CN101407635B - Addition type heat conducting silicon rubber and manufacturing method thereof - Google Patents
Addition type heat conducting silicon rubber and manufacturing method thereof Download PDFInfo
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- CN101407635B CN101407635B CN200810046554XA CN200810046554A CN101407635B CN 101407635 B CN101407635 B CN 101407635B CN 200810046554X A CN200810046554X A CN 200810046554XA CN 200810046554 A CN200810046554 A CN 200810046554A CN 101407635 B CN101407635 B CN 101407635B
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Abstract
The invention relates to an addition type heat-conducting silicone rubber and a preparation method thereof. The addition type heat-conducting silicone rubber is characterized in that 100 weight portions of vinyl silicone oil and 200 weight portions to 500 weight portions of heat-conducting material are dewatered and mixed in a vacuum kneader for 30 to 200 minutes with the temperature of 100 to 150 DEG C and the vacuum degree of 0.06 to 0.099 MPa so as to obtain base material; under normal temperature, 0.5 weight portion to 1.5 weight portions of hydrogeneous silicone oil, 0.01 weight portion to 0.06 weight portion of inhibitor and 3 weight portions to 10 weight portions of diluent are added and stirred in a stirrer for 15 to 40 minutes so as to obtain A glue; 100 weight portions of base material are taken, 0.25 weight to 0.75 weight portion of platinum catalyst and 3 weight portions to 10 weight portions are added and stirred in the stirrer for 15 to 40 minutes so as to obtain B glue. The A glue and the B glue with the same weight portions are taken, mixed evenly and defoamed for 3 to 10 minutes at the vacuum degree of 0.06 to 0.09 MPa so as to obtain addition type heat-conducting silicone rubber. The heat-conducting silicone rubber is cured at normal temperature or low temperature, has good flow property and convenient use, has higher heat conductivity after fluidization and can be used for the components with the need of heat dissipation and heat transmission in the electronic appliance field.
Description
Technical field
The present invention relates to a kind of addition type heat conducting silicon rubber and manufacture method thereof, belong to polymeric material field.
Background technology
Along with science and technology development, electronic component, logical circuit are tending towards densification and miniaturization; Stability to electrical equipment is had higher requirement.In order to prevent the intrusion of moisture, dust and obnoxious flavour to electronic devices and components, slow down vibrations, prevent external force damage and stablize component parameter, the detrimentally affect in the external world is dropped to minimum, need electronic devices and components etc. are carried out embedding.The raising of appliance power requires potting compound to have good heat conduction and insulating property simultaneously.If heat can not in time conduct, easily form localized hyperthermia, damage electronic devices and components, assembly, influence the reliability and the works better cycle of system, therefore heat radiation is very important to electronic product.
At present using more Embedding Material is various synthetic polymers, wherein most widely used with Resins, epoxy, urethane and rubber.Heat conductive rubber is basic glue with silicon rubber or silicone resin usually.Typically very poor without the silicon rubber thermal conductivity of filling, thermal conductivity is generally 0.2W/mk, but after filling heat conductive filler, can obtain the good silicon rubber of heat conductivility.Chinese patent CN1205721A discloses a kind of high heat conduction, extension at break greater than 30% silicone elastomer, and CN101168620A discloses a kind of heat-conducting anti-flaming liquid silicon rubber, but all not mentioned flowing property of these two patents; 200610093711.3 a kind of thermally-conductive silicone composition is disclosed, at room temperature can not solidify or curing speed very slow, set time is very long, can not satisfy the requirement that electron trade develops rapidly.Therefore, develop a kind of high heat conduction, flowing property excellence, can be extremely urgent at the addition type heat conducting silicon rubber of room temperature or low-temperature curing.
Summary of the invention
The objective of the invention is provides a kind of addition type heat conducting silicon rubber and manufacture method thereof at the deficiencies in the prior art, be characterized in that this addition type heat conducting silicon rubber has excellent cold-resistant, heat-resisting, anti-ozone, good flowability and heat conductivility are arranged, be used for the embedding of electronic apparatus.
