CN108441133A - A kind of preparation method of magnetism heat-conducting silica gel sheet - Google Patents

A kind of preparation method of magnetism heat-conducting silica gel sheet Download PDF

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CN108441133A
CN108441133A CN201810199283.5A CN201810199283A CN108441133A CN 108441133 A CN108441133 A CN 108441133A CN 201810199283 A CN201810199283 A CN 201810199283A CN 108441133 A CN108441133 A CN 108441133A
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heat
silica gel
parts
gel sheet
conducting silica
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姬娟宁
何伟仁
陈可
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NOTTING CHANGZHOU PRECISION MACHINERY Co Ltd
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NOTTING CHANGZHOU PRECISION MACHINERY Co Ltd
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    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04Homopolymers or copolymers of ethene
    • C09J123/08Copolymers of ethene
    • C09J123/0846Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
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    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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Abstract

The invention discloses a kind of preparation methods of magnetic heat-conducting silica gel sheet, belong to silica gel piece preparing technical field.The present invention is using Mn-Zn soft magnetic ferrite powder as heat-conducting silica gel sheet conductive powder,The magnetic flux of Mn-Zn soft magnetic ferrite powder first is big,It is larger for the magnetic attracting force of certain metallic elements,So that heat-conducting silica gel sheet is not needed adhesive can be assembled,Interfacial bonding material of the acrylic latex in heat-conducting silica gel sheet as fiberglass resin and conductive powder in the present invention,With acrylate hydroxyl condensation dehydration occurs for epoxidized soybean oil to form network interpenetrating cross-linked structure in the preparation process of acrylic latex,Latex only can minor change because of high crosslink density viscosity,In addition vinyl ester resin can be improved the compatibility of Mn-Zn soft magnetic ferrite powder and glass fibre by coupled action,Expanded graphite powder can expand in heat-conducting silica gel sheet and connect to form heat conduction network with the Mn-Zn soft magnetic ferrite powder of heat conduction when high temperature,To improve the heat conductivility of heat-conducting silica gel sheet.

Description

A kind of preparation method of magnetism heat-conducting silica gel sheet
Technical field
The invention discloses a kind of preparation methods of magnetic heat-conducting silica gel sheet, belong to silica gel piece preparing technical field.
Background technology
Silica gel piece, transparent flexible but waterproof can allow scar to keep a degree of temperature wet skin toughness Degree, pressure, amount of oxygen etc. prevent scar hyperplasia, finally reach the effect for subtracting light scar to soften scar.Silica gel piece can press Conjunction, damping, heat-blocking action, long-time service are not likely to produce cracking, can also be die-cut to the sheet material of any shape, can gum, while silicon Film can soften scar, prevent scar hyperplasia, finally reach the effect for subtracting light scar.
Silica gel piece can be used as electric insulation:Silica gel piece has higher electrical isolation grade, can bear high-voltage loaded, can make At products such as empire cloth, casings.Silica gel piece can soften scar, prevent scar hyperplasia, finally reach the effect for subtracting light scar.It is anti- Rotten aspect:Silicone Rubber Coated glass fabric can be used as pipeline, and the inside and outside anticorrosive coating of savings, antiseptic property is excellent, and intensity is high, It is a kind of ideal anti-corrosion material.
In daily life, people can be widely applied to various electronic products, and all electronic products all relate to And heat dissipation problem because temperature can increase the electronic component in electronic product in use, especially transistor and some Semiconductor device is particularly easy to generate heat, and when the temperature in use of electronic component is very high, electronic component performance can be caused to decline, thus It needs to radiate to electronic component.When heat dissipation element is connect with heater element, it usually needs use packing material and heat conduction material Expect to fill the gap between heater element and heat dissipation element.Heat conductive silica gel sheet material is a kind of common heat-conducting interface material. In actual use, heat conductive silica gel sheet material is attached on heater element, is reassembled and is fixed on heat dissipation element.If heat conduction The both side surface of silica gel sheet material all has viscosity, then there are the following problems, first, making attachment position Ge be not easy to be aligned because of viscous hand;Mesh Preceding electronic product use scope is very wide, indivisible in people's lives.And generate heat that be that electronic product plays its good The barrier of good performance, thus high performance heat dissipation Heat Conduction Material come into being.High thermal coefficient will add very high number Conduction powder, thus can cause to expect that the mobility before vulcanization is very poor, it is difficult to glass is infiltrated, to realize high heat conduction system thus Several can not possibly.
