heats, existing heat conductive silica gel sheet material thickness limit value is at 0.3mm, and under this thickness, the thermal conductivity of heat conductive silica gel sheet material is general the highest only can reach 1.5W/mK; (2) because mixture material is one-component material, in heat conductive silica gel sheet material preparation process, raw-material stability in storage also has certain restriction, easily cause solidifying uneven phenomenon simultaneously, usually need in compositing formula, to add inhibitor to extend the stability in storage of compositing formula and to avoid solidification uneven, and the addition of inhibitor needs strictly to control, avoid having an impact to performance; (3) because increasing heat conducting element adopts special-shaped shape and structure (as " convex " font), the heat conductive silica gel sheet material obtained of the prior art often needs the shape and structure cutting to adapt to heat conducting element, cut and will cause a large amount of spillages of material and waste, for the heating element of special-shaped shape and structure, only to cut and the loss caused can up to more than 30%; (4) heat conductive silica gel sheet material solidification process often needs carry out sulfuration and add vulcanizing agent; cause serious environmental pollution; be unfavorable for environment protection and HUMAN HEALTH; though infrared curing does not have too many environmental problem; but still there is solidification process and time uncontrollable problem, be unfavorable for the adjustment of producing.
Summary of the invention
The invention, for solving the problems of the prior art, first provides a kind of two component heat conductive silica gel sheet material, can be applicable to the heat conduction demand of miniaturization, integrated equipment especially, under the prerequisite keeping good over-all properties, have higher thermal conductivity.
Two component heat conductive silica gel sheet materials that the invention provides have two kinds of components:
Component A comprises:
The dimethyl polysiloxane of the two rare base end-blocking of a1:90-100 weight part;
The polysiloxane of the two hydroxyalkyl end-blocking of a2:20-40 weight part;
The two hydroxy-end capped dimethyl siloxane of a3:20-40 weight part and the multipolymer of methyl vinyl silicone;
A4:0.5-5 weight part methyl ethylene annular siloxane;
A5:150-180 weight part heat conductive filler;
A6:2-5 parts by weight epoxy modified silane coupler;
B component comprises:
The mixture of b1:40-80 weight part phenyl hydrogen-containing silicon oil or itself and containing hydrogen silicone oil;
B2:0.5-5 weight part methyl ethylene annular siloxane;
B3:2-10 weight part platinum group catalyst;
Wherein, described component A and B component are with weight ratio 1:(0.7-1) ratio mixing.
Further, described B component can also comprise:
B4:5-30 weight part heat-resisting additive;
And/or
B5:5-30 weight part tackifier;
And/or
B6:1-30 weight part toughener.
Wherein, described a1 is one of basal component in constituent of the present invention, and its viscosity is preferably between 100-10000cps, is preferably between 100-5000cps, is more preferably between 100-2000cps.In described a1, rare base is exemplary comprises vinyl, allyl group, the rare base of fourth, penta rare base etc., is preferably vinyl.Further, the molecular-weight average of the dimethyl polysiloxane of the two rare base end-blocking of described a1-is preferably 30-100 ten thousand, and the average quality percentage composition of vinyl is preferably 0.1-0.5%.
Wherein, described a2 is the basal component two in constituent of the present invention, and its viscosity is preferably between 100-10000cps, is preferably between 100-5000cps, is more preferably between 100-2000cps.Described a2 provides lasting moisture curing cross-linking process while addition reaction of silicon with hydrogen under different humidity temperature condition, makes shaping rear sheet material still can continue solidification, avoids the phenomenon of local solidification inequality.Further, the molecular-weight average of the polysiloxane of the two hydroxyalkyl end-blocking of described a2-is preferably 0.2-10 ten thousand.
Wherein, containing hydroxyl in described a3, auxiliary moisture curing process can be provided while addition reaction of silicon with hydrogen, be conducive to regulating set time, realize the controllability of solidification process; Meanwhile, a3 as the linking agent between a1 and a2, can also play crosslinked and bridging action, is beneficial to the curing molding of network polymer, and realizes in-situ solidifying effect, greatly reduce cure shrinkage.Described a3 viscosity is preferably below 2000cps.Preferred further, in described a3, hydroxyl mass content is between 1-10%; The mass content of methyl vinyl silicone is between 10-40%.
