CN108731095A - A kind of preparation method of the porous copper radiating rib of high heat conduction - Google Patents
A kind of preparation method of the porous copper radiating rib of high heat conduction Download PDFInfo
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- CN108731095A CN108731095A CN201810593414.8A CN201810593414A CN108731095A CN 108731095 A CN108731095 A CN 108731095A CN 201810593414 A CN201810593414 A CN 201810593414A CN 108731095 A CN108731095 A CN 108731095A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24D—DOMESTIC- OR SPACE-HEATING SYSTEMS, e.g. CENTRAL HEATING SYSTEMS; DOMESTIC HOT-WATER SUPPLY SYSTEMS; ELEMENTS OR COMPONENTS THEREFOR
- F24D19/00—Details
- F24D19/008—Details related to central heating radiators
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/02—Constructions of heat-exchange apparatus characterised by the selection of particular materials of carbon, e.g. graphite
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/08—Constructions of heat-exchange apparatus characterised by the selection of particular materials of metal
- F28F21/081—Heat exchange elements made from metals or metal alloys
- F28F21/085—Heat exchange elements made from metals or metal alloys from copper or copper alloys
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- Polymers & Plastics (AREA)
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- Combustion & Propulsion (AREA)
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- Materials Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract
The invention discloses a kind of preparation methods of the porous copper radiating rib of high heat conduction, belong to metallurgical casting preparing technical field.The coarsening process of polyurethane is, as chemical plating carries out being grown into form continuous sheet metal copper in matrix surface, to improve the specific surface area of Porous Cu to increase the binding force of polyurethane surface and the coat of metal, while accelerating the flowing heat dissipation of flowing gas；Electronics in electroplating process of the present invention on metal ion and cathode is combined generation metallic atom, metallic atom constantly crystallization forms continuous metal deposition layer in matrix surface, the magnetic flux of manganese-zinc ferrite powder first is big, it is larger for the magnetic attracting force of conductive metal electronic component, the magnetic pull that porous copper radiating rib passes through heat-conducting resin is set to reinforce bonding assembling, the dehydrating condensation of multiple hydroxyls makes crosslink density rise, under hot conditions when circuit board works, latex is because of high crosslink density viscosity meeting minor change, to improve the heat conductivility of cooling fin, it has a extensive future.
Description
Technical field
The invention discloses a kind of preparation methods of the porous copper radiating rib of high heat conduction, belong to metallurgical casting technology of preparing neck
Domain.
Background technology
Cooling fin is a kind of device to the easy heat-generating electronic elements heat dissipation in electric appliance, mostly by aluminium alloy, brass or bronze
Make plate, sheet, splintery etc..Common cooling fin material is copper and aluminium alloy, and the two respectively has its advantage and disadvantage.The heat conduction of copper
Property it is good but expensive, difficulty of processing is higher, and weight is excessive, and thermal capacity is smaller, and be easy oxidation.And fine aluminium is too soft, it cannot
Directly use, the advantages of enough hardness could be provided by being all the aluminium alloy used, aluminium alloy be it is cheap, it is light-weight, but
Thermal conductivity will be far short of what is expected than copper.Some radiators just respectively take the chief, the embedded a piece of copper coin on aluminium alloy heat radiator pedestal.
The radiator of north of china in winter heating is also cooling fin.Cooling fin occupies important role in the composition of radiator,
In addition to the active heat removal of fan, the quality of a radiator is evaluated, the heat absorption energy of cooling fin itself is heavily dependent on
Power and capacity of heat transmission.It is well known that the operating temperature of electronic device directly determines its service life and stability, to allow PC each
The operating temperature of component is maintained in reasonable range, in addition to ensure PC working environments temperature in the reasonable scope other than, also
It has to carry out radiating treatment.And with the enhancing of PC computing capabilitys, power consumption has become with heat dissipation problem does not allow that avoids to ask
Topic.In general, the heat source rich and influential family in PC includes CPU, mainboard, video card and other component such as hard disk etc., they disappear when working
The electric energy of consumption has quite a few and converts non-heat.
The acceleration constantly to upgrade with electronic product and mini, highly integrated and high performance electronics days
Benefit increases, and work package volume size is smaller and smaller, and the speed and efficiency of work are higher and higher, and calorific value is increasing.At present
The heat that existing porous copper heat sink is conducted through heat dissipation base can not reach heat-delivery surface, the stomata be connected in cooling fin in time
It is larger to the flow resistance of flowing gas, it is difficult to the problems such as playing the high-specific surface area advantage of porous metals, in the prior art mostly
Using metal fin and graphite heat radiation fin, although metal fin thermal coefficient itself is high, interfacial property is very poor, with heat
There is prodigious thermal contact resistance in source when contacting, and cannot heat be transmitted to metal from heat source well, to influence to radiate, and graphite
Cooling fin is very low in longitudinal thermal coefficient, and its interfacial property is also poor, can not well pass heat from heat source
The defect for passing out.Therefore, invent a kind of porous copper radiating rib of high heat conduction has actively meaning to metallurgical casting preparing technical field
Justice.