Purpose of the present invention is realized that by following technical measures wherein said starting material umber is mass fraction except that specified otherwise.
The feed composition of addition type heat conducting silicon rubber is
1, base-material
100 parts of vinyl silicone oils
200～500 parts of fillers
2, A component
100 parts of base-materials
0.5～1.5 part of containing hydrogen silicone oil
0.01～0.06 part in inhibitor
3～10 parts of thinners
3, B component
100 parts of base-materials
0.25～0.75 part of platinum catalyst
3～10 parts of thinners
Wherein, heat conductive filler is at least a in aluminium sesquioxide, silicon carbide and the silicon nitride.
Inhibitor is 2-methyl-3-butynyl-2 alcohol, 3-methyl isophthalic acid-hexin base-3-alcohol, 3, and is at least a in 5-dimethyl-1-hexin base-3-alcohol, 1-ethynyl-1-hexalin, methyl three (methyl fourth alkynyloxy group) silane, phenyl three (methyl fourth alkynyloxy group) silane, vinyl three (methyl fourth alkynyloxy group) silane and the many vinyl polysiloxane.
Platinum catalyst be Platinic chloride alcoholic solution, Platinic chloride the vinylsiloxane inner complex or make in the platinum catalyst of carrier any with carbon or aluminium sesquioxide.
The containing hydrogen silicone oil hydrogen content is 0.3～1.5%.
Viscosity when vinyl silicone oil is 25 ℃ of temperature is 250mpas～3000mpas.
Thinner is at least a in octamethylcyclotetrasiloxane, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane and the hexamethyldisiloxane.
The manufacture method of addition type heat conducting silicon rubber:
1, the preparation of base-material:
With 100 parts of vinyl silicone oils, 200～500 parts of heat conductive fillers add in the vacuum kneader, in 100～150 ℃ of temperature, and vacuum tightness 0.06～0.099MPa, 30～200 minutes acquisition base-materials of dehydration blend;
2, the preparation of A, B component:
(1) preparation of A component:
With 100 parts of base-materials, 0.5～1.5 part of containing hydrogen silicone oil, 0.01～0.06 part in inhibitor, 3～10 parts of thinners add in the stirrer and stirred 15～40 minutes under the room temperature, obtain the A component;
(2) preparation of B component:
With 100 parts of base-materials, 0.25～0.75 part of platinum catalyst, 3～10 parts of thinners add in the stirrer and stirred 15～40 minutes, obtain the B component;
3, the preparation of heat-conducting silicon rubber:
At room temperature, with etc. A, the B component of quality mix, vacuum tightness 0.06～0.09MPa deaeration 3～10 minutes, obtain addition type heat conducting silicon rubber.
With the addition type heat conducting silicon rubber that aforesaid method makes, press GB/T531-1999 test shore hardness; Press GB/T528-1998 test elongation at break and breaking tenacity; Press the GB10247-1988 tested viscosity; Press GB11205-89 test thermal conductivity.Test result is detailed to be shown in Table 1, the result shows: by not addition type heat conducting silicon rubber and addition type heat conducting silicon rubber comparison made in accordance with the present invention made in accordance with the present invention, the thermal conductivity height of addition type heat conducting silicon rubber of the present invention, good fluidity is suitable as the embedding of electronic devices and components.
The present invention has the following advantages:
1. added an amount of heat conductive filler in the base-material, after being solidified, addition type heat conducting silicon rubber has higher heat-conductivity, add a certain amount of volatile thinner that has, make addition type heat conducting silicon rubber before curing, have than low viscosity, has outstanding flowing property, help embedding, thinner solidifies slowly volatilization of back at silicon rubber, can not influence the performance of silicon rubber;
2. addition type heat conducting silicon rubber of the present invention use and manufacture method simple, will wait mass parts A component and the blend deaeration at room temperature of B component after, can use;
3. addition type heat conducting silicon rubber of the present invention can solidify at room temperature 24～72 hours, and smooth surface smooth, be not clamminess, avoid the damage of hot setting to electronic component, heating can be quickened its curing speed.