Wherein, the methyl ethylene annular siloxane of described a4 and b2 can be identical or different, preferably identical, containing the ring texture that silica replaces in its structure, add in component A and B component the effect simultaneously playing crosslinked, softening and dispersion respectively, be conducive to effective mixing of component A and B component mixing process simultaneously.The example of described a4 and/or b2 indefiniteness comprises t etram-ethyltetravinylcyclotetrasiloxane, 2,4-divinyl-2,4,6,6,8,8-hexamethyl cyclotetrasiloxane, hexamethyl six ethene basic ring six siloxanes, 2,4,6-trivinyl-2,4,6-trimethylammonium cyclotrisiloxane etc.It should be noted that described methyl ethylene annular siloxane is owing to being low molecular weight substance, and easily open loop, addition needs strict control.
Wherein, the example of described a5 indefiniteness can be one or more in silicon-dioxide, aluminum oxide, zinc oxide, magnesium oxide, aluminium nitride, silicon nitride, boron nitride, aluminium powder, silver powder, copper powder, graphite, carbon nanotube etc.The particle diameter of described a5 heat conductive filler can be preferably 0.1-50 μm.
Wherein, described a6 is used for carrying out surface modification to described a5, improves addition and the dispersion effect of heat conductive filler.In silane coupling agent, introduce epoxide group, be namely more conducive to the crosslinking reaction of itself and other moiety, improve the consistency of heat conductive filler in system.The example of described a6 indefiniteness can be γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane etc.
Wherein, in described b1, per molecule has at least two and is good for the hydrogen atom of conjunction with silicon, is the basal component three in constituent of the present invention.The introducing of phenyl improves reactive behavior and the thermotolerance of product, but in order to promote crosslinking curing consistency, needs the strict content controlling phenyl.Preferably, in described b1, the average quality percentage composition of phenyl is 5-20%.
Wherein, described b3 can be the complex compound of the polysiloxane of Platinic chloride or Platinic chloride and ethenyl blocking, as the complex compound of the polydimethylsiloxane of Platinic chloride and ethenyl blocking.
Wherein, the example of described b4 indefiniteness can be one or more in ferric oxide, carbon black, gas-phase silica; Preferably, the heat-resisting additive of described b4 also carries out modification through epoxy silane coupling agent, for, the consumption of the epoxy silane coupling agent of described b4 modification is preferably the 0.1-3% of b4 quality consumption.
Wherein, the example of described b5 indefiniteness can be the organoalkoxysilane containing amido, isocyanate group, as γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane etc.
Wherein, the example of described b6 indefiniteness can be one or more in glass fibre, carbon fiber, ceramic fiber; Preferably, the toughener of described b6 also carries out modification through epoxy silane coupling agent, for, the consumption of the epoxy silane coupling agent of described b6 modification is preferably the 0.1-3% of b4 quality consumption.
The invention additionally provides the preparation method of a kind of pair of component heat conductive silica gel sheet material, comprises the steps:
S1: use the epoxide modified silane coupling agent of a6 to carry out surface modification to a5 heat conductive filler by metering ratio;
S2: after the multipolymer of the polysiloxane of the dimethyl polysiloxane of two for a1 rare base end-blocking, the two hydroxyalkyl end-blocking of a2, the two hydroxy-end capped dimethyl siloxane of a3 and methyl vinyl silicone, a4 methyl ethylene annular siloxane fully being mixed by metering ratio, add through the modified heat conductive filler of step S1 several times wherein, and fully mix, obtain the mixture of component A;
S3: fully mix than the b4 heat-resisting additive that b1 phenyl hydrogen-containing silicon oil or its mixture with containing hydrogen silicone oil, b2 methyl ethylene annular siloxane, b3 platinum group catalyst and may needing is added and/or b5 tackifier and/or b6 toughener by metering, the mixture of acquisition B component;
S4: by metering than after the mixture of component A and the mixture of B component are fully mixed, by shaping in forming mould, then through room temperature spontaneous curing or be heating and curing, acquisition heat conductive silica gel sheet material finished product.