Invention content
Present invention mainly solves the technical issues of, the heat conducted through heat dissipation base for current existing porous copper heat sink
Amount can not reach heat-delivery surface in time, and the stomata be connected in cooling fin is larger to the flow resistance of flowing gas, it is difficult to play porous
The problems such as high-specific surface area advantage of metal, mostly uses metal fin and graphite heat radiation fin, heat dissipation metal in the prior art
Although piece thermal coefficient itself is high, interfacial property is very poor, there is prodigious thermal contact resistance when being contacted with heat source, cannot be good
Heat is transmitted to metal from heat source, to influence to radiate, and graphite heat radiation fin is very low in longitudinal thermal coefficient, and its boundary
Surface properties are also poor, and the defect that can not well pass out heat from heat source provides a kind of high heat conduction Porous Cu
The preparation method of cooling fin.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of the porous copper radiating rib of high heat conduction, it is characterised in that specifically preparation process is：
（1）Liquor potassic permanganate is poured into beaker, warming-in-water, polyurethane foam is taken to be put into beaker and makes polyurethane foam
It is completely immersed in acid permanganate soln, impregnation obtains roughening polyurethane foam, and roughening polyurethane foam is put into quality
It is impregnated in the oxalic acid solution that score is 5%, roughening polyurethane foam is stirred and squeezed with glass bar, obtains polyurethane matrix；
（2）100~120mL tin chloride solutions are configured, add 5~7g glass puttys, 30~40mL hydrochloric acid to obtain into tin chloride solution quick
Change liquid, polyurethane matrix is put into sensitizing solution and is impregnated, sensitization polyurethane matrix is obtained, by palladium chloride solution and hydrochloric acid solution etc.
Volume mixture obtains solution glue, and above-mentioned sensitization polyurethane matrix is immersed in 120~150mL solution glues, after dispergation processing, is taken out
Polyurethane matrix is put into 200~220mL formalins, is impregnated, is obtained surface active polyurethane matrix；
（3）It counts in parts by weight, by 20~25 parts of copper sulphate, 30~40 parts of formaldehyde, 80~90 parts of sodium tartrates, 12~15 parts of hydrogen
Sodium oxide molybdena, which is put into 400~500 parts of distilled water, to be dissolved, and chemical-electrical plating solution is obtained, by 90~100 parts of surface active polyurethane matrixes
It is put into chemical-electrical plating solution, after heat temperature raising, 5~10 parts of di-mercaptobenzothiazolbies of addition into chemical-electrical plating solution, insulation reaction,
Obtain micro- copper facing polyurethane；
（4）The copper-bath that 400~500mL mass fractions are 40% is configured, the dense sulphur of 50~60mL is added to copper-bath
Acid, 8~10g polyethylene glycol, 12~15g1,4- butynediols, 20~30g nickel chlorides obtain electrolyte, electrolyte are put into electricity
Slot is solved, using copper rod as anode, micro- copper facing polyurethane as cathode, is electrolysed, taking-up cathode is washed with water 3~5 times and obtains copper facing
Polyurethane；
（5）Count in parts by weight, into four-hole boiling flask be added 50~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~
5 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 200~220r/min, and warming-in-water continuously adds 40~45 parts of propylene
After four-hole boiling flask is added in acid, 20~30 parts of methacrylic acids, the reaction was continued obtains seed emulsion；
（6）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 with the drop rate of 3~5mL/min in flask, after being added dropwise, insulation reaction continues heating and rises
Temperature, insulation reaction, then cool down, pH is adjusted with ammonium hydroxide, discharging obtains acrylate latex, takes 20~30 parts of ethene-vinyl acetates
Ester copolymer, 40~50 parts of manganese-zinc ferrite powder, 10~15 parts of expanded graphite powder, 8~10 parts of vinyl ester resins are put into reaction
In kettle, heat temperature raising is kneaded, heat-conducting resin is obtained after being cooled to room temperature；
（7）Copper facing polyurethane is put into resistance furnace, mixed gas is passed through into resistance furnace, temperature programming to 400~420 DEG C,
Heat preservation reduction, is continuously heating to 850~900 DEG C, heat preservation pyrolysis, obtains porous copper product, then by the heat-conducting resin of pre- heat fusing
Seepage flow enters in porous copper product, and the porous copper radiating rib of high heat conduction is obtained after cooled to room temperature.
Step（1）The pH of the liquor potassic permanganate is 2~3, and the mass fraction of liquor potassic permanganate is 20%, water-bath
Temperature is 45~50 DEG C after heating, and the impregnation time is 10~15min, and the mass fraction of oxalic acid solution is 5%, polyurethane foam
The foam time is 10~15min.
