CN102795617B - Graphite block material and preparation method thereof - Google Patents
Graphite block material and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种石墨块材料及其制备方法。石墨块材料包括两层石墨层结构，所述第一层石墨层结构各向异性，所述第一层石墨层结构设置在所述第二层石墨层结构上，所述第一层石墨层结构的相对高导热方向为与所述第二层石墨层结构表面平行的方向，两层石墨层结构经炭化烧成一体后形成一个整体。本发明石墨块材料由两层石墨层结构构成，第一层石墨层结构的相对高导热方向为与所述第二层石墨层结构表面平行的方向，且两层石墨层结构经炭化后形成一个整体，两者烧成一体使得两层结构近似“无缝”接触，界面热阻很低，传热效果显著。本发明的石墨块材料设置两层结构，且由于烧成一体，石墨块材料内部传热效果好，用于散热或者发热时的性能较显著。
The invention discloses a graphite block material and a preparation method thereof. The graphite block material includes two layers of graphite layer structure, the first layer of graphite layer structure is anisotropic, the first layer of graphite layer structure is arranged on the second layer of graphite layer structure, and the first layer of graphite layer structure The relatively high thermal conductivity direction is a direction parallel to the surface of the second graphite layer structure, and the two graphite layer structures form a whole after carbonization and firing. The graphite block material of the present invention is composed of two layers of graphite layer structure, the relatively high thermal conductivity direction of the first layer of graphite layer structure is a direction parallel to the surface of the second layer of graphite layer structure, and the two layers of graphite layer structure are formed after carbonization. On the whole, the two are fired together to make the two-layer structure nearly "seamless" contact, the interface thermal resistance is very low, and the heat transfer effect is remarkable. The graphite block material of the present invention has a two-layer structure, and because it is fired into one body, the internal heat transfer effect of the graphite block material is good, and the performance when used for heat dissipation or heat generation is relatively remarkable.
Description
Technical field
The present invention relates to the preparation method of graphite material and graphite material.
Background technology
Graphite has good heat, electrical property, has a wide range of applications.Say from microtexture, graphite crystal has laminate structure, has anisotropic feature, and its mechanics, electricity, thermal property are all anisotropic.Thermal conductivity is no exception, and anisotropic graphite material has a high heat conducting direction and vertical low heat conduction direction with it, and wherein relatively high heat conduction direction is the main heat conduction direction of graphite material.The graphite material crystal grain of natural formation is all smaller, and synthetic graphite is also there are no the report of the graphite monocrystalline of macro-size, and the graphite material that therefore macroscopic view is used is all the polycrystal of graphite, and the inner degree of crystallinity that always has some parts, is also that degree of graphitization is not high.For polycrystalline graphite material, if the orientation degree of crystallite is not high, or even random alignment, the thermal conductivity of entirety is not high, generally all below 100W/mK.Only have the high heat conduction direction of adjacent crystal grain parallel to each other or approach parallelly, entirety just can have higher thermal conductivity.The graphite material of high heat conduction, because graphite density is low, thermal conductivity is high, price is compared with the invocation point such as low and there is application prospect very widely on thermal management materials.
Being used as heat sink material is an important Application Areas of graphite material, and the heat that needs are left passes by graphite.If but use merely graphite material, the part conventionally only contacting with thermal source in graphite material can be brought into play radiating effect, all the other parts that do not contact with thermal source are difficult to bring into play heat dispersion, cause the now heat dispersion of graphite material to be difficult to comprehensive performance.On the other hand, due to high conduction and high temperature resistant, graphite is also the heating element of a lot of high temperature application.As heating element, be often placed in a side of heated parts, and existing graphite material is during as heating element, heat is propagated along all directions, wherein can pass to the finite energy of heated parts for heating, and energy utilization efficiency is lower.
Summary of the invention
Technical problem to be solved by this invention is: make up above-mentioned the deficiencies in the prior art, propose a kind of graphite block material and preparation method thereof, the graphite block material making is for dispelling the heat or the better performances of adstante febre.