4. heat conductivility brilliance can be widely used in elastic adhesive, heat radiation, the sealing of electronics, electrical equipment, instrument industry.
Embodiment
Below by the embodiment description concrete to the present invention; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can content according to the present invention do some nonessential improvement and adjustment.
Embodiment 1: will be in 25 ℃ of viscosity of temperature vinyl silicone oil 100 mass parts that are 400mpas, and aluminium sesquioxide 450 mass parts, silicon nitride 50 mass parts add in the vacuum kneader, in 150 ℃ of temperature, vacuum tightness 0.06MPa, 200 minutes acquisition base-materials of dehydration blend.With hydrogen content is 0.5% containing hydrogen silicone oil 1 mass parts, pure 0.01 mass parts of 2-methyl-3-butynyl-2, and 3 mass parts octamethylcyclotetrasiloxanes add stirrer and 100 mass parts base-materials mixed 30 minutes, obtain the A component; With alcoholic solution 0.25 mass parts of Platinic chloride, octamethylcyclotetrasiloxane 3 mass parts add stirrer and 100 mass parts base-materials and mix 30 minutes acquisition B components; Get etc. after the A component of quality and B component mix, vacuum tightness 0.06MPa deaeration 3 minutes, obtain addition type heat conducting silicon rubber, the test result details of product performance are shown in Table 1.
Embodiment 2: will be in 25 ℃ of following viscosity of temperature vinyl silicone oil 100 mass parts that are 1000mpas, aluminium sesquioxide 350 mass parts, silicon carbide 50 mass parts add in the vacuum kneader, in 100 ℃ of temperature, vacuum tightness 0.099MPa, 120 minutes acquisition base-materials of dehydration blend.With hydrogen content is 1% containing hydrogen silicone oil 2 mass parts, methyl three (methyl fourth alkynyloxy group) silane 0.06 mass parts, and tetramethyl-tetrem thiazolinyl cyclotetrasiloxane 5 mass parts add in the stirrer and 100 mass parts base-materials mixed 30 minutes, obtain the A component; With vinylsiloxane inner complex 0.5 mass parts of Platinic chloride, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane 5 mass parts add stirrer and 100 mass parts base-materials mix 30 minutes acquisition B components; Get etc. after the A component of quality and B component mix, vacuum tightness 0.08MPa deaeration 5 minutes, obtain addition type heat conducting silicon rubber, the product performance test result is detailed to be shown in Table 1.
Embodiment 3: with vinyl silicone oil 100 mass parts of 25 ℃ of viscosity 3000mpas, aluminium sesquioxide 180 mass parts, silicon carbide 20 mass parts add in the vacuum kneader, in 150 ℃ of temperature, and vacuum tightness 0.06MPa, the dehydration blend obtained base-material in 30 minutes.With hydrogen content is 0.75% containing hydrogen silicone oil 2 mass parts, methyl three (methyl fourth alkynyloxy group) silane 0.03 mass parts, and hexamethyldisiloxane 10 mass parts add in the stirrer and 100 mass parts base-materials mixed 15 minutes, obtain the A component; With vinylsiloxane inner complex 0.75 mass parts of Platinic chloride, hexamethyldisiloxane 10 mass parts, add in the stirrer with 100 parts of base-materials mixed 40 minutes the B component; Get etc. after the A component of quality and B component mix, vacuum tightness 0.09MPa deaeration 10 minutes, obtain addition type heat conducting silicon rubber, the product performance test result is detailed to be shown in Table 1.