Wherein, above-mentioned steps S3 and S1 and S2 is without the restriction of sequencing.
Wherein, in described step S4, moulding process can adopt the forming mould of common heat conductive silica gel sheet material and method to carry out shaping, also two component extrusion forming devices with adjustable extruding outlet preferably can be adopted to carry out the shaping of special-shaped shape, or can preferably adopt the pouring device with special-shaped shape pouring gate to carry out shaping.The heat conductive silica gel sheet material that the invention provides directly can carry out the shaping of special-shaped shape, avoids the loss of post-production, and shaped device can be purchased or make by oneself.
The invention additionally provides two component extrusion forming devices of a kind of adjustable extruding outlet, be specially adapted to the shaping of the special-shaped shape of two component heat conductive silica gel sheet materials of the invention, comprise respectively with two storage tanks of pressing mechanism, described two storage tanks are connected to tapping channel, it is a hybrid channel that described tapping channel converges after a segment distance, and described hybrid channel end connects discharge port.
Further, described discharge port is the bar shaped outlet with controllable width.
Further, described hybrid channel is also provided with mixing tank, in described mixing tank, also can be provided with stirring or kneading mechanism further.
The invention has following advantage:
(1) mixture material is bicomponent material, can improve the addition of heat conductive filler, and when heat conductive silica gel sheet material thickness is 0.3mm, thermal conductivity can reach more than 3.0W/mK;
(2) without the need to adding inhibitor, stability in storage is good, and two components can distinguish long-time storage, carry out mixing moulding again during use;
(3) can carry out thermofixation and be aided with moisture curing, solidification process be controlled; Under can reaching room temperature, 1-2h solidifies, 0.5-1h solidification under 50-80 DEG C of condition of heating; And solidification is evenly complete;
(4) over-all properties is good, meets even higher than other performances of general heat conductive silica gel sheet material, as hardness, temperature tolerance, intensity, toughness etc. under the condition keeping high thermal conductivity coefficient;
(5) cure shrinkage is little, is applicable to the straight forming of easy shape and structure, avoids loss to waste, cost-saving;
(6) without the need to sulfuration and high temperature, environmental friendliness, energy consumption is little.
Accompanying drawing explanation
Fig. 1 is the structural representation of two component extrusion forming devices of a kind of adjustable of the invention extruding outlet;
Fig. 2 is the partial enlarged drawing of discharge port part in Fig. 1.
Wherein, 1-storage tank A; 2-storage tank B; 3-pressing mechanism; 4-tapping channel A; 5-tapping channel B; 6-hybrid channel C; 7-discharge port; 8-bar shaped exports; 9-mixing tank; 10-stirs or kneading mechanism.
Embodiment
Below the invention is further described.Convenient in order to describe, the equipment in the invention omits operation steps or the condition of necessity or routine, and as weighing, temperature control, control stir speed (S.S.) etc., those skilled in the art can adjust arbitrarily according to the needs of reaction.Under the condition of not conflicting, the feature in the present invention program in each embodiment can combine mutually.Following embodiment is only and object of the present invention is described, is not limited to the present invention.
Performance evaluation testing method of the present invention is as follows:
Shao 00 hardness: carry out with reference to GB/T531.1-2008 standard.
Tensile strength: carry out with reference to GB/T529-2008 standard.
Elongation at break: carry out with reference to GB/T528-2009 standard.
Voltage breakdown: carry out with reference to GB/T1695-2009 standard.
Thermal conductivity: carry out with reference to ASTM-D5470 standard.
Temperature tolerance: film is placed in 150 DEG C of environment 1000h, observes variable color, heat conduction and insulation stability.
Cold-hot impact: 100 circulations film being carried out-40-105 DEG C, observes variable color, heat conduction and insulation stability.
Viscosity described in the invention is the viscosity at 25 DEG C.