Technical problem of the present invention is solved by following technical scheme:
A kind of graphite block material, comprise two-layer graphite linings structure, described the first layer graphite linings structural anisotropy, described the first layer graphite linings structure is arranged in described second layer graphite linings structure, the relatively high heat conduction direction of described the first layer graphite linings structure is the direction parallel with described second layer graphite linings body structure surface, and two-layer graphite linings structure forms an entirety after one is burnt till in charing.
Technical problem of the present invention is solved by following further technical scheme:
A kind of preparation method of graphite block material, comprise the following steps: anisotropic the first layer graphite linings structure is arranged in described second layer graphite linings structure, while setting, the relatively high heat conduction direction of described the first layer graphite linings structure is parallel to the surface of described second layer graphite linings structure; After again the charing of two-layer graphite linings structure being burnt till to one, form an entirety, obtain described graphite block material.
The beneficial effect that the present invention is compared with the prior art is:
In graphite block material of the present invention and preparation method thereof, graphite block material is made up of two-layer graphite linings structure, the relatively high heat conduction direction of the first layer graphite linings structure is the direction parallel with described second layer graphite linings body structure surface, and two-layer graphite linings structure forms an entirety after charing, both burn till one and make double-layer structure approximate " seamless " contact, interface resistance is very low, and heat-transfer effect is remarkable.Like this when dispelling the heat, second layer graphite linings structure is as heat dissipating layer, and the first layer graphite linings structure on it is as equal thermosphere, thereby makes the whole surface part of second layer graphite linings structure all for transferring heat heat radiation by equal thermosphere, improves radiating efficiency.For adstante febre, second layer graphite linings structure is as heating layer, the first layer graphite linings structure on it is as thermofin, can stop the heat of heating layer towards deviating from the parts direction transmission that needs heating, make heating layer heat as much as possible towards the parts place direction transmission of need heating, improve heating efficiency.Graphite block material of the present invention arranges double-layer structure, and owing to burning till one, graphite block material internal heat-transfer effect is good, for dispel the heat or the improved performance of adstante febre more remarkable.
Brief description of the drawings
Fig. 1 is the structural representation of the graphite block material in the specific embodiment of the invention one;
The use view that Fig. 2 is graphite block material in the specific embodiment of the invention one when dispelling the heat;
Fig. 3 is graphite block material in the specific embodiment of the invention one use view for adstante febre;
Fig. 4 is the section decomposing schematic representation of the graphite block material in the specific embodiment of the invention four;
Fig. 5 is the structural representation of the graphite block material in the specific embodiment of the invention six.
Embodiment
Below in conjunction with embodiment and contrast accompanying drawing the present invention is described in further details.
As shown in Figure 1, for the structural representation of graphite block material in this embodiment, graphite block material 100 comprises two-layer graphite linings structure, the first layer graphite linings structure A anisotropy, the first layer graphite linings structure A is arranged on described second layer graphite linings structure B, and the relatively high heat conduction direction of the first layer graphite linings structure A is the direction parallel with described second layer graphite linings structure B surface, and two-layer graphite linings structure forms an entirety after one is burnt till in charing.Relatively high heat conduction direction is herein the main heat conduction direction of graphite linings.In the vertical direction, horizontal direction all has thermal conductivity to graphite linings, as the thermal conductivity far of vertical direction is greater than the thermal conductivity of horizontal direction, can think that vertical direction is for relatively high heat conduction direction, mainly vertically heat conduction.Similarly, as the thermal conductivity far of horizontal direction is greater than the thermal conductivity of vertical direction, can think that horizontal direction is for relatively high heat conduction direction, main along continuous straight runs heat conduction.In figure, be the heat conduction direction of signal the first layer graphite linings structure A, showing its heat conduction direction with horizontal line is along the direction parallel with second layer graphite linings structure B surface.
