CN101518867B - Integral die forming manufacturing method for graphite-base composite material radiator - Google Patents

Integral die forming manufacturing method for graphite-base composite material radiator Download PDF

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CN101518867B
CN101518867B CN2009100613230A CN200910061323A CN101518867B CN 101518867 B CN101518867 B CN 101518867B CN 2009100613230 A CN2009100613230 A CN 2009100613230A CN 200910061323 A CN200910061323 A CN 200910061323A CN 101518867 B CN101518867 B CN 101518867B
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radiator
graphite
graphitization
temperature
hour
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CN101518867A (en
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史玉升
张军
张少君
魏青松
刘锦辉
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Abstract

The invention discloses an integral die forming manufacturing method for a graphite-base composite material radiator. The method comprises the following steps: firstly, mixing and pinching moderate temperature coal pitch, graphite and petroleum coke at a temperature of between 95 and 195 DEG C to prepare paste, adjusting the temperature of the prepared paste to between 70 and 130 DEG C, filling the paste into a radiator die for die forming, setting the die forming pressure of 10 to 90 MPa, and keeping the pressure for 1 to 10 minutes; secondly, baking and graphitizing the raw die forming product; and finally impregnating the graphitized die forming product with an epoxy resin to obtain the radiator. The method can be used to manufacture the graphite radiator with a complex shape; the method has the characteristics of great flexibility, simple process flow, high production efficiency, accurate product size and good product surface quality. The method can be used to manufacture the graphite radiator with the complex shape. The radiator has the advantages of good heat conduction, light mass, and the like. The technological process has little pollution, simplicity and feasibility, low energy consumption and high efficiency, and easy realization of mechanization and automated production.

