CN104846230A - Preparation method of aluminum-base graphene composite material - Google Patents
Preparation method of aluminum-base graphene composite material Download PDFInfo
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- CN104846230A CN104846230A CN201510279542.1A CN201510279542A CN104846230A CN 104846230 A CN104846230 A CN 104846230A CN 201510279542 A CN201510279542 A CN 201510279542A CN 104846230 A CN104846230 A CN 104846230A
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Abstract
The invention discloses a preparation method of an aluminum-base graphene composite material, which comprises the following steps: 1) dispersing graphene in an organic solvent to form a graphene dispersion solution, wherein the organic solvent can not chemically react with aluminum; 2) acidizing interlocking pore foamed aluminum to remove the surface oxidizing layer, and drying; 3) immersing the interlocking pore foamed aluminum treated by the step 2) in the graphene dispersion solution, taking out, and drying to obtain the graphene/foamed aluminum composite; and 4) preheating the graphene/foamed aluminum composite, and rolling to finally obtain the aluminum-base graphene composite material, wherein the step 1) and step 2) can be exchanged, and the mass of the graphene and interlocking pore foamed aluminum is 0.1-10 wt%. The method prevents the high-energy ball mill from damaging graphene in the traditional powder metallurgical technique, can implement effective dispersion by using the foamed aluminum as the framework, is simple in technique, and has obvious industrialized application prospects.
Description
Technical field
The present invention relates to a kind of preparation technology of matrix material, be related specifically to a kind of preparation method of aluminium base graphene composite material.
Background technology
Aluminium carbon composite has the characteristics such as low density, high heat conduction and thermal expansivity can design, there is processing and welding advantage of metal simultaneously, be Electronic Packaging and the thermal management materials of a new generation, in electronic apparatus, aerospace, dynamoelectric equipment field, there is major application prospect.Conventional aluminium carbon composite adopts natural graphite to be main heat conduction modified filler, because yardstick easily causes matrix material uneven comparatively greatly.And natural graphite is subject to the restriction of degree of crystallization and impurity level, seems more and more difficult to the further lifting of thermal conductivity.Therefore, development of new heat conductive filler, prepares high-performance aluminum carbon composite now particularly important.Graphene is a kind of one dimension carbon material of perfect sp2 hydridization, and Theoretical Calculation shows its thermal conductivity with superelevation (5000-6000W/m.K) and mechanical property, enters brand-new visual angle for leading new material development.
Although theoretical investigation shows that Graphene has excellent thermal property, the complicacy of technique and the surface reaction of matrix material hinder the suitability for industrialized production of graphene/aluminum matrix material.The patent of the retrieval through to existing patent: CN102329976A is by the pre-ball milling to aluminium powder, cold pressing after joining filtration in the solution of Graphene, oven dry, finally also need at high temperature heat extrusion forming, this complex process, in addition, due to needs at high temperature heat extrusion forming, increase surface reaction, thus the composite property prepared does not give full play to the performance of Graphene, and the thermal conductivity of matrix material only has 145W/m.K.So far, still there is larger challenge in the preparation of high thermal conductance aluminum matrix composite.
Summary of the invention
The invention provides a kind of preparation method of aluminium base graphene composite material, process avoids prior powder metallurgy technique high-energy ball milling to the destruction of Graphene, be that skeleton can realize it and effectively disperses with foamed aluminium, on the basis realizing raising matrix material high heat conductance performance and low thermal coefficient of expansion, the production of aluminium carbon high-heat-conductive composite material is simplified more.
In order to realize foregoing invention object, present invention employs following technical scheme: a kind of preparation method of aluminium base graphene composite material, specifically comprises the steps:
1) form graphene dispersing solution by graphene dispersion to organic solvent, described organic solvent is the organic solvent that chemical reaction does not occur with aluminium;
2) communicating aperture foamed aluminium acidification is removed the zone of oxidation post-drying on surface;
3) by through step 2) handled by communicating aperture foamed aluminium be placed in graphene dispersing solution and soak, then take out, after oven dry, obtain Graphene/foamed aluminium complex body;
4) by Graphene/foamed aluminium complex body preheating, then through the final matrix material of the shaping acquisition of mill milling.
Wherein, step 1) and step 2) in no particular order sequentially, the mass ratio of Graphene and communicating aperture foamed aluminium is 0.1wt%-10wt%.
Graphene content in graphene dispersing solution is 0.1mg/ml-3mg/ml.
Do not occurring in the organic solvent of chemical reaction with aluminium, described organic solvent is preferably from the combination of a kind of of ethanol, ethylene glycol, glycerol, Virahol, butanols, acetone, butanone, hexanaphthene, heptane, ethyl acetate, toluene, dimethylbenzene, N methyl-2-pyrrolidone etc. or two or more arbitrary proportion.
In order to graphite evenly dispersion in organic solvent, step 1) by graphene dispersion to when organic solvent, first by Graphene and dispersant, this dispersion agent is selected from the combination of a kind of or two or more arbitrary proportion in Mierocrystalline cellulose, methylcellulose gum, Walocel MT 20.000PV, polyacrylic acid, Polyvinylpyrolidone (PVP), polysorbate, polyoxyethylene glycol, polypropylene glycol, alkylol amide, and described dispersion agent add-on is the 0.1-1wt% of organic solvent; Described dispersing technology adopts the one of the dispersing technologies such as ball milling, ultrasonic, grinding, high speed shear.
The diameter of described Graphene is 200 nanometer-20 microns.
Step 2) described in acidification in acid used be selected from any one of hydrochloric acid, acetic acid, nitric acid, sulfuric acid, phosphoric acid etc., the concentration of acid is 0.1wt%-10wt%;
Step 3) in soak time be 0.5-4 hour, bake out temperature is 100-200 degree.
Described drying course carries out under vacuum, vacuum tightness 0.01mbar-0.1bar, or carry out under protection of inert gas condition, rare gas element is selected from the one in nitrogen, argon gas, in order to prevent the oxidation of at high temperature foamed aluminium.
Step 4) preheating temperature of Graphene/foamed aluminium complex body is 250-600 degree, warm up time is 2 hours, and rolling pressure is 100MPa-700MPa.
The present invention compares to prior art and has outstanding beneficial effect, is simply described below:
1) utilize organic solvent and dispersion agent that Graphene can be made to be uniformly dispersed in the solution, be conducive to being uniformly distributed in foamed aluminium.
2) communicating aperture foamed aluminium is selected, graphene solution can well enter in foamed aluminium communicating aperture, thus make Graphene be dispersed in foamed aluminium according to the communicating aperture path of foamed aluminium, because foamed aluminium communicating aperture is more even, thus Graphene is well-proportioned is dispersed in foamed aluminium, by other technique before comparing in addition, as ball milling mixing, by Graphene and metal mixed, technique is simplified more.
3) process avoids prior powder metallurgy technique high-energy ball milling to the destruction of Graphene, remain the performance of original Graphene, in addition, because high-temperature time stops short in the operation of rolling, decrease the deleterious interfacial reaction of Graphene and foamed aluminium, be ensure that the densification of material by the process of rolling simultaneously, realize the regulation and control to its weave construction and interfacial characteristics, the performance of the matrix material finally prepared is guaranteed, the thermal conductivity of the aluminium carbon composite of gained is not less than 180W/m.K, and thermal expansivity is not more than 15 × 10
-6