Step（2）The mass fraction of the tin chloride solution is 5%, and the mass fraction of hydrochloric acid is 10%, is soaked in sensitizing solution
The bubble time is 5~8min, is 8% by the mass fraction of palladium chloride solution, and the mass fraction of hydrochloric acid solution is 5%, when dispergation is handled
Between be 4~5min, the mass fraction of formalin is 75%.
Step（3）Temperature is 40~45 DEG C after the heat temperature raising, and the insulation reaction time is 3~4h.
Step（4）The mass fraction of the copper-bath is 40%, and the mass fraction of the concentrated sulfuric acid is 98%, is electrolysed time control
Current density processed is 2~3A/dm3, electrolysis time is 2~3h.
Step（5）The warming-in-water is 70~80 DEG C, and the reaction was continued, and the time is 10~15min.
Step（6）The insulation reaction time is 30~40min, and it is 90~100 DEG C to continue heat temperature raising, insulation reaction
Time is 45~55min, then it is 55~60 DEG C to cool down, the mass fraction 20% of ammonium hydroxide, and it is 6.0~7.0 to adjust pH, and reaction kettle adds
Heat heating is 230~250 DEG C, and mixing time is 4~5h.
Step（7）The mixed gas is that hydrogen, nitrogen are that 3 ︰ 1 are made by volume, and resistance furnace heating rate is 2
~3 DEG C/min, the heat preservation recovery time is 2~3h, and heat preservation pyrolysis time is 3~4h.
The beneficial effects of the invention are as follows：
（1）The present invention is roughened to obtain roughening polyurethane foam through acid permanganate soln using polyurethane foam as basis material,
Roughening polyurethane foam is immersed after oxalic acid solution again to wash to be put into sensitizing solution to impregnate and obtains sensitization polyurethane matrix, sensitization is poly-
Urethane matrix obtains copper facing polyurethane through surface active, electroless plating, electro-deposition, then through drying, surface reduction, thermal depolymerization ammonia
Ester, cooling annealing obtain porous copper product, and the coarsening process of polyurethane is to increase the knot of polyurethane surface and the coat of metal
With joint efforts, blind hole and the inner passage for opening simultaneously foam base plate, being generated on the surface of polyurethane foam has hydrophilic base
Group, and make surface roughening, chemically coating surface grows out the coat of metal, and coarsening process considerably increases polyurethane
The surface area of the surface area of matrix, matrix is bigger, matrix with and coating contact surface it is also bigger, it is activated after in polyurethane matrix
Surface forms many activated centres, in plating process, these crystalline substances of equally distributed activated centre as metallic crystal
Core, as chemical plating carries out being grown into form continuous sheet metal copper in matrix surface, the intensive hair in sheet metal copper surface
Pore structure, when being impacted by flowing gas of sheet metal copper, gas can branch to intensive pore from main aperture road, make gas
Flow resistance reduce, improve the specific surface area of Porous Cu, at the same accelerate flowing gas flowing heat dissipation；
（2）Electronics in electroplating process of the present invention on metal ion and cathode is combined generation metallic atom, and metallic atom is continuous
Crystallization forms continuous metal deposition layer in matrix surface, and formation of the metallic crystal on cathode can be roughly divided into metal crystal nuclei
Two processes of growth with metal grain are generated, polyethylene glycol, Isosorbide-5-Nitrae-butynediols is mixed in electroplate liquid, inhibits the life of nucleus
It is long, cause the speed of growth of nucleus to be less than it and form speed, tiny crystal grain can make the accumulation of Porous Cu more fine and close, Porous Cu
Surface is not likely to produce protrusion, more smooth, in addition, conductive powder of the present invention using manganese-zinc ferrite powder as heat-conducting resin, first
The magnetic flux of manganese-zinc ferrite powder is big, larger for the magnetic attracting force of conductive metal electronic component, makes porous copper radiating rib
Reinforce bonding assembling by the magnetic pull of heat-conducting resin, acrylic latex is in heat-conducting resin as resin and magnetic conductive powder
Interfacial bonding material, with acrylate hydroxyl condensation dehydration occurs for epoxidized soybean oil in the preparation process of acrylic latex
To form network interpenetrating cross-linked structure, contain epoxy group, ehter bond, hydroxyl isopolarity group and activity in epoxidized soybean oil
Group makes acrylate latex show excellent adhesive strength, electrical insulation capability and high temperature resistance, and it is resistance to that phenyl ring assigns latex
Hot and rigid, epoxy group and hydroxyl make material that there is reactivity adhesion strength, the dehydrating condensation of multiple hydroxyls to make crosslink density
Rise, under the hot conditions when circuit board works, latex makes Porous Cu radiate because of high crosslink density viscosity meeting minor change
The interfacial property of piece and electronic component is stablized, and in addition vinyl ester resin can be by manganese-zinc ferrite powder and metal by coupled action
The compatibility of element improves, and reduces contact resistance, and expanded graphite powder can expand and the manganese of heat conduction in heat-conducting resin when high temperature
Zn ferrite powder connects to form heat conduction network, to improve the heat conductivility of cooling fin, has a extensive future.