Therefore, a kind of magnetic heat-conducting silica gel sheet of invention has positive effect to silica gel piece preparing technical field.
Invention content
Present invention mainly solves the technical issues of, for it is current make heat-conducting silica gel sheet when to add to improve thermal coefficient Add the conduction powder of very high number, thus mobility of the silica gel sheet material before vulcanization can be caused very poor, it is difficult to glass is infiltrated, The heat conductivility of heat-conducting silica gel sheet is set to be difficult to be promoted, in addition heat-conducting silica gel sheet is usually required through sheet material side coating binder, Convenient for being bonded electronic component, and adhesive can make the viscous hand of heat-conducting silica gel sheet that attachment Wei Ge be made to be not easy to be aligned, and common adhesives Adhesion strength can decline the defect for being unfavorable for persistently being bonded at high temperature, provide a kind of preparation method of magnetic heat-conducting silica gel sheet.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of magnetism heat-conducting silica gel sheet, it is characterised in that specifically preparation process is:
(1)Iron oxide, zinc oxide, mangano-manganic oxide are mixed, abrasive material is obtained, abrasive material is mixed to get with poly-vinyl alcohol solution outstanding Suspension is put into ball mill by supernatant liquid, ball milling, obtains MnZn soft magnet oxygen powdery pulp;
(2)MnZn soft magnet oxygen powdery pulp is poured into mold, mold is put into after being suppressed in forcing press, mold is put into electricity It hinders in stove, is demoulded after cooled to room temperature and obtain Mn-Zn soft magnetic ferrite powder;
(3)It counts in parts by weight, 50~60 parts is added into the four-hole boiling flask with blender, reflux condensing tube, dropping funel Distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates start blender stirring, warming-in-water, by 40~45 After four-hole boiling flasks are added in part acrylic acid, 20~30 parts of methacrylic acids, the reaction was continued, obtains seed emulsion;
(4)It counts in parts by weight, 20~30 parts of epoxidized soybean oils is added into above-mentioned four-hole boiling flask, then with dropping funel to four mouthfuls 1~3 part of potassium peroxydisulfate is added dropwise in flask, after being added dropwise, insulation reaction continues heat temperature raising, insulation reaction, and ammonia is used in cooling Water adjusts pH, and discharging obtains acrylate latex;
(5)It counts in parts by weight, weighs 20~30 parts of ethylene-vinyl acetate copolymers, 40~50 parts of glass fibres, 10~15 Part expanded graphite powder, 8~10 parts of vinyl ester resins are put into reaction kettle, and heat temperature raising is kneaded, glass is obtained after being cooled to room temperature Fiberized resin;
(6)Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin are mixed, are put into stainless steel mould, it will after preheating Stainless steel mould is placed on vulcanizing press, heat temperature raising, pressurization, heat-insulation pressure keeping, taking-up mold, die sinking postcooling to room temperature, Vulcanization silica gel piece is obtained, vulcanization silica gel piece is placed in capacitance magnet charger and is magnetized, magnetic heat-conducting silica gel sheet is obtained.
Step(1)The iron oxide, zinc oxide, mangano-manganic oxide mixing quality ratio are 7 ︰, 1 ︰ 3, abrasive material and polyvinyl alcohol Solution mixing quality ratio is 1 ︰ 1, and the mass fraction of poly-vinyl alcohol solution is 20%, and control ball abrasive grain diameter is 0.1~0.3mm, ball milling Time is 15~20h.
Step(2)The die size is 40mm × 40mm × 100mm, and press pressure is 10~12MPa, when compacting Between be 5~8min, mold is put into sintering process in resistance furnace and is:1050~1100 DEG C are warming up to the rate of 2~3 DEG C/min, 2~3h of heat preservation sintering is naturally cooling to 1050~1100 immediately after continuation rises to 1200~1250 DEG C with same heating rate DEG C, 1~2h of heat preservation sintering.
Step(3)The speed of agitator is 200~220r/min, and temperature is 70~80 DEG C after warming-in-water, is continued anti- It is 10~15min between seasonable.
Step(4)The dropping funel drop rate is 3~5mL/min, and the insulation reaction time is 30~40min, after Temperature is 90~100 DEG C after continuous heat temperature raising, and the insulation reaction time is 45~55min, and temperature is 55~60 DEG C after cooling, ammonium hydroxide Mass fraction is 20%, and it is 6.0~7.0 to adjust pH with ammonium hydroxide.