The preparation of following each embodiment can adopt equipment as illustrated in fig. 1 and 2, comprise respectively with storage tank A1 and the storage tank B2 of pressing mechanism 3, described storage tank A1 and storage tank B2 is connected to tapping channel A4 and tapping channel B5, described tapping channel A4 and tapping channel B5 converges for hybrid channel C6 after a segment distance, and described hybrid channel C6 end connects discharge port 7.Wherein, described discharge port 7 is for having the bar shaped outlet 8 of controllable width.Described hybrid channel C6 is also provided with mixing tank 9, also can be provided with stirring or kneading mechanism 10 in described mixing tank 9 further, as stirring rake.Pressing mechanism 3 on described batch can A1 and storage tank B2 can be cylinder.Described bar shaped outlet 8 can be set to required thickness width, as 0.3mm etc.
The process that employing aforesaid device prepares the invention heat conductive silica gel sheet material is as follows:
First, the epoxide modified silane coupling agent of a6 is used to carry out surface modification to a5 heat conductive filler by metering ratio;
Second, after the multipolymer of the polysiloxane of the dimethyl polysiloxane of two for a1 rare base end-blocking, the two hydroxyalkyl end-blocking of a2, the two hydroxy-end capped dimethyl siloxane of a3 and methyl vinyl silicone, a4 methyl ethylene annular siloxane fully being mixed by metering ratio, add through the modified heat conductive filler of step S1 several times wherein, and fully mix, obtain the mixture of component A, be placed on storage tank A1;
3rd, fully mix than the b4 heat-resisting additive that b1 phenyl hydrogen-containing silicon oil or its mixture with containing hydrogen silicone oil, b2 methyl ethylene annular siloxane, b3 platinum group catalyst and may needing is added and/or b5 tackifier and/or b6 toughener by metering, obtain the mixture of B component, be placed on storage tank B2;
4th, by pressing mechanism 3 respectively to storage tank A1 and storage tank B2, the mixture of the mixture of component A and B component is extruded from tapping channel A4 and tapping channel B5 in proportion respectively, and fully mixing in hybrid channel C6 and mixing tank 9, the bar shaped outlet 8 finally by discharge port 7 is extruded and shaping.
5th, by shaping sheet material through room temperature spontaneous curing or be heating and curing, obtain heat conductive silica gel sheet material finished product.
Embodiment 1
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:90 weight part bi-vinyl end-blocking, its viscosity 2000cps, molecular-weight average is 600,000, and the average quality percentage composition of vinyl is 0.2%;
The polysiloxane that a2:40 weight part is bis-hydroxypropyl terminated, its viscosity 5000cps, molecular-weight average is 1.0 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:3 weight part hexamethyl six ethene basic ring six siloxanes;
A5:150 weight part silicon nitride, particle diameter 20 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
The mixture of b1:40 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 10%;
B2:2 weight part hexamethyl six ethene basic ring six siloxanes;
B3:5 parts by weight chloroplatinic acid;
Wherein, described component A and B component mix with the ratio of weight ratio 1:1.
Embodiment 2
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:95 weight part diallyl end-blocking, its viscosity 1500cps, molecular-weight average is 800,000, and the average quality percentage composition of vinyl is 0.5%;
The polysiloxane that a2:20 weight part is bis-hydroxypropyl terminated, its viscosity 3000cps, molecular-weight average is 0.6 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:2 weight part hexamethyl six ethene basic ring six siloxanes;
A5:160 part by weight of zinc oxide and magnesian mixture, particle diameter 50 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
The mixture of b1:60 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 15%;
B2:2 weight part t etram-ethyltetravinylcyclotetrasiloxane;
The complex compound of the polydimethylsiloxane of b3:5 parts by weight chloroplatinic acid and ethenyl blocking;
The gas-phase silica of b4:5 weight part surface gamma-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent modified (coupling agent consumption is 0.5% of gas-phase silica quality);
B5:5 weight part γ-aminopropyl triethoxysilane.
Wherein, described component A and B component mix with the ratio of weight ratio 1:0.8.