Specific implementation mode
It is that 20% liquor potassic permanganate pours into beaker by the pH mass fractions for being 2~3, warming-in-water takes to 45~50 DEG C
Polyurethane foam is put into beaker and polyurethane foam is made to be completely immersed in acid permanganate soln, 10~15min of impregnation,
Roughening polyurethane foam is obtained, polyurethane foam will be roughened and be put into mass fraction to be impregnated in 5% oxalic acid solution, use glass bar
Roughening 10~15min of polyurethane foam is stirred and squeezed, polyurethane matrix is obtained；It is 5% to configure 100~120mL mass fractions
Tin chloride solution, into tin chloride solution plus 5~7g glass puttys, the hydrochloric acid that 30~40mL mass fractions are 10% obtain sensitizing solution, will
Polyurethane matrix is put into 5~8min of immersion in sensitizing solution, obtains sensitization polyurethane matrix, and the palladium bichloride for being 8% by mass fraction is molten
The hydrochloric acid solution that liquid and mass fraction are 5% is mixed to get solution glue in equal volume, above-mentioned sensitization polyurethane matrix is immersed 120~
150mL is solved in glue, after dispergation handles 4~5min, is taken out polyurethane matrix and is put into the first that 200~220mL mass fractions are 75%
In aldehyde solution, 5~10min is impregnated, surface active polyurethane matrix is obtained；It counts in parts by weight, by 20~25 parts of copper sulphate, 30
~40 parts of formaldehyde, 80~90 parts of sodium tartrates, 12~15 parts of sodium hydroxides, which are put into 400~500 parts of distilled water, to be dissolved, and is changed
Electroplate liquid is learned, 90~100 parts of surface active polyurethane matrixes are put into chemical-electrical plating solution, after being heated to 40~45 DEG C,
5~10 parts of di-mercaptobenzothiazolbies are added into chemical-electrical plating solution, 3~4h of insulation reaction obtains micro- copper facing polyurethane；Configuration
400~500mL mass fractions be 40% copper-bath, to copper-bath be added 50~60mL mass fractions be 98% it is dense
Sulfuric acid, 8~10g polyethylene glycol, 12~15g1,4- butynediols, 20~30g nickel chlorides, obtain electrolyte, electrolyte are put into
Electrolytic cell, using copper rod as anode, micro- copper facing polyurethane as cathode, control current density is 2~3A/dm3, it is electrolysed 2~3h,
Taking-up cathode is washed with water 3~5 times and obtains copper facing polyurethane；It counts in parts by weight, 50~60 parts of steamings is added into four-hole boiling flask
Distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 200~220r/min
It mixes, warming-in-water continuously adds 40~45 parts of acrylic acid, four-hole boiling flask is added in 20~30 parts of methacrylic acids to 70~80 DEG C
Afterwards, the reaction was continued 10~15min, obtains seed emulsion；It counts in parts by weight, 20~30 parts of rings is added into above-mentioned four-hole boiling flask
Oxygen soybean oil, then 1~3 part of potassium peroxydisulfate, drop are added dropwise with the drop rate of 3~5mL/min into four-hole boiling flask with dropping funel
After adding, 30~40min of insulation reaction continues to be heated to 90~100 DEG C, 45~55min of insulation reaction, then is cooled to
55~60 DEG C, it is 6.0~7.0 to adjust pH with the ammonium hydroxide of mass fraction 20%, and discharging obtains acrylate latex, takes 20~30 parts
Ethylene-vinyl acetate copolymer, 40~50 parts of manganese-zinc ferrite powder, 10~15 parts of expanded graphite powder, 8~10 parts of vinyl esters
Resin is put into reaction kettle, is heated to 230~250 DEG C, is kneaded 4~5h, heat-conducting resin is obtained after being cooled to room temperature；It will plating
Copper polyurethane is put into resistance furnace, be passed through into resistance furnace hydrogen, nitrogen volume ratio be 3 ︰ 1 mixed gas, with 2~3 DEG C/
The rate of min is warming up to 400~420 DEG C, keeps the temperature reductase 12~3h, is continuously heating to 850~900 DEG C, and heat preservation 3~4h of pyrolysis is obtained
Enter in porous copper product to porous copper product, then by the heat-conducting resin seepage flow of pre- heat fusing, is obtained after cooled to room temperature
The porous copper radiating rib of high heat conduction.