Step(5)Temperature is 230~250 DEG C after the heat temperature raising, and mixing time is 3~5h.
Step(6)The Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin mixing quality ratio are 2 ︰, 1 ︰ 5, Stainless steel mould temperature is 100~150 DEG C, and preheating time is 30~35min, and temperature is 200~220 DEG C after heat temperature raising, is added Pressure pressure is 15~20MPa, and the heat-insulation pressure keeping time is 4~5h, and vulcanization silica gel piece, which is placed in capacitance magnet charger the time of magnetizing, is 10~15min, control magnetize magnetic field intensity as 1.2~1.8Tesla.
The beneficial effects of the invention are as follows:
(1)Iron oxide, mangano-manganic oxide, zinc oxide and poly-vinyl alcohol solution are mixed to get suspension by the present invention, by ball milling MnZn soft magnet oxygen powdery pulp is obtained, heating sintering after the die-filling compacting of MnZn soft magnet oxygen powdery pulp is obtained into MnZn soft magnetism Ferrite powder, by dodecyl sodium sulfate, sodium bicarbonate, the raw materials such as acrylic acid, methacrylic acid are placed in heat temperature raising in water-bath Seed emulsion is obtained by the reaction, then epoxidized soybean oil, potassium peroxydisulfate are added into seed emulsion, heating initiation reaction obtains acrylic acid Ester gum breast, with ethylene-vinyl acetate copolymer, glass fibre, part expanded graphite powder, vinyl ester resin etc. is raw material, It heats and is kneaded in reaction kettle, obtain fiberglass resin, finally mix Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin Conjunction is put into mold and preheats, and places into vulcanizing press and vulcanizes, and pressure heat-preserving magnetizes to obtain magnetic heat-conducting silica gel sheet, the present invention Using Mn-Zn soft magnetic ferrite powder as heat-conducting silica gel sheet conductive powder, the magnetic flux of Mn-Zn soft magnetic ferrite powder first is big, to Mr. Yu The magnetic attracting force of a little metallic elements is larger, and so that heat-conducting silica gel sheet is not needed adhesive can be assembled, and will not glue hand, in addition Mn-Zn soft magnetic ferrite powder high temperature when electronic component is powered can be such that its magnetism weakens, and avoid heat-conducting silica gel sheet viscous with heat dissipation element It connects too closely, keeps assembly element, detachable maintaining more convenient;
(2)Interfacial bonding material of the acrylic latex in heat-conducting silica gel sheet as fiberglass resin and conductive powder in the present invention, third With acrylate hydroxyl condensation dehydration occurs for epoxidized soybean oil to form network interpenetrating in the preparation process of olefin(e) acid latex Cross-linked structure contains epoxy group, ehter bond, hydroxyl isopolarity group and activity group in epoxidized soybean oil, makes acrylate Latex shows excellent adhesive strength, electrical insulation capability and high temperature resistance, and phenyl ring assigns latex heat resistance and rigidity, epoxy Base and hydroxyl make material have reactivity adhesion strength, and the dehydrating condensation of multiple hydroxyls makes crosslink density rise, in circuit board work Under hot conditions when making, latex passes through to be coupled and make because of high crosslink density viscosity meeting minor change, in addition vinyl ester resin With can improve the compatibility of Mn-Zn soft magnetic ferrite powder and glass fibre, expanded graphite powder can be in heat-conducting silica gel sheet when high temperature Middle expansion connect to form heat conduction network with the Mn-Zn soft magnetic ferrite powder of heat conduction, to improve the heat conductivility of heat-conducting silica gel sheet.