Description

A kind of integral die forming manufacturing method for graphite-base composite material radiator
Technical field
The present invention relates to electronic device class thermal source heat sink technology field, be specially a kind of integral die forming manufacturing method of graphite-base composite material radiator.
Background technology
Usually, electronic device or equipment the time can produce a lot of heats in work, as dispel the heat and badly will produce higher temperature, thereby the operate as normal that influences components and parts causes the instability of system, even cause the damage of system.Show that according to related data for electronic equipment, present Problem of Failure 50% all causes owing to device is overheated.Simultaneously, along with constantly bringing forth new ideas of science and technology, the improving constantly of large scale integrated circuit integration density, the speed of service of microprocessor is more and more faster, and function integrated in monolithic chip is also more and more, and the energy that chip need consume will be more.Moore's Law is also pointed out: approximately every a year and a half, the transistor size of chip can double, and corresponding power consumption also can double.This means that all electronic chip will be more and more hotter, and heat dissipation problem has become the bottleneck that the restriction chip performance promotes.Therefore the cooling problem of electronic device is more and more noticeable.
At present, the used radiator major part of electronic device still adopts fin shape radiator, usually by aluminium or copper and alloy manufacturing thereof.In order to strengthen the heat exchange of element in limited space, to satisfy the requirement of its Performance And Reliability index to conducting heat, engineers is often improved on the radiator profile.Yet be limited to the deficiency (wherein the fine copper thermal conductivity factor is 398W/mK, and the fine aluminium thermal conductivity factor is 237W/mK) owing to copper, aluminium and the heat-sinking capability of alloy own thereof, improved effect is also not obvious.Research points out, the graphite microcrystal material surpasses 2000W/mK along the thermal conductivity of (002) face direction, has than metallic copper, thermal conductivity that aluminium is higher, and the lower density of graphite material itself simultaneously very meets the demand of current electronic device lightweight development.Therefore, graphite material has begun more and more to be paid close attention in the heat radiation field, and relevant researcher has been made into radiator, uses aspects such as notebook computer, LCD TV, has obtained good effect.Yet because there is great fragility in graphite material, have certain difficulty on being shaped making, thus this kind radiator often shape is very simple, it is planar to be generally single flat, or it is carried out simple concatenation becomes required form.Even so, shape is still simple, be difficult to field is widely arrived in its application, and its complex process of while, efficient is low, and is not suitable for industrialization production.Current, the method for monolithic molding heat radiator does not appear in the world as yet.Therefore, seek out a kind of can monolithic molding the method for complicated shape heat radiator significant for changing this present situation.
Summary of the invention
Purpose of the present invention is to provide a kind of heat radiator integral die forming manufacturing method of simple, low-consumption high-efficiency just, and adopt this method can make the heat radiator of complex contour, and the heat radiator of manufacturing has, and heat conduction is good, the advantage of light weight.
Integral die forming manufacturing method for graphite-base composite material radiator provided by the invention, its step comprises
(1), medium temperature coal pitch, graphite and petroleum coke mixed between 95~195 ℃ pinch, make thickener, wherein, the mass percent of medium temperature coal pitch and graphite is respectively 20%~40% and 25%~40%;
(2), with thickener temperature adjustment to 70~130 that make ℃, insert and carry out die forming in the radiator mould, molding pressure is 10~90MPa, and keeps this pressure 1~10 minute;
(3), the mold pressing raw product is carried out roasting and graphitization processing;
(4), to the graphitization goods epoxy resin that infiltrates, promptly get radiator.
The present invention at first utilizes mould pressing process to have added the graphite-base composite material monolithic molding of bonding agent, pass through proper heat treatment then, comprise that roasting, graphitization make radiator have sufficiently high thermal conductivity factor, strengthen by the infiltration resin again, finally obtain required heat radiator.Following defective when this invention has overcome metal heat sinks such as conventional method manufactured copper, aluminium: the severe contamination the when exploitation of (1) raw material is smelted; (2) radiator is heavier, is unfavorable for the lightweight of electronic product; (3) prices of raw and semifnished materials are higher; (4) heat-sinking capability is relatively low etc.Also avoided simultaneously existing non-integral to make the following drawback of heat radiator: (1) raw material are handled loaded down with trivial details; (2) can only the be shaped radiator of simple shape; (3) splicing shaping timeliness rate is low; (4) be difficult to realize mechanization and automated production etc.