Example 1
It is that 20% liquor potassic permanganate pours into beaker by the pH mass fractions for being 2, warming-in-water takes polyurethane foam to 45 DEG C
It is put into beaker and polyurethane foam is made to be completely immersed in acid permanganate soln, impregnation 10min obtains roughening polyurethane
Foam will be roughened polyurethane foam and be put into mass fraction to be impregnated in 5% oxalic acid solution, and be stirred with glass bar and squeeze roughening
Polyurethane foam 10min, obtains polyurethane matrix；The tin chloride solution that 100mL mass fractions are 5% is configured, to tin chloride solution
In plus 5g glass puttys, 30mL mass fractions be 10% hydrochloric acid obtain sensitizing solution, polyurethane matrix is put into sensitizing solution and is impregnated
5min obtains sensitization polyurethane matrix, the hydrochloric acid solution etc. for being 5% by palladium chloride solution and mass fraction that mass fraction is 8%
Volume mixture obtains solution glue, and above-mentioned sensitization polyurethane matrix is immersed in 120mL solution glues, after dispergation handles 4min, is taken out
Polyurethane matrix is put into the formalin that 200mL mass fractions are 75%, is impregnated 5min, is obtained surface active polyurethane matrix；
It counts in parts by weight, 20 parts of copper sulphate, 30 parts of formaldehyde, 80 parts of sodium tartrates, 12 parts of sodium hydroxides is put into 400 parts of distilled water
Dissolving, obtains chemical-electrical plating solution, 90 parts of surface active polyurethane matrixes is put into chemical-electrical plating solution, are heated to 40 DEG C
Afterwards, 5 parts of di-mercaptobenzothiazolbies are added into chemical-electrical plating solution, insulation reaction 3h obtains micro- copper facing polyurethane；Configure 400mL
The concentrated sulfuric acid that 50mL mass fractions are 98%, the poly- second of 8g two is added to copper-bath in the copper-bath that mass fraction is 40%
Alcohol, 12g1,4- butynediols, 20g nickel chlorides, obtain electrolyte, and electrolyte is put into electrolytic cell, using copper rod as anode, micro-
For copper facing polyurethane as cathode, control current density is 2A/dm3, it is electrolysed 2h, cathode is taken out and is washed with water that obtain copper facing for 3 times poly-
Urethane；It counts in parts by weight, 50 parts of distilled water, 10 parts of dodecyl sodium sulfates, 4 parts of sodium bicarbonates is added into four-hole boiling flask,
Start blender to stir with the rotating speed of 200r/min, warming-in-water continuously adds 40 parts of acrylic acid, 20 parts of metering systems to 70 DEG C
After four-hole boiling flask is added in acid, the reaction was continued 10min obtains seed emulsion；It counts, is added into above-mentioned four-hole boiling flask in parts by weight
20 parts of epoxidized soybean oils, then 1 part of potassium peroxydisulfate, drop are added dropwise with the drop rate of 3mL/min into four-hole boiling flask with dropping funel
After adding, insulation reaction 30min continues to be heated to 90 DEG C, insulation reaction 45min, then is cooled to 55 DEG C, with quality point
It is 6.0 that the ammonium hydroxide of number 20%, which adjusts pH, and discharging obtains acrylate latex, take 20 parts of ethylene-vinyl acetate copolymers, 40 parts
Manganese-zinc ferrite powder, 10 parts of expanded graphite powder, 8 parts of vinyl ester resins are put into reaction kettle, are heated to 230 DEG C, are kneaded
4h obtains heat-conducting resin after being cooled to room temperature；Copper facing polyurethane is put into resistance furnace, hydrogen, nitrogen are passed through into resistance furnace
Volume ratio is the mixed gas of 3 ︰ 1, is warming up to 400 DEG C with the rate of 2 DEG C/min, keeps the temperature reductase 12 h, be continuously heating to 850 DEG C,
Heat preservation pyrolysis 3h obtains porous copper product, then the heat-conducting resin seepage flow of pre- heat fusing is entered in porous copper product, natural cooling
The porous copper radiating rib of high heat conduction is obtained after to room temperature.