Specific implementation mode
It is that 7 ︰, 1 ︰ 3 are mixed in mass ratio by iron oxide, zinc oxide, mangano-manganic oxide, abrasive material is obtained, by abrasive material and quality point Number is that 1 ︰ 1 is mixed to get suspension in mass ratio for 20% poly-vinyl alcohol solution, suspension is put into ball mill, control ball Abrasive grain diameter is 0.1~0.3mm, 15~20h of ball milling, obtains MnZn soft magnet oxygen powdery pulp;By MnZn soft magnet oxygen powder slurry It is that mold is put into forcing press the compacting of the pressure with 10~12MPa 5 in 40mm × 40mm × 100mm molds that material, which pours into size, After~8min, mold is put into resistance furnace, 1050~1100 DEG C are warming up to the rate of 2~3 DEG C/min, heat preservation sintering 2~ 3h is naturally cooling to 1050~1100 DEG C, heat preservation sintering immediately after continuation rises to 1200~1250 DEG C with same heating rate 1~2h, after cooled to room temperature demoulding obtain Mn-Zn soft magnetic ferrite powder;It counts in parts by weight, to blender, reflux Condenser pipe, dropping funel four-hole boiling flask in be added 50~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of carbon Sour hydrogen sodium is started blender and is stirred with the rotating speed of 200~220r/min, and warming-in-water is to 70~80 DEG C, by 40~45 parts of propylene After four-hole boiling flasks are added in acid, 20~30 parts of methacrylic acids, the reaction was continued 10~15min obtains seed emulsion;In parts by weight Meter, into above-mentioned four-hole boiling flask be added 20~30 parts of epoxidized soybean oils, then with dropping funel into four-hole boiling flask with 3~5mL/ 1~3 part of potassium peroxydisulfate is added dropwise in min drop rates, after being added dropwise, 30~40min of insulation reaction, and continue to be heated to 90~ 100 DEG C, 45~55min of insulation reaction is cooled to 55~60 DEG C, and it is 6.0~7.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, is gone out Material, obtains acrylate latex;It counts in parts by weight, weighs 20~30 parts of ethylene-vinyl acetate copolymers, 40~50 parts of glass Glass fiber, 10~15 parts of expanded graphite powder, 8~10 parts of vinyl ester resins are put into reaction kettle, are heated to 230~250 DEG C, it is kneaded 3~5h, fiberglass resin is obtained after being cooled to room temperature;It is in mass ratio 2 ︰, 1 ︰ 5, by Mn-Zn soft magnetic ferrite powder, propylene Acid esters latex, fiberglass resin mixing, are put into and are preheated in 100~150 DEG C of stainless steel mould, will not after 30~35min of preheating Rust steel mold is placed on vulcanizing press, is heated to 200~220 DEG C, is forced into 15~20MPa, 4~5h of heat-insulation pressure keeping, Mold is taken out, die sinking postcooling obtains vulcanization silica gel piece to room temperature, vulcanization silica gel piece is placed in capacitance magnet charger and magnetizes 10~ 15min, control magnetize magnetic field intensity as 1.2~1.8Tesla, obtain magnetic heat-conducting silica gel sheet.
Example 1
It is that 7 ︰, 1 ︰ 3 are mixed in mass ratio by iron oxide, zinc oxide, mangano-manganic oxide, obtains abrasive material, be by abrasive material and mass fraction 20% poly-vinyl alcohol solution is that 1 ︰ 1 is mixed to get suspension in mass ratio, suspension is put into ball mill, control ball abrasive grain Diameter is 0.1mm, ball milling 15h, obtains MnZn soft magnet oxygen powdery pulp;MnZn soft magnet oxygen powdery pulp, which is poured into size, is In 40mm × 40mm × 100mm molds, after mold is put into forcing press the compacting of the pressure with 10MPa 5min, mold is put into In resistance furnace, 1050 DEG C, heat preservation sintering 2h are warming up to the rate of 2 DEG C/min, continues to rise to 1200 with same heating rate After DEG C, it is naturally cooling to 1050 DEG C, heat preservation sintering 1h immediately, is demoulded after cooled to room temperature and obtains Mn-Zn soft magnetic ferrite Powder;It counts in parts by weight, 50 parts of distilled water, 10 is added into the four-hole boiling flask with blender, reflux condensing tube, dropping funel Part dodecyl sodium sulfate, 4 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 200r/min, and warming-in-water, will to 70 DEG C After four-hole boiling flasks are added in 40 parts of acrylic acid, 20 parts of methacrylic acids, the reaction was continued 10min obtains seed emulsion;In parts by weight 20 parts of epoxidized soybean oils are added into above-mentioned four-hole boiling flask, then speed is added dropwise with 3mL/min into four-hole boiling flask with dropping funel for meter 1 part of potassium peroxydisulfate is added dropwise in rate, and after being added dropwise, insulation reaction 30min continues to be heated to 90 DEG C, insulation reaction 45min, 55 DEG C are cooled to, it is 6.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylate latex;It counts in parts by weight, 20 parts of ethylene-vinyl acetate copolymers, 40 parts of glass fibres, 10 parts of expanded graphite powder are weighed, 8 parts of vinyl ester resins are put into In reaction kettle, 230 DEG C are heated to, 3h is kneaded, fiberglass resin is obtained after being cooled to room temperature;It is in mass ratio 2 ︰, 1 ︰ 5, by manganese Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin mixing, are put into and are preheated in 100 DEG C of stainless steel mould, preheat Stainless steel mould is placed on vulcanizing press after 30min, is heated to 200 DEG C, is forced into 15MPa, heat-insulation pressure keeping 4h takes Going out mold, die sinking postcooling to room temperature obtains vulcanization silica gel piece, and vulcanization silica gel piece is placed in capacitance magnet charger the 10min that magnetizes, Control magnetizes magnetic field intensity as 1.2Tesla, obtains magnetic heat-conducting silica gel sheet.