When preparation, anisotropic the first layer graphite linings structure A is arranged on to second layer graphite linings structure B upper, while setting, the relatively high heat conduction direction of the first layer graphite linings structure A is parallel to the surface of second layer graphite linings structure B; After again the charing of two-layer graphite linings structure being burnt till to one, form an entirety, obtain graphite block material.Specifically can comprise the following steps: 1) be dispersed in solvent and form slurry being added with the natural flake graphite of binding agent or expanded graphite, as the component of the first layer graphite linings structure A; 2) slurry described step 1) being made is molded directly within on one deck graphite block or graphite precursor by the method for curtain coating or coating; 3) at the temperature lower than described solvent boiling point by described step 2) in be covered with the graphite block of slurry or graphite precursor is dried, form an entirety after two-layer graphite linings structure being burnt till to one after charing, obtain described graphite block material and make graphite block material.By the method for curtain coating, can make natural flake graphite reach the anisotropy orientation degree higher than techniques such as hot pressing herein, can further improve the soaking effect of heat insulation of the graphite block material making.
The following is specific examples, in conjunction with so that above-mentioned preparation method to be described: 1) petroleum pitch is dissolved in organic solvent, elimination insolubles, adds natural flake graphite to stir, form slurry, as the component of the first layer graphite linings structure A.2) with casting method, the above-mentioned slurry curtain coating making or coating are molded directly within to the high heat-conductive carbon piece surface for dispelling the heat, charcoal piece is as the component of second layer graphite linings structure B herein, coating thickness is 100 microns, at 100 DEG C, dry, 500 DEG C of charings 3 hours of pressurizeing, make double-layer structure burn till one, obtain burning till by two-layer graphite linings structure the overall graphite block material being integrally formed.
As shown in Figure 2, the use view while being used for dispelling the heat for the graphite block material of the specific embodiment of the invention.While being used for dispelling the heat, mainly utilize the second layer graphite linings structure B heat radiation in graphite block material 100, need the parts 200 of heat radiation to contact with the first layer graphite linings structure A in graphite block material 100.The relatively high heat conduction direction of the first layer graphite linings structure A is along the parallel direction in second layer graphite linings structure B surface, therefore heat in the first layer graphite linings structure A along the direction transmission parallel with the surface of second layer graphite linings structure B, thereby can be used as the effect of equal thermosphere performance soaking, heat is passed to the whole surperficial part of second layer graphite linings structure B, the whole volume of second layer graphite linings structure B all dispels the heat for transferring heat, and be no longer only to have the part contacting to dispel the heat with thermal component 200, can improve radiating efficiency.
As shown in Figure 3, be used for the use view of adstante febre for the graphite block material of the specific embodiment of the invention.For adstante febre, after mainly utilizing the second layer graphite linings structure B reception external heat in graphite block material 100, transfer heat to the parts that need heating, the parts 300 that need to add contact with the second layer graphite linings structure B in graphite block material 100, the relatively high heat conduction direction of the first layer graphite linings structure A is along the parallel direction in second layer graphite linings structure B surface, therefore low perpendicular to the direction thermal conductivity on the second graphite linings structure B surface, therefore in second layer graphite linings structure B, heat is not easy " penetrating " the first layer graphite linings structure A, the first layer graphite linings structure can be used as thermofin, can stop the heat of heating element (second layer graphite linings structure B) towards the direction transmission that deviates from the parts 300 that need heating, the parts 300 place direction transmission that heating element heat is heated towards need as much as possible, improve heating efficiency.
Above-mentioned, when heat radiation, soaking adds the scheme of heat radiation, and the heat insulation scheme that adds heating of adstante febre, can realize by two-layer graphite linings structure in theory, but find after research, because the interface resistance between two-layer graphite linings structure is very large, so only arrange and two-layerly improve obtained heat radiation heating effect and promote very limited.Therefore in this embodiment, graphite block material is except comprising that above-mentioned two-layer graphite linings structure, two-layer graphite linings structure also forms an entirety after one is burnt till in charing.Burn till the graphite block material that one obtains, near seamless connects, between double-layer structure interface, thermal resistance is very little, interface heat-transfer effect is good, for dispel the heat or the improved performance of adstante febre more remarkable, meanwhile graphite block material burns till one by charing, does not also increase process complexity, is to be applied to industrial scheme.