Comparative example 1: will be vinyl silicone oil 100 mass parts that 25 ℃ of following viscosity are 1000mpas in temperature, aluminium sesquioxide 350 mass parts, silicon nitride 50 mass parts add in the vacuum kneader, in 150 ℃ of temperature, vacuum tightness 0.099MPa, 60 minutes acquisition base-materials of dehydration blend.With hydrogen content is 0.5% containing hydrogen silicone oil 2 mass parts, and pure 0.06 mass parts of 2-methyl-3-butynyl-2 adds in the stirrer and 100 mass parts base-materials mixed 15 minutes, obtains the A component; The vinylsiloxane inner complex 0.75 mass parts adding stirrer and the 100 mass parts base-materials of Platinic chloride are mixed 40 minutes acquisition B components; Get etc. after the A component of quality and B component mix,, obtain addition type heat conducting silicon rubber vacuum tightness 0.08MPa deaeration 8 minutes.The test result details of product performance are shown in Table 1:
Table 1 addition type heat conducting silicon rubber The performance test results
Claims (3)
1. addition type heat conducting silicon rubber is characterized in that the feed composition of this heat-conducting silicon rubber is counted by following mass parts:
(1) A component
100 parts of base-materials
0.5～1.5 part of containing hydrogen silicone oil
0.01～0.06 part in inhibitor
3～10 parts of thinners
(2) B component
100 parts of base-materials
0.25～0.75 part of platinum catalyst
3～10 parts of thinners
Wherein said base-material consists of:
100 parts of vinyl silicone oils
200～500 parts of heat conductive fillers;
Described heat conductive filler is at least a in aluminium sesquioxide, silicon carbide and the silicon nitride;
Described inhibitor is 2-methyl-3-butynyl-2 alcohol, 3-methyl isophthalic acid-hexin base-3-alcohol, 3, and is at least a in 5-dimethyl-1-hexin base-3-alcohol, 1-ethynyl-1-hexalin, methyl three (methyl fourth alkynyloxy group) silane, phenyl three (methyl fourth alkynyloxy group) silane, vinyl three (methyl fourth alkynyloxy group) silane and the many vinyl polysiloxane;
Described containing hydrogen silicone oil is a hydrogen content at 0.3～1.5% containing hydrogen silicone oil;
The viscosity of described vinyl silicone oil when temperature is 25 ℃ is 250mpas～3000mpas;
Described thinner is at least a in octamethylcyclotetrasiloxane, tetramethyl-tetrem thiazolinyl cyclotetrasiloxane and the hexamethyldisiloxane.
2. according to the described addition type heat conducting silicon rubber of claim 1, it is characterized in that platinum catalyst be Platinic chloride alcoholic solution, Platinic chloride the vinylsiloxane inner complex or make in the platinum catalyst of carrier any with carbon or aluminium sesquioxide.
3. according to the manufacture method of claim 1 or 2 described addition type heat conducting silicon rubbers, it is characterized in that this method may further comprise the steps:
(1) preparation of base-material:
With vinyl silicone oil 100 mass parts, heat conductive filler 200～500 mass parts add in the vacuum kneader, in 100～150 ℃ of temperature, and vacuum tightness 0.06～0.099MPa, 30～200 minutes acquisition base-materials of dehydration blend;
(2) preparation of A, B component:
The preparation of A component:
With base-material 100 mass parts, containing hydrogen silicone oil 0.5～1.5 mass parts, inhibitor 0.01～0.06 mass parts, thinner 3～10 mass parts add in the stirrer and stirred under room temperature 15～40 minutes, obtain the A component;
The preparation of B component:
With base-material 100 mass parts, platinum catalyst 0.25～0.75 mass parts, thinner 3～10 mass parts add in the stirrer and stirred 15～40 minutes, obtain the B component;
(3) preparation of heat-conducting silicon rubber:
At room temperature will wait A, the B component of quality to mix,, obtain addition type heat conducting silicon rubber vacuum tightness 0.06～0.09MPa deaeration 3～10 minutes.
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