Embodiment 3
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:90 weight part bi-vinyl end-blocking, its viscosity 2000cps, molecular-weight average is 600,000, and the average quality percentage composition of vinyl is 0.2%;
The polysiloxane that a2:40 weight part is bis-hydroxypropyl terminated, its viscosity 5000cps, molecular-weight average is 1.0 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:3 weight part hexamethyl six ethene basic ring six siloxanes;
A5:150 weight part silicon nitride, particle diameter 20 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
The mixture of b1:60 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 15%;
B2:2 weight part t etram-ethyltetravinylcyclotetrasiloxane;
The complex compound of the polydimethylsiloxane of b3:5 parts by weight chloroplatinic acid and ethenyl blocking;
The gas-phase silica of b4:5 weight part surface gamma-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent modified (coupling agent consumption is 0.5% of gas-phase silica quality);
B6:2 weight part surface gamma-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent modified (coupling agent consumption is 1% of carbon fiber quality) carbon fiber.
Wherein, described component A and B component mix with the ratio of weight ratio 1:1.
Comparative example 1
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:90 weight part bi-vinyl end-blocking, its viscosity 2000cps, molecular-weight average is 600,000, and the average quality percentage composition of vinyl is 0.2%;
The polysiloxane that a2:40 weight part is bis-hydroxypropyl terminated, its viscosity 5000cps, molecular-weight average is 1.0 ten thousand;
A4:3 weight part hexamethyl six ethene basic ring six siloxanes;
A5:150 weight part silicon nitride, particle diameter 20 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
The mixture of b1:40 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 10%;
B2:2 weight part hexamethyl six ethene basic ring six siloxanes;
B3:5 parts by weight chloroplatinic acid;
Wherein, described component A and B component mix with the ratio of weight ratio 1:1.
Comparative example 2
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:90 weight part bi-vinyl end-blocking, its viscosity 2000cps, molecular-weight average is 600,000, and the average quality percentage composition of vinyl is 0.2%;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:3 weight part hexamethyl six ethene basic ring six siloxanes;
A5:80 weight part silicon nitride, particle diameter 20 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
The mixture of b1:40 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 10%;
B2:2 weight part hexamethyl six ethene basic ring six siloxanes;
B3:5 parts by weight chloroplatinic acid;
Wherein, described component A and B component mix with the ratio of weight ratio 1:1.
Comparative example 3
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:90 weight part bi-vinyl end-blocking, its viscosity 2000cps, molecular-weight average is 600,000, and the average quality percentage composition of vinyl is 0.2%;
The polysiloxane that a2:40 weight part is bis-hydroxypropyl terminated, its viscosity 5000cps, molecular-weight average is 1.0 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:3 weight part viscosity is at the dimethyl silicone oil of about 500cps;
A5:100 weight part silicon nitride, particle diameter 20 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
The mixture of b1:40 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 10%;
B2:2 weight part viscosity is at the dimethyl silicone oil of about 500cps;
B3:5 parts by weight chloroplatinic acid;
Wherein, described component A and B component mix with the ratio of weight ratio 1:1.
Comparative example 4
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:95 weight part diallyl end-blocking, its viscosity 1500cps, molecular-weight average is 800,000, and the average quality percentage composition of vinyl is 0.5%;
The polysiloxane that a2:20 weight part is bis-hydroxypropyl terminated, its viscosity 3000cps, molecular-weight average is 0.6 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:2 weight part hexamethyl six ethene basic ring six siloxanes;
A5:90 part by weight of zinc oxide and magnesian mixture, particle diameter 50 μm;
A6:5 parts by weight of ethylene base Trimethoxy silane;
B component comprises:
The mixture of b1:60 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 15%;
B2:2 weight part t etram-ethyltetravinylcyclotetrasiloxane;
The complex compound of the polydimethylsiloxane of b3:5 parts by weight chloroplatinic acid and ethenyl blocking;
The gas-phase silica of b4:5 weight part surface vinyl trimethoxy silane coupler modified (coupling agent consumption is 0.5% of gas-phase silica quality);
B5:5 weight part γ-aminopropyl triethoxysilane.