Manufacture method provided by the invention has the following advantages: (1) can the whole heat radiator of making complex contour; (2) flexibility is big, can be implemented in production shape on same the press, heat radiator that specification is different with kind by changing molding die; (3) need not follow-up machined, technological process is simple, the production efficiency height; (4) product size is accurate, and surface quality is good.This method can be made complex-shaped heat radiator, and this kind radiator has advantages such as heat conduction is good, light weight, can satisfy the current new demand that proposes for radiator performance.The technical process of the inventive method is polluted little, simple, easily realizes mechanization and automated production.
The specific embodiment
The integral die forming manufacturing method of graphite-base composite material radiator provided by the invention, its manufacturing process steps is:
(1), raw material is carried out heat mix and to pinch, make mix, thickener that visco-plasticity is good;
Describedly raw material is carried out heat mix and to pinch, make mix, thickener that visco-plasticity is good is meant medium temperature coal pitch put into kneading machine, the rising temperature is also mixed simultaneously and is pinched, and pack into after coal tar pitch partly begins fusing graphite and petroleum coke mixed powder are proceeded to mix and pinched.Or earlier medium temperature coal pitch powder, graphite powder and the petroleum coke powder for preparing stirred in mixer in advance, make its even mixing, mix in the kneading machine of packing into simultaneously then and pinch.Kneading temperature is controlled between 95~195 ℃, mixes and pinches time remaining 20~50 minutes, and the mass percent of coal tar pitch, graphite is respectively 20%~40% and 25%~40%, and all the other are petroleum coke powder.
(2), the thickener that makes is inserted carried out die forming in the radiator mould;
The thickener that makes inserted carry out die forming in the radiator mould and be meant and pack into and regulate temperature in the baking oven, perhaps thickener is put into and carried out the cool material of mechanization on the cooler, make its temperature to 70~130 ℃ mixing the thickener pinch; Immediately it is inserted mould then and carry out die forming, molding pressure is 10~90MPa, and keeps this pressure 1~10 minute, then the demoulding take out the mold pressing raw product.
(3), the mold pressing raw product is carried out roasting and graphitization processing;
The maximum temperature of the mold pressing raw product being carried out roasting is 900~1500 ℃, the heating rate in each stage of roasting process is for maintaining 30~60 ℃/hour from room temperature to 330 a ℃ stage, stage is at 10~25 ℃/hour from 330 ℃ to 800 ℃, final stage is 40~80 ℃/hour, is incubated 1~8 hour after reaching maximum temperature, begins to cool down then, in initial cooling velocity per hour must be controlled at 50 ℃, the cooling of can giving free rein to during to 800 ℃ can be come out of the stove in the time of 400 ℃, promptly gets roasting product.
Described graphitization processing is meant that roasting product is put into graphitizing furnace carries out graphitization processing, and the graphitization maximum temperature is 2000~3000 ℃.Heating rate when the graphitization incipient stage is a room temperature to 1100 ℃ is 45~100 ℃/hour, reduce heating rate to 25~40 ℃/hour then, make temperature reach 1700 ℃, continue to heat up and reach 2000~3000 ℃ until temperature, kept under maximum temperature 1~10 hour, cooling is come out of the stove and is promptly got the graphitization goods then.
(4), the graphitization goods epoxy resin that infiltrates is promptly got final radiator product.
Described the graphitization goods epoxy resin that infiltrates is meant the graphitization goods is put into the vacuum impregnation equipment epoxy resin that infiltrates, satisfy the requirement of using to improve its intensity.After the graphitization goods were put into impregnating autoclave, dipping process must vacuumize earlier, makes jar internal gas pressure not be higher than 10KPa, sucks resin then, and the amount of the resin that sucks must be flooded the graphitization goods fully.In impregnating autoclave, charge into gases at high pressure then, make a jar internal gas pressure be not less than 1MPa, keep this pressure can release take out goods after 1~15 minute.Immediately goods are put into baking oven then and be cured, taking-up gets final product behind the completion of cure.
Below in conjunction with embodiment the present invention is further described:
Example 1
(1) medium temperature coal pitch of mass percent 20% is packed in the kneading machine, begin heating, heating-up temperature is transferred to 175 ℃, begin then to mix and pinch.Add the mixed powder of graphite and petroleum coke when the coal tar pitch partial melting, both respectively account for mass percent 25% and 55%, and kneading process continues 35 minutes, makes the good thickener of visco-plasticity.
(2) during the thickener that step (1) is made is packed baking oven into, adjust the temperature to 130 ℃.
(3) step (2) cooling is good thickener is inserted rapidly in the molding die, and the beginning mold pressing applies pressure to 55MPa, and keeps 1 minute under this pressure, forms the mold pressing raw product.