Example 2
It is that 20% liquor potassic permanganate pours into beaker by the pH mass fractions for being 2, warming-in-water takes polyurethane foam to 47 DEG C
It is put into beaker and polyurethane foam is made to be completely immersed in acid permanganate soln, impregnation 12min obtains roughening polyurethane
Foam will be roughened polyurethane foam and be put into mass fraction to be impregnated in 5% oxalic acid solution, and be stirred with glass bar and squeeze roughening
Polyurethane foam 12min, obtains polyurethane matrix；The tin chloride solution that 110mL mass fractions are 5% is configured, to tin chloride solution
In plus 6g glass puttys, 35mL mass fractions be 10% hydrochloric acid obtain sensitizing solution, polyurethane matrix is put into sensitizing solution and is impregnated
6min obtains sensitization polyurethane matrix, the hydrochloric acid solution etc. for being 5% by palladium chloride solution and mass fraction that mass fraction is 8%
Volume mixture obtains solution glue, and above-mentioned sensitization polyurethane matrix is immersed in 140mL solution glues, after dispergation handles 4min, is taken out
Polyurethane matrix is put into the formalin that 210mL mass fractions are 75%, is impregnated 7min, is obtained surface active polyurethane matrix；
It counts in parts by weight, 22 parts of copper sulphate, 35 parts of formaldehyde, 85 parts of sodium tartrates, 14 parts of sodium hydroxides is put into 450 parts of distilled water
Dissolving, obtains chemical-electrical plating solution, 95 parts of surface active polyurethane matrixes is put into chemical-electrical plating solution, are heated to 42 DEG C
Afterwards, 7 parts of di-mercaptobenzothiazolbies are added into chemical-electrical plating solution, insulation reaction 3.5h obtains micro- copper facing polyurethane；Configuration
It is poly- that the concentrated sulfuric acid, 9g that 55mL mass fractions are 98% is added to copper-bath in the copper-bath that 450mL mass fractions are 40%
Ethylene glycol, 14g1,4- butynediols, 25g nickel chlorides, obtain electrolyte, and electrolyte is put into electrolytic cell, using copper rod as sun
As cathode, control current density is 2A/dm for pole, micro- copper facing polyurethane3, it is electrolysed 2.5h, taking-up cathode is washed with water 4 times and obtains
Copper facing polyurethane；It counts in parts by weight, 55 parts of distilled water, 12 parts of dodecyl sodium sulfates, 4 parts of carbonic acid is added into four-hole boiling flask
Hydrogen sodium is started blender and is stirred with the rotating speed of 210r/min, and warming-in-water continuously adds 42 parts of acrylic acid, 25 parts of first to 75 DEG C
After four-hole boiling flask is added in base acrylic acid, the reaction was continued 12min obtains seed emulsion；It counts in parts by weight, to above-mentioned four-hole boiling flask
25 parts of epoxidized soybean oils of middle addition, then 2 parts of persulfuric acid are added dropwise with the drop rate of 4mL/min into four-hole boiling flask with dropping funel
Potassium, after being added dropwise, insulation reaction 35min continues to be heated to 95 DEG C, insulation reaction 50min, then is cooled to 57 DEG C, uses
It is 6.7 that the ammonium hydroxide of mass fraction 20%, which adjusts pH, and discharging obtains acrylate latex, takes 25 parts of ethylene-vinyl acetate copolymerization
Object, 45 parts of manganese-zinc ferrite powder, 12 parts of expanded graphite powder, 9 parts of vinyl ester resins are put into reaction kettle, are heated to 240
DEG C, it is kneaded 4.5h, heat-conducting resin is obtained after being cooled to room temperature；Copper facing polyurethane is put into resistance furnace, is passed through into resistance furnace
Hydrogen, the mixed gas that nitrogen volume ratio is 3 ︰ 1, are warming up to 410 DEG C with the rate of 2 DEG C/min, reductase 12 .5h are kept the temperature, after of continuing rising
To 870 DEG C, heat preservation pyrolysis 3.5h obtains porous copper product, then the heat-conducting resin seepage flow of pre- heat fusing is entered porous copper material temperature
The porous copper radiating rib of high heat conduction is obtained in material, after cooled to room temperature.
Example 3
It is that 20% liquor potassic permanganate pours into beaker by the pH mass fractions for being 3, warming-in-water takes polyurethane foam to 50 DEG C
It is put into beaker and polyurethane foam is made to be completely immersed in acid permanganate soln, impregnation 15min obtains roughening polyurethane
Foam will be roughened polyurethane foam and be put into mass fraction to be impregnated in 5% oxalic acid solution, and be stirred with glass bar and squeeze roughening
Polyurethane foam 15min, obtains polyurethane matrix；The tin chloride solution that 120mL mass fractions are 5% is configured, to tin chloride solution
In plus 7g glass puttys, 40mL mass fractions be 10% hydrochloric acid obtain sensitizing solution, polyurethane matrix is put into sensitizing solution and is impregnated
8min obtains sensitization polyurethane matrix, the hydrochloric acid solution etc. for being 5% by palladium chloride solution and mass fraction that mass fraction is 8%
Volume mixture obtains solution glue, and above-mentioned sensitization polyurethane matrix is immersed in 150mL solution glues, after dispergation handles 5min, is taken out
Polyurethane matrix is put into the formalin that 220mL mass fractions are 75%, is impregnated 10min, is obtained surface active polyurethane
Body；It counts in parts by weight, 25 parts of copper sulphate, 40 parts of formaldehyde, 90 parts of sodium tartrates, 15 parts of sodium hydroxides is put into 500 parts of distillations