Example 2
It is that 7 ︰, 1 ︰ 3 are mixed in mass ratio by iron oxide, zinc oxide, mangano-manganic oxide, obtains abrasive material, be by abrasive material and mass fraction 20% poly-vinyl alcohol solution is that 1 ︰ 1 is mixed to get suspension in mass ratio, suspension is put into ball mill, control ball abrasive grain Diameter is 0.2mm, ball milling 17h, obtains MnZn soft magnet oxygen powdery pulp;MnZn soft magnet oxygen powdery pulp, which is poured into size, is In 40mm × 40mm × 100mm molds, after mold is put into forcing press the compacting of the pressure with 11MPa 7min, mold is put into In resistance furnace, 1070 DEG C, heat preservation sintering 2.5h are warming up to the rate of 2 DEG C/min, continuation is risen to same heating rate After 1220 DEG C, it is naturally cooling to 1070 DEG C, heat preservation sintering 1.5h immediately, is demoulded after cooled to room temperature and obtains MnZn soft magnet Oxysome powder;It counts in parts by weight, 55 parts of distillations is added into the four-hole boiling flask with blender, reflux condensing tube, dropping funel Water, 12 parts of dodecyl sodium sulfates, 4 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 210r/min, warming-in-water to 75 DEG C, after four-hole boiling flasks are added in 42 parts of acrylic acid, 25 parts of methacrylic acids, the reaction was continued 12min obtains seed emulsion;By weight Measure number meter, into above-mentioned four-hole boiling flask be added 25 parts of epoxidized soybean oils, then with dropping funel into four-hole boiling flask with 4mL/min 2 parts of potassium peroxydisulfates are added dropwise in drop rate, and after being added dropwise, insulation reaction 35min continues to be heated to 95 DEG C, insulation reaction 50min is cooled to 57 DEG C, and it is 6.5 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylate latex;By weight Number meter weighs 25 parts of ethylene-vinyl acetate copolymers, 45 parts of glass fibres, 12 parts of expanded graphite powder, 9 parts of vinyl esters Resin is put into reaction kettle, is heated to 240 DEG C, is kneaded 4h, fiberglass resin is obtained after being cooled to room temperature;It is 2 ︰ in mass ratio Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin are mixed, are put into and are preheated to 120 DEG C of stainless steel mould by 1 ︰ 5 In, stainless steel mould is placed on vulcanizing press after preheating 32min, is heated to 210 DEG C, is forced into 17MPa, heat preservation is protected 4.5h is pressed, mold is taken out, die sinking postcooling to room temperature obtains vulcanization silica gel piece, and vulcanization silica gel piece is placed in capacitance magnet charger Magnetize 12min, and control magnetizes magnetic field intensity as 1.5Tesla, obtains magnetic heat-conducting silica gel sheet.