Wherein, described component A and B component mix with the ratio of weight ratio 1:0.8.
Comparative example 5
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:95 weight part diallyl end-blocking, its viscosity 1500cps, molecular-weight average is 800,000, and the average quality percentage composition of vinyl is 0.5%;
The polysiloxane that a2:20 weight part is bis-hydroxypropyl terminated, its viscosity 3000cps, molecular-weight average is 0.6 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:2 weight part hexamethyl six ethene basic ring six siloxanes;
A5:160 part by weight of zinc oxide and magnesian mixture, particle diameter 50 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
B1:60 weight part is not containing the containing hydrogen silicone oil of phenyl;
B2:2 weight part t etram-ethyltetravinylcyclotetrasiloxane;
The complex compound of the polydimethylsiloxane of b3:5 parts by weight chloroplatinic acid and ethenyl blocking;
The gas-phase silica of b4:5 weight part surface gamma-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent modified (coupling agent consumption is 0.5% of gas-phase silica quality);
B5:5 weight part γ-aminopropyl triethoxysilane.
Wherein, described component A and B component mix with the ratio of weight ratio 1:0.8.
Comparative example 6
Adopt aforesaid device and method to prepare heat conductive silica gel sheet material, the service condition of raw material is as follows:
Component A comprises:
The dimethyl polysiloxane of a1:95 weight part diallyl end-blocking, its viscosity 1500cps, molecular-weight average is 800,000, and the average quality percentage composition of vinyl is 0.5%;
The polysiloxane that a2:20 weight part is bis-hydroxypropyl terminated, its viscosity 3000cps, molecular-weight average is 0.6 ten thousand;
The two hydroxy-end capped dimethyl siloxane of a3:30 weight part and the multipolymer of methyl vinyl silicone, hydroxyl mass content is 4%; The mass content of methyl vinyl silicone is 30%;
A4:4 weight part hexamethyl six ethene basic ring six siloxanes;
A5:160 part by weight of zinc oxide and magnesian mixture, particle diameter 50 μm;
A6:5 weight part γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane;
B component comprises:
The mixture of b1:60 weight part phenyl hydrogen-containing silicon oil and containing hydrogen silicone oil, the average quality percentage composition of phenyl is 15%;
The complex compound of the polydimethylsiloxane of b3:5 parts by weight chloroplatinic acid and ethenyl blocking;
The gas-phase silica of b4:5 weight part surface gamma-(2,3-epoxy third oxygen) propyl trimethoxy silicane coupling agent modified (coupling agent consumption is 0.5% of gas-phase silica quality);
B5:5 weight part γ-aminopropyl triethoxysilane.
Wherein, described component A and B component mix with the ratio of weight ratio 1:0.8.
Detected by the heat conductive silica gel sheet material that above-described embodiment and comparative example obtain, result is as shown in table 1.Wherein, because addO-on therapy changes in part comparative example, and have impact on the added total amount of heat conductive filler, end reaction is difficult to reach higher heat-conducting effect in thermal conductivity.
Table 1
Claims (10)
1. a two component heat conductive silica gel sheet material, comprises two kinds of components:
Component A comprises:
The dimethyl polysiloxane of the two rare base end-blocking of a1:90-100 weight part;
The polysiloxane of the two hydroxyalkyl end-blocking of a2:20-40 weight part;
The two hydroxy-end capped dimethyl siloxane of a3:20-40 weight part and the multipolymer of methyl vinyl silicone;
A4:0.5-5 weight part methyl ethylene annular siloxane;
A5:150-180 weight part heat conductive filler;
A6:2-5 parts by weight epoxy modified silane coupler;
B component comprises:
The mixture of b1:40-80 weight part phenyl hydrogen-containing silicon oil or itself and containing hydrogen silicone oil;
B2:0.5-5 weight part methyl ethylene annular siloxane;
B3:2-10 weight part platinum group catalyst;
Wherein, described component A and B component are with weight ratio 1:(0.7-1) ratio mixing.