(4) the mold pressing raw product is taken out in the demoulding, and puts it into and carry out roasting in the roaster.The setting roasting technique is: at room temperature be warming up to 330 ℃ through 6 hours, be warming up to 550 ℃ in 12 hours, be warming up to 800 ℃ in 15 hours, be warming up to 1300 ℃ in 10 hours, be incubated after 8 hours, be cooled to 800 ℃ with 50 ℃/hour speed, cool to 400 ℃ then with the furnace, come out of the stove.
(5) the resulting roasting product of step (4) is packed in the graphitizing furnace, carry out graphitization, high graphitization temperature is 2500 ℃, the graphitization technique of setting is: at room temperature be warming up to 1100 ℃ through 20 hours, 24 hours to 1700 ℃, 10 hours to 2200 ℃, 12 hours to 2500 ℃, insulation is 1 hour under this temperature, and cooling is come out of the stove then.
(6) the graphitization goods of step (5) gained are put into the vacuum impregnation equipment epoxy resin that infiltrates, sucked epoxy resin to flooding the graphitization goods fully after being evacuated to 5KPa.Charge into gases at high pressure then immediately to 1MPa, release after keeping 2 minutes under this pressure, the taking-up goods are put into baking oven and are cured, and take out behind the completion of cure to get final product.
Example 2
(1) with mass percent is pack in mixer mechanical mixture 10 minutes of the mixed-powder of the petroleum coke of 40% medium temperature coal pitch, 40% graphite and 20%, then the powder that mixes is packed into and carry out heat in the kneading machine and mix and pinch, setting kneading temperature is 100 ℃, makes the good thickener of visco-plasticity in 50 minutes through mixing to pinch.
(2) thickener that step (1) is made is discharged to and is cooled to 90 ℃ on the cooler.
(3) step (2) cooling is good thickener is inserted rapidly in the molding die, and the beginning mold pressing applies pressure to 90MPa, and keeps 2 minutes under this pressure, forms the mold pressing raw product.
(4) the mold pressing raw product is taken out in the demoulding, and puts it into and carry out roasting in the roaster.The setting roasting technique is: at room temperature be warming up to 330 ℃ through 5 hours, be warming up to 550 ℃ in 10 hours, be warming up to 800 ℃ in 18 hours, be warming up to 1300 ℃ in 10 hours, be incubated after 3 hours, be cooled to 800 ℃ with 50 ℃/hour speed, cool to 400 ℃ then with the furnace, come out of the stove.
(5) the resulting roasting product of step (4) is packed in the graphitizing furnace, carry out graphitization, high graphitization temperature is 2100 ℃, the graphitization technique of setting is: at room temperature be warming up to 1100 ℃ through 20 hours, 30 hours to 1700 ℃, 10 hours to 2100 ℃, insulation was 10 hours under this temperature, and cooling is come out of the stove then.
(6) the graphitization goods of step (5) gained are put into the vacuum impregnation equipment epoxy resin that infiltrates, sucked epoxy resin to flooding the graphitization goods fully after being evacuated to 8KPa.Charge into gases at high pressure then immediately to 1MPa, release after keeping 10 minutes under this pressure, the taking-up goods are put into baking oven and are cured, and take out behind the completion of cure to get final product.
Example 3
(1) with mass percent is 30% medium temperature coal pitch, 30% graphite and 40%
Pack in mixer mechanical mixture 10 minutes of the mixed-powder of petroleum coke is carried out heat and is mixed and pinch in the kneading machine of then powder that mixes being packed into, setting kneading temperature is 195 ℃, makes the good thickener of visco-plasticity in 20 minutes through mixed pinching.
(2) thickener that step (1) is made is discharged to and is cooled to 110 ℃ on the cooler.
(3) step (2) cooling is good thickener is inserted rapidly in the molding die, and the beginning mold pressing applies pressure to 65MPa, and keeps 1.5 minutes under this pressure, forms the mold pressing raw product.
(4) the mold pressing raw product is taken out in the demoulding, and puts it into and carry out roasting in the roaster.The setting roasting technique is: at room temperature be warming up to 330 ℃ through 7.5 hours, be warming up to 550 ℃ in 10 hours, be warming up to 800 ℃ in 13 hours, be warming up to 1300 ℃ in 15 hours, be incubated after 5 hours, be cooled to 800 ℃ with 50 ℃/hour speed, cool to 400 ℃ then with the furnace, come out of the stove.
(5) the resulting roasting product of step (4) is packed in the graphitizing furnace, carry out graphitization, high graphitization temperature is 2300 ℃, the graphitization technique of setting is: at room temperature be warming up to 1100 ℃ through 16 hours, 18 hours to 1700 ℃, 15 hours to 2300 ℃, insulation was 3 hours under this temperature, and cooling is come out of the stove then.
(6) the graphitization goods of step (5) gained are put into the vacuum impregnation equipment epoxy resin that infiltrates, sucked epoxy resin to flooding the graphitization goods fully after being evacuated to 10KPa.Charge into gases at high pressure then immediately to 2MPa, release after keeping 15 minutes under this pressure, the taking-up goods are put into baking oven and are cured, and take out behind the completion of cure to get final product.
The above embodiment is a preferred embodiments of the present invention, is not to limit the scope of the present invention, so all equivalences of doing according to the described structure of the present patent application scope, feature and principle change or modify, all should be included in the present patent application scope.