Preferably, between two-layer graphite linings structure, bond by binding agent, after bonding, after one is burnt till in charing, form an entirety.Binding agent can be pitch, mesophase pitch or resol.Increase after binding agent bonding after charing again, intermediate is converted into Carbon Materials, now also can improve interface resistance.Experiment records, and burns all-in-one-piece graphite block material after now adding binding agent, more than the thermal conductivity of the Carbon Materials that double-layer structure interface forms can reach 80W/mK.Comparatively speaking, at present industry is usually used in improving the heat interfacial material such as heat-conducting silicone grease, heat-conducting pad at hot interface, and the thermal conductivity of the best heat interfacial material of thermal conductivity is also less than 10W/mK at present.Effectively and thermal conductivity heat-transfer effect more than 80W/mK promotes herein, thermal resistance is very little, and interface heat-transfer effect is good, for dispel the heat or the improved performance of adstante febre more remarkable.
Embodiment two
This embodiment is with the difference of embodiment one: in this embodiment, control the thickness of one deck graphite linings structure A and get 0.01～1 millimeter.
In this embodiment, because the thickness of controlling the first layer graphite linings structure A is at 0.01～1 millimeter, thinner thickness, thinner graphite linings elasticity is better, therefore can make in use retention of graphite block material, avoids the generation of the situations such as cracking.In this scheme, require to control the thinner thickness of graphite linings structure, the use occasion thinner for thickness requirement can be suitable for.
The following is object lesson: prepare common graphite linings, set it as second layer graphite linings structure B, the ethanolic soln of coating film epoxy resin glue or resol in its surface, then bonding a layer thickness is 0.01～1 millimeter, density is greater than 1.7g/cm
3flexible graphite platelet.Herein, flexible graphite platelet is anisotropic graphite, as the first layer graphite linings structure A.When bonding, the high heat conduction direction of soft graphite is along the parallel direction setting in common graphite surface.Then under inert atmosphere, be slowly heated to 700 degree by the charing of two-layer graphite linings structure, now middle resin glue of filling is also by charing, and after charing, double-layer structure burns till one and obtains monoblock graphite block material.In sintering procedure, as flexible graphite platelet generation bubbling phenomenon, in carbonization process, pressurize.
Embodiment three
This embodiment is with the difference of embodiment two: in this embodiment, prepare the first layer graphite linings structure A by isotropy and anisotropic graphite composite powder, the first layer graphite linings structure A thickness can be obtained thicker, is 0.01～10 millimeter.In this embodiment, the thickness of the first layer graphite linings structure A is got 10 millimeters.
In this embodiment, owing to containing isotropy and anisotropic graphite composite powder in the first layer graphite linings structure A, therefore the anisotropic heat conductivity degree of graphite linings is low than the anisotropic degree of the graphite linings of being made up of anisotropy graphite composite powder merely, reduce with the difference of second layer graphite linings structure B like this, therefore can avoid equally ftractureing in graphite block materials'use process.Simultaneously because anisotropic degree decreases, therefore can relatively be prepared into thicklyer, record through test, the thicklyest approximately can reach 1 centimetre.With respect to embodiment two, applicable to the thicker use occasion of some thickness requirement.
The following is object lesson: get natural flake graphite powder (anisotropy graphite) 40%, graphous graphite powder or microlite ink powder (isotropic graphite) 30% and refinery coke 20% are mixed to get mixture (above-mentioned each percentage ratio is massfraction), as the component of the first layer graphite linings structure A; Be placed in the mould that graphite block (the second graphite linings structure B) is the end, be slowly warmed up to 500 DEG C, pressurization charing 3h, obtains two-layer graphite linings structure and burns the graphite block material being integrated.After taking out in mould, 2400 DEG C of thermal treatments.
Embodiment four
This embodiment is with the difference of embodiment one: in this embodiment, control the first layer graphite linings structure A and be made up of the different graphite linings of multi-layered anisotropic degree.Particularly, the first layer graphite linings structure A will be made after charing and greying successively after stacked Multi-layer graphite being added together according to the sequence of anisotropic degree.While setting, the graphite linings that in described the first layer graphite linings structure A, anisotropic degree is lower is contacted with described second layer graphite linings structure B.