Example 3
It is that 7 ︰, 1 ︰ 3 are mixed in mass ratio by iron oxide, zinc oxide, mangano-manganic oxide, obtains abrasive material, be by abrasive material and mass fraction 20% poly-vinyl alcohol solution is that 1 ︰ 1 is mixed to get suspension in mass ratio, suspension is put into ball mill, control ball abrasive grain Diameter is 0.3mm, ball milling 20h, obtains MnZn soft magnet oxygen powdery pulp;MnZn soft magnet oxygen powdery pulp, which is poured into size, is In 40mm × 40mm × 100mm molds, after mold is put into forcing press the compacting of the pressure with 12MPa 8min, mold is put into In resistance furnace, 1100 DEG C, heat preservation sintering 3h are warming up to the rate of 3 DEG C/min, continues to rise to 1250 with same heating rate After DEG C, it is naturally cooling to 1100 DEG C, heat preservation sintering 2h immediately, is demoulded after cooled to room temperature and obtains Mn-Zn soft magnetic ferrite Powder;It counts in parts by weight, 60 parts of distilled water, 15 is added into the four-hole boiling flask with blender, reflux condensing tube, dropping funel Part dodecyl sodium sulfate, 5 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 220r/min, and warming-in-water, will to 80 DEG C After four-hole boiling flasks are added in 45 parts of acrylic acid, 30 parts of methacrylic acids, the reaction was continued 15min obtains seed emulsion;In parts by weight 30 parts of epoxidized soybean oils are added into above-mentioned four-hole boiling flask, then speed is added dropwise with 5mL/min into four-hole boiling flask with dropping funel for meter 3 parts of potassium peroxydisulfates are added dropwise in rate, and after being added dropwise, insulation reaction 40min continues to be heated to 100 DEG C, insulation reaction 55min, 60 DEG C are cooled to, it is 7.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylate latex;It counts in parts by weight, 30 parts of ethylene-vinyl acetate copolymers, 50 parts of glass fibres, 15 parts of expanded graphite powder are weighed, 10 parts of vinyl ester resins are put Enter in reaction kettle, be heated to 250 DEG C, is kneaded 5h, fiberglass resin is obtained after being cooled to room temperature;It is 2 ︰, 1 ︰ 5 in mass ratio, it will Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin mixing, are put into and are preheated in 150 DEG C of stainless steel mould, preheat Stainless steel mould is placed on vulcanizing press after 35min, is heated to 220 DEG C, is forced into 20MPa, heat-insulation pressure keeping 5h takes Going out mold, die sinking postcooling to room temperature obtains vulcanization silica gel piece, and vulcanization silica gel piece is placed in capacitance magnet charger the 15min that magnetizes, Control magnetizes magnetic field intensity as 1.8Tesla, obtains magnetic heat-conducting silica gel sheet.
Comparative example
With the magnetic heat-conducting silica gel sheet of Henan company production as a comparison case to magnetic heat-conducting silica gel sheet produced by the present invention and Magnetic heat-conducting silica gel sheet in comparative example carries out performance detection, and testing result is as shown in table 1:
1, test method:
Determination of conductive coefficients is detected by GBT 5990-2006 standards;
Gluing strength test is stretched to be detected by JC/T547-2005 standards;
High temperature resistant type is tested:By thermally conductive sheet after molding, thermally conductive sheet is the aluminium sheet of surfacing up and down, is put into thermostatic drying chamber In, its hardness of partial test and thermal resistance variation are taken out in 250 DEG C of agings in 200h respectively.
The test method reference of hardness《ASTM D2240-2005 rubber hardness testing standards》
The test method reference of thermal resistance《ASTM D5470-2006 heat transfer solid electrical insulation thin material heat-conductive characteristics test side Method (10.02)》
1 silica gel piece performance measurement result of table
Test event Example 1 Example 2 Example 3 Comparative example
Thermal coefficient(W/mK) 3.0 3.1 3.2 1.5
Stretch gluing intensity(MPa) 5.3 5.4 5.5 3.5
Thermal resistance before aging(m2k/W) 2.015 2.022 2.024 1.056
Hardness before aging(HR) 32 30 25 45
Thermal resistance after 200h agings(m2k/W) 1.985 1.995 1.997 0.985
Hardness after 200h agings(HR) 42 40 35 55
High according to the magnetic heat-conducting silica gel sheet thermal coefficient produced by the present invention of data among the above, good heat conductivity bonds strong Degree is high, and high temperature resistance is good, has broad application prospects.