Claims (1)

1. integral die forming manufacturing method for graphite-base composite material radiator, its step comprises
(1), medium temperature coal pitch, graphite and petroleum coke mixed between 95~195 ℃ pinch, make thickener, wherein the mass percent of coal tar pitch and graphite is respectively 20%~40% and 25%~40%;
(2), with thickener temperature adjustment to 70~130 that make ℃, insert and carry out die forming in the radiator mould, molding pressure is 10~90MPa, and keeps this pressure 1~10 minute;
(3), the mold pressing raw product is carried out roasting and graphitization processing;
(4), to the graphitization goods epoxy resin that infiltrates, promptly get radiator;
The detailed process of roasting is in the step (3):
The maximum temperature of roasting is 900~1500 ℃, the heating rate in each stage of roasting process is for maintaining 30~60 ℃/hour from room temperature to 330 a ℃ stage, stage is at 10~25 ℃/hour from 330 ℃ to 800 ℃, and final stage is 40~80 ℃/hour, is incubated 1~8 hour after reaching maximum temperature, begin to cool down then, initial cooling velocity is cooled to 400 ℃ and comes out of the stove, the cooling of giving free rein to during perhaps to 800 ℃ in per hour being controlled at 50 ℃, in the time of 400 ℃, come out of the stove, promptly get roasting product;
The detailed process of graphitization processing is in the step (3):
Roasting product is put into graphitizing furnace carry out graphitization processing, the graphitization maximum temperature is 2000~3000 ℃; Heating rate when the graphitization incipient stage is a room temperature to 1100 ℃ is 45~100 ℃/hour, reduce heating rate to 25~40 ℃/hour then, make temperature reach 1700 ℃, continue to heat up and reach 2000~3000 ℃ until temperature, kept under maximum temperature 1~10 hour, cooling is come out of the stove and is promptly got the graphitization goods then;
Detailed process is in the step (4):
After the graphitization goods are put into impregnating autoclave, dipping process vacuumizes earlier, make jar internal gas pressure smaller or equal to 10KPa, suck epoxy resin then, the amount of the epoxy resin that sucks is flooded the graphitization goods, charges into gases at high pressure then in impregnating autoclave, make jar internal gas pressure more than or equal to 1MPa, kept this pressure 1~15 minute, and again goods were put into baking oven and be cured, take out behind the completion of cure.
CN2009100613230A 2009-03-27 2009-03-27 Integral die forming manufacturing method for graphite-base composite material radiator Expired - Fee Related CN101518867B (en)

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CN102775147A (en) * 2012-01-16 2012-11-14 惠州市日盛光电科技有限公司 Manufacture process of carbon type superconductive heat radiator
CN102838108B (en) * 2012-06-16 2014-03-12 淄博大陆炭素有限责任公司 Minor-structure high-density graphite product and preparation method thereof
CN102795623B (en) * 2012-09-19 2013-06-19 江苏省特种设备安全监督检验研究院南通分院 Method for producing artificial graphite heat exchange element
CN108863423A (en) * 2018-07-03 2018-11-23 大同新成新材料股份有限公司 A kind of production technology of vinylite dipping electrode graphite
CN115340381B (en) * 2022-09-22 2023-04-07 东莞市鸿亿导热材料有限公司 Graphite heat dissipation material and preparation method thereof

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