In this embodiment, make in graphite block material, its section decomposing schematic representation as shown in Figure 4, four layers of different graphite linings A1, A2, A3 and A4 of anisotropic degree form the first layer graphite linings structure A jointly, topmost the graphite linings A1 that anisotropic degree is the highest, its performance soaking effect of heat insulation is relatively best, next be which floor relatively low graphite linings of anisotropic degree, A2, A3 and A4, it is as transition layer, the top one deck graphite linings A1 and below second layer graphite linings structure B between transferring heat.Like this, preparation multilayer, wherein the anisotropic degree of adjacent layers differs less, by reduce the amplitude that between each layer, anisotropy changes as far as possible, thereby improves the globality of the first layer graphite linings structure A, prevents cracking.Meanwhile, because of the existence of which floor transition layer of centre, make the thickness of the first layer graphite linings structure A thicker, with respect to embodiment two, require applicable to some the use occasion that heat dissipating layer thickness is thicker.And with respect to embodiment three, embodiment three is to add isotropy powder to reduce anisotropic degree in the first layer graphite linings structure A, it is the improvement that the anisotropic properties of having sacrificed the first layer graphite linings structure A exchanges thickness aspect for.And in this embodiment, do not sacrifice the anisotropic degree of the first layer graphite linings structure A, and reducing anisotropic properties if do not wanted, thickness does thicklyer again simultaneously, can use the improvement project in this embodiment.
The following is object lesson: get natural flake graphite, micro crystal graphite, refinery coke, pitch according to different ratio mixing; At 200 DEG C, stir and be kneaded into pasty state, extrude and be tabular, 5 millimeters of thicknesss of slab.Natural flake graphite content difference, the anisotropic degree of each carbon slab is different.Carbon slab is piled up successively by anisotropic degree order from low to high, be unified in hot pressing charing at 500 DEG C, unified greying, makes the first layer graphite linings structure A.Then the first layer graphite linings structure A is arranged in common graphite linings (second layer graphite linings structure B), the minimum graphite linings of anisotropic degree is in bottom, B contacts with second layer graphite linings structure, finally the charing of twenty percent graphite linings structure is burnt till to one and obtain the graphite block material of monoblock.Because anisotropic degree and the thermal conductivity of different layers are relatively slowly to change, the thermal stress distribution scope that temperature variation causes is wide, can not cause the cracking of self, can use the occasion violent in temperature variation.
Embodiment five
This embodiment is with the difference of embodiment four: in this embodiment, at least one deck in the Multi-layer graphite layer of composition the first layer graphite linings structure A, also comprise filamentary material.
In this embodiment, improvement project is the scheme based in embodiment four, is also to comprise filamentary material at least one deck in Multi-layer graphite layer.Filamentary material can be charcoal fiber, can be also organic fibre.Preferably, filamentary material is short carbon fiber, carbon fiber or macromolecular fibre.Filamentary material becomes charcoal fiber or graphite fibre in overall carbonization process, can improve the intensity of the first layer graphite linings structure A of formation, further prevents its cracking.
The following is object lesson: get natural flake graphite, micro crystal graphite, refinery coke, short carbon fiber, pitch according to different ratio mixing; At 200 DEG C, stir and be kneaded into pasty state, extrude and be tabular, 5 millimeters of thicknesss of slab.Natural flake graphite content difference, the anisotropic degree of each carbon slab is different.Carbon slab is piled up successively by anisotropic degree order from low to high, be unified in hot pressing charing at 500 DEG C, unified greying, makes the first layer graphite linings structure A.Then the first layer graphite linings structure A is arranged in common graphite linings (second layer graphite linings structure B), the minimum graphite linings of anisotropic degree is in bottom, B contacts with second layer graphite linings structure, finally the charing of twenty percent graphite linings structure is burnt till to one and obtain the graphite block material of monoblock.Owing to increasing and having this filamentary material of short carbon fiber in the raw material of preparation graphite linings, the first layer graphite linings structure A intensity of therefore making increases, and can further prevent cracking.