It is dissolved in water, obtains chemical-electrical plating solution, 100 parts of surface active polyurethane matrixes are put into chemical-electrical plating solution, are heated to
After 45 DEG C, 10 parts of di-mercaptobenzothiazolbies are added into chemical-electrical plating solution, insulation reaction 4h obtains micro- copper facing polyurethane；Configuration
The concentrated sulfuric acid, the 10g that 60mL mass fractions are 98% is added to copper-bath in the copper-bath that 500mL mass fractions are 40%
Polyethylene glycol, 15g1,4- butynediols, 30g nickel chlorides, obtain electrolyte, and electrolyte is put into electrolytic cell, using copper rod as sun
As cathode, control current density is 3A/dm for pole, micro- copper facing polyurethane3, it is electrolysed 3h, taking-up cathode is washed with water 5 times and is plated
Copper polyurethane；It counts in parts by weight, 60 parts of distilled water, 15 parts of dodecyl sodium sulfates, 5 parts of bicarbonates is added into four-hole boiling flask
Sodium is started blender and is stirred with the rotating speed of 220r/min, and warming-in-water continuously adds 45 parts of acrylic acid, 30 parts of methyl to 80 DEG C
After four-hole boiling flask is added in acrylic acid, the reaction was continued 15min obtains seed emulsion；It counts in parts by weight, into above-mentioned four-hole boiling flask
30 parts of epoxidized soybean oils are added, then 3 parts of persulfuric acid are added dropwise with the drop rate of 5mL/min into four-hole boiling flask with dropping funel
Potassium, after being added dropwise, insulation reaction 40min continues to be heated to 100 DEG C, insulation reaction 55min, then is cooled to 60 DEG C, uses
It is 7.0 that the ammonium hydroxide of mass fraction 20%, which adjusts pH, and discharging obtains acrylate latex, takes 30 parts of ethylene-vinyl acetate copolymerization
Object, 50 parts of manganese-zinc ferrite powder, 15 parts of expanded graphite powder, 10 parts of vinyl ester resins are put into reaction kettle, are heated to
250 DEG C, it is kneaded 5h, heat-conducting resin is obtained after being cooled to room temperature；Copper facing polyurethane is put into resistance furnace, is passed through into resistance furnace
Hydrogen, the mixed gas that nitrogen volume ratio is 3 ︰ 1 are warming up to 420 DEG C with the rate of 3 DEG C/min, and heat preservation reduction 3h continues to heat up
To 900 DEG C, heat preservation pyrolysis 4h obtains porous copper product, then the heat-conducting resin seepage flow of pre- heat fusing is entered in porous copper product,
The porous copper radiating rib of high heat conduction is obtained after cooled to room temperature.
Comparative example
With the porous copper radiating rib of high heat conduction of Weifang company production as a comparison case to high heat conduction Porous Cu produced by the present invention
The porous copper radiating rib progressive of high heat conduction in cooling fin and comparative example can detect, and testing result is as shown in table 1：
Test method：
Heat dissipation performance is tested：The cooling fin of identical size in example 1~3 and comparative example is welded on identical aluminium heat dissipation base dress
It sets, is compared（The radiator portion of aluminium heat dissipation base is removed after measuring device integral heat sink performance）As a result as follows：
Using forced circulation mode, wind speed 5m/s, the radiating efficiency of cooling fin of the invention is 5.1 times of comparative example cooling fin
（Vertical fins）；Using the natural type of cooling, the radiating efficiency of cooling fin of the invention is 1.9 times of comparative example cooling fin.
Surface area test is detected using Surface Area Analyzer.
Exothermic temperature is tested：By the cooling fin of the identical size in example 1~3 and comparative example in same test equipment
Compare, test condition is identical, after a certain period of time, measures the temperature of each equipment.
Determination of conductive coefficients is detected using heat conduction coefficient tester.
Porosity test is detected using porosity tester.
1 cooling fin performance measurement result of table
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Surface area（cm2） | 9.67 | 9.76 | 9.85 | 3.53 |
| Exothermic temperature（℃） | 45 | 44 | 43 | 62 |
| Thermal coefficient（W/mK） | 370 | 375 | 380 | 250 |
| The porosity（%） | 55.0 | 55.8 | 56.5 | 23.5 |
Radiating efficiency according to the cooling fin of the present invention of data among the above is 5.1 times of comparative example cooling fin radiating efficiency,
Perfect heat-dissipating, surface area is big, and the thermal diffusivity of cooling fin is good, and radiating efficiency is high, and thermal coefficient is high, and thermal resistance is relatively low, and thermal diffusivity is good,
It has broad application prospects.
Claims (8)
1. a kind of preparation method of the porous copper radiating rib of high heat conduction, it is characterised in that specifically preparation process is：
（1）Liquor potassic permanganate is poured into beaker, warming-in-water, polyurethane foam is taken to be put into beaker and makes polyurethane foam
It is completely immersed in acid permanganate soln, impregnation obtains roughening polyurethane foam, and roughening polyurethane foam is put into quality
It is impregnated in the oxalic acid solution that score is 5%, roughening polyurethane foam is stirred and squeezed with glass bar, obtains polyurethane matrix；
（2）100~120mL tin chloride solutions are configured, add 5~7g glass puttys, 30~40mL hydrochloric acid to obtain into tin chloride solution quick
Change liquid, polyurethane matrix is put into sensitizing solution and is impregnated, sensitization polyurethane matrix is obtained, by palladium chloride solution and hydrochloric acid solution etc.