2. the two component heat conductive silica gel sheet material of one according to claim 1, it is characterized in that, described B component can also comprise:
B4:5-30 weight part heat-resisting additive;
And/or
B5:5-30 weight part tackifier;
And/or
B6:1-30 weight part toughener.
3. the two component heat conductive silica gel sheet material of one according to claim 1, it is characterized in that, described a1 viscosity is preferably between 100-10000cps, is preferably between 100-5000cps, is more preferably between 100-2000cps; The molecular-weight average of described a1 is preferably 30-100 ten thousand, and the average quality percentage composition of vinyl is preferably 0.1-0.5%.
4. the two component heat conductive silica gel sheet material of one according to claim 1, it is characterized in that, described a2 viscosity is preferably between 100-10000cps, is preferably between 100-5000cps, is more preferably between 100-2000cps; The molecular-weight average of described a2 is preferably 0.2-10 ten thousand.
5. the two component heat conductive silica gel sheet material of one according to claim 1, it is characterized in that, in described a3, hydroxyl mass content is between 1-10%; The mass content of methyl vinyl silicone is between 10-40%.
6. the two component heat conductive silica gel sheet material of one according to claim 1, it is characterized in that, in described b1, the average quality percentage composition of phenyl is 5-20%.
7. the two component heat conductive silica gel sheet material of one according to claim 2, it is characterized in that, the heat-resisting additive of described b4 and/or the toughener of b6 also carry out modification through epoxy silane coupling agent.
8. the preparation method of a kind of pair of component heat conductive silica gel sheet material according to claim 1, comprises the steps:
S1: use the epoxide modified silane coupling agent of a6 to carry out surface modification to a5 heat conductive filler by metering ratio;
S2: after the multipolymer of the polysiloxane of the dimethyl polysiloxane of two for a1 rare base end-blocking, the two hydroxyalkyl end-blocking of a2, the two hydroxy-end capped dimethyl siloxane of a3 and methyl vinyl silicone, a4 methyl ethylene annular siloxane fully being mixed by metering ratio, add through the modified heat conductive filler of step S1 several times wherein, and fully mix, obtain the mixture of component A;
S3: fully mix than the b4 heat-resisting additive that b1 phenyl hydrogen-containing silicon oil or its mixture with containing hydrogen silicone oil, b2 methyl ethylene annular siloxane, b3 platinum group catalyst and may needing is added and/or b5 tackifier and/or b6 toughener by metering, the mixture of acquisition B component;
S4: by metering than after the mixture of component A and the mixture of B component are fully mixed, by shaping in forming mould, then through room temperature spontaneous curing or be heating and curing, acquisition heat conductive silica gel sheet material finished product;
Wherein, above-mentioned steps S3 and S1 and S2 is without the restriction of sequencing.
9. the preparation method of a kind of pair of component heat conductive silica gel sheet material according to claim 8, it is characterized in that, in described step S4, moulding process can adopt the forming mould of common heat conductive silica gel sheet material and method to carry out shaping, also two component extrusion forming devices with adjustable extruding outlet preferably can be adopted to carry out the shaping of special-shaped shape, or can preferably adopt the pouring device with special-shaped shape pouring gate to carry out shaping.
10. for two component extrusion forming devices of a kind of pair of component heat conductive silica gel sheet material according to claim 1, comprise respectively with two storage tanks of pressing mechanism, described two storage tanks are connected to tapping channel, it is a hybrid channel that described tapping channel converges after a segment distance, and described hybrid channel end connects discharge port;
As the further improvement of such scheme, described discharge port is the bar shaped outlet with controllable width;
As the further improvement of such scheme, described hybrid channel is also provided with mixing tank, in described mixing tank, also can be provided with stirring or kneading mechanism further.
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| CN108559272A (en) * | 2018-04-02 | 2018-09-21 | 东莞太洋橡塑制品有限公司 | Low-temp low-pressure silica gel moulding process |
| CN109627776A (en) * | 2018-11-14 | 2019-04-16 | 深圳市飞荣达科技股份有限公司 | Solidfied material made of heat-conductive silicone composition and its solidification |
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