Claims (7)

1. a kind of preparation method of magnetism heat-conducting silica gel sheet, it is characterised in that specifically preparation process is:
(1)Iron oxide, zinc oxide, mangano-manganic oxide are mixed, abrasive material is obtained, abrasive material is mixed to get with poly-vinyl alcohol solution outstanding Suspension is put into ball mill by supernatant liquid, ball milling, obtains MnZn soft magnet oxygen powdery pulp;
(2)MnZn soft magnet oxygen powdery pulp is poured into mold, mold is put into after being suppressed in forcing press, mold is put into electricity It hinders in stove, is demoulded after cooled to room temperature and obtain Mn-Zn soft magnetic ferrite powder;
(3)It counts in parts by weight, 50~60 parts is added into the four-hole boiling flask with blender, reflux condensing tube, dropping funel Distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates start blender stirring, warming-in-water, by 40~45 After four-hole boiling flasks are added in part acrylic acid, 20~30 parts of methacrylic acids, the reaction was continued, obtains seed emulsion;
(4)It counts in parts by weight, 20~30 parts of epoxidized soybean oils is added into above-mentioned four-hole boiling flask, then with dropping funel to four mouthfuls 1~3 part of potassium peroxydisulfate is added dropwise in flask, after being added dropwise, insulation reaction continues heat temperature raising, insulation reaction, and ammonia is used in cooling Water adjusts pH, and discharging obtains acrylate latex;
(5)It counts in parts by weight, weighs 20~30 parts of ethylene-vinyl acetate copolymers, 40~50 parts of glass fibres, 10~15 Part expanded graphite powder, 8~10 parts of vinyl ester resins are put into reaction kettle, and heat temperature raising is kneaded, glass is obtained after being cooled to room temperature Fiberized resin;
(6)Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin are mixed, are put into stainless steel mould, it will after preheating Stainless steel mould is placed on vulcanizing press, heat temperature raising, pressurization, heat-insulation pressure keeping, taking-up mold, die sinking postcooling to room temperature, Vulcanization silica gel piece is obtained, vulcanization silica gel piece is placed in capacitance magnet charger and is magnetized, magnetic heat-conducting silica gel sheet is obtained.
2. a kind of preparation method of magnetic heat-conducting silica gel sheet according to claim 1, it is characterised in that:Step(1)It is described Iron oxide, zinc oxide, mangano-manganic oxide mixing quality ratio be 7 ︰, 1 ︰ 3, abrasive material and poly-vinyl alcohol solution mixing quality ratio are 1 ︰ 1, the mass fraction of poly-vinyl alcohol solution is 20%, and control ball abrasive grain diameter is 0.1~0.3mm, and Ball-milling Time is 15~20h.
3. a kind of preparation method of magnetic heat-conducting silica gel sheet according to claim 1, it is characterised in that:Step(2)It is described Die size be 40mm × 40mm × 100mm, press pressure is 10~12MPa, and the pressing time is 5~8min, and mold puts Entering sintering process in resistance furnace is:1050~1100 DEG C, 2~3h of heat preservation sintering are warming up to the rate of 2~3 DEG C/min, is continued After rising to 1200~1250 DEG C with same heating rate, it is naturally cooling to 1050~1100 DEG C immediately, 1~2h of heat preservation sintering.
4. a kind of preparation method of magnetic heat-conducting silica gel sheet according to claim 1, it is characterised in that:Step(3)It is described Speed of agitator be 200~220r/min, temperature is 70~80 DEG C after warming-in-water, and the reaction was continued, and the time is 10~15min.
5. a kind of preparation method of magnetic heat-conducting silica gel sheet according to claim 1, it is characterised in that:Step(4)It is described Dropping funel drop rate be 3~5mL/min, the insulation reaction time be 30~40min, continue heat temperature raising after temperature be 90 ~100 DEG C, the insulation reaction time is 45~55min, and temperature is 55~60 DEG C after cooling, and ammonium hydroxide mass fraction is 20%, uses ammonium hydroxide It is 6.0~7.0 to adjust pH.
6. a kind of preparation method of magnetic heat-conducting silica gel sheet according to claim 1, it is characterised in that:Step(5)It is described Heat temperature raising after temperature be 230~250 DEG C, mixing time be 3~5h.
7. a kind of preparation method of magnetic heat-conducting silica gel sheet according to claim 1, it is characterised in that:Step(6)It is described Mn-Zn soft magnetic ferrite powder, acrylate latex, fiberglass resin mixing quality ratio be 2 ︰, 1 ︰ 5, stainless steel mould temperature be 100 ~150 DEG C, preheating time is 30~35min, and temperature is 200~220 DEG C after heat temperature raising, and moulding pressure is 15~20MPa, is protected The warm dwell time is 4~5h, and vulcanization silica gel piece is placed in capacitance magnet charger the time of magnetizing as 10~15min, controls the magnetic that magnetizes Field intensity is 1.2~1.8Tesla.
CN201810199283.5A 2018-03-12 2018-03-12 A kind of preparation method of magnetism heat-conducting silica gel sheet Pending CN108441133A (en)

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