Embodiment six
This embodiment is with the difference of embodiment one: in this embodiment, second layer graphite linings structure is improved, by long graphite linings and short graphite linings composition second layer graphite linings structure B.
As shown in Figure 5, for the structural representation of graphite block material in this embodiment, graphite block material 100 comprises two-layer graphite linings structure, the first layer graphite linings structure A anisotropy, the first layer graphite linings structure A is arranged on described second layer graphite linings structure B, and the relatively high heat conduction direction of the first layer graphite linings structure A is the direction parallel with described second layer graphite linings structure B surface, and two-layer graphite linings structure forms an entirety after one is burnt till in charing.Wherein, second layer graphite linings structure B comprises multiple long graphite linings B1 and multiple short graphite linings B2, and long graphite linings B1 and short graphite linings B2 interval arrange, and the formation second layer graphite linings structure B that is bonded to one after end face side-by-side alignment.The first layer graphite linings structure A is arranged on the end face being formed by long graphite linings B1 and short graphite linings B2 side-by-side alignment of second layer graphite linings structure B.While preparing second layer graphite linings structure B, first prepare the long graphite linings B1 of multilayer and the short graphite linings B2 of multilayer, to grow graphite linings B1 and short graphite linings B2 interval and arrange, and after end face side-by-side alignment, each graphite linings is bonded to one and form described second layer graphite linings structure B.
The following is specific examples: by the mesophase pitch heating kneading (each percentage ratio is massfraction) of 95% natural flake graphite and 5%, be hot pressed into the thin slice of thickness 5mm; Strike out rectangular parallelepiped different in size, obtain the long graphite linings of multilayer and the short graphite linings of multilayer.Then on one side of long graphite linings and short graphite linings, it is pasted into piece with glue, long graphite linings and short graphite layers are every setting, and end face side-by-side alignment.On the end face forming in alignment again, paste anisotropic graphite flake as the first layer graphite linings structure, wait static pressure charing, obtain burning till an overall graphite block material by two-layer graphite linings structure.Normal heating to 3000 DEG C greying 2 hours again.
Graphite block material in this embodiment, for dispelling the heat with the working process of adstante febre with embodiment one, in this not repeat specification, therefore the graphite block material of this embodiment, double-layer structure arranges, can bring into play soaking and add heat radiation, or the heat insulation effect that adds heating, the performance that promotes the heat radiation of graphite block material or generate heat.Meanwhile, interface seamless link, between double-layer structure interface, thermal resistance is very little, interface heat-transfer effect is good, for dispel the heat or the improved performance of adstante febre more remarkable.In this embodiment, graphite block material is with respect to the graphite block material in embodiment one, the structure of graphite linings for the second time in this embodiment is made up of length graphite linings, feldspar China ink layer segment forms long fin, short graphite linings part forms short fin, when dispelling the heat, being provided with of long fin and short fin is beneficial to further improving radiating effect.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, make without departing from the inventive concept of the premise some substituting or obvious modification, and performance or purposes identical, all should be considered as belonging to protection scope of the present invention.
Claims (14)
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| CN105120634B (en) * | 2015-09-06 | 2017-11-14 | 张永锋 | A kind of high conduction heat radiator |
| KR102094925B1 (en) * | 2018-05-03 | 2020-03-30 | 에스케이씨 주식회사 | Multilayer graphite sheet having excellent electromagnetic shielding property and thermal conductivity, and preparation method thereof |
| CN109177368A (en) * | 2018-09-06 | 2019-01-11 | 三峡大学 | A kind of graphite film lamination composite board and preparation method thereof |
| CN114702316B (en) * | 2022-03-23 | 2023-05-30 | 湖南大学 | Preparation method and application of low-cost high-purity graphite material |
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| CN101449374A (en) * | 2006-06-08 | 2009-06-03 | 国际商业机器公司 | Highly heat conductive, flexible sheet |
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