Volume mixture obtains solution glue, and above-mentioned sensitization polyurethane matrix is immersed in 120~150mL solution glues, after dispergation processing, is taken out
Polyurethane matrix is put into 200~220mL formalins, is impregnated, is obtained surface active polyurethane matrix；
（3）It counts in parts by weight, by 20~25 parts of copper sulphate, 30~40 parts of formaldehyde, 80~90 parts of sodium tartrates, 12~15 parts of hydrogen
Sodium oxide molybdena, which is put into 400~500 parts of distilled water, to be dissolved, and chemical-electrical plating solution is obtained, by 90~100 parts of surface active polyurethane matrixes
It is put into chemical-electrical plating solution, after heat temperature raising, 5~10 parts of di-mercaptobenzothiazolbies of addition into chemical-electrical plating solution, insulation reaction,
Obtain micro- copper facing polyurethane；
（4）The copper-bath that 400~500mL mass fractions are 40% is configured, the dense sulphur of 50~60mL is added to copper-bath
Acid, 8~10g polyethylene glycol, 12~15g1,4- butynediols, 20~30g nickel chlorides obtain electrolyte, electrolyte are put into electricity
Slot is solved, using copper rod as anode, micro- copper facing polyurethane as cathode, is electrolysed, taking-up cathode is washed with water 3~5 times and obtains copper facing
Polyurethane；
（5）Count in parts by weight, into four-hole boiling flask be added 50~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~
5 parts of sodium bicarbonates are started blender and are stirred with the rotating speed of 200~220r/min, and warming-in-water continuously adds 40~45 parts of propylene
After four-hole boiling flask is added in acid, 20~30 parts of methacrylic acids, the reaction was continued obtains seed emulsion；
（6）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 with the drop rate of 3~5mL/min in flask, after being added dropwise, insulation reaction continues heating and rises
Temperature, insulation reaction, then cool down, pH is adjusted with ammonium hydroxide, discharging obtains acrylate latex, takes 20~30 parts of ethene-vinyl acetates
Ester copolymer, 40~50 parts of manganese-zinc ferrite powder, 10~15 parts of expanded graphite powder, 8~10 parts of vinyl ester resins are put into reaction
In kettle, heat temperature raising is kneaded, heat-conducting resin is obtained after being cooled to room temperature；
（7）Copper facing polyurethane is put into resistance furnace, mixed gas is passed through into resistance furnace, temperature programming to 400~420 DEG C,
Heat preservation reduction, is continuously heating to 850~900 DEG C, heat preservation pyrolysis, obtains porous copper product, then by the heat-conducting resin of pre- heat fusing
Seepage flow enters in porous copper product, and the porous copper radiating rib of high heat conduction is obtained after cooled to room temperature.
2. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（1）
The pH of the liquor potassic permanganate is 2~3, and the mass fraction of liquor potassic permanganate is 20%, after warming-in-water temperature be 45~
50 DEG C, the impregnation time is 10~15min, and the mass fraction of oxalic acid solution is 5%, the polyurethane foam time is 10~
15min。
3. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（2）
The mass fraction of the tin chloride solution is 5%, and the mass fraction of hydrochloric acid is 10%, and soaking time is 5~8min in sensitizing solution,
It is 8% by the mass fraction of palladium chloride solution, the mass fraction of hydrochloric acid solution is 5%, and dispergation processing time is 4~5min, formaldehyde
The mass fraction of solution is 75%.
4. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（3）
Temperature is 40~45 DEG C after the heat temperature raising, and the insulation reaction time is 3~4h.
5. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（4）
The mass fraction of the copper-bath is 40%, and the mass fraction of the concentrated sulfuric acid is 98%, when electrolysis control current density be 2~
3A/dm3, electrolysis time is 2~3h.
6. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（5）
The warming-in-water is 70~80 DEG C, and the reaction was continued, and the time is 10~15min.
7. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（6）
The insulation reaction time be 30~40min, continue heat temperature raising be 90~100 DEG C, the insulation reaction time be 45~
55min, then it is 55~60 DEG C to cool down, the mass fraction 20% of ammonium hydroxide, it is 6.0~7.0 to adjust pH, and reaction kettle heat temperature raising is 230
~250 DEG C, mixing time is 4~5h.
8. a kind of preparation method of the porous copper radiating rib of high heat conduction according to claim 1, it is characterised in that：Step（7）
The mixed gas is that hydrogen, nitrogen are that 3 ︰ 1 are made by volume, and resistance furnace heating rate is 2~3 DEG C/min, and heat preservation is also
The former time is 2~3h, and heat preservation pyrolysis time is 3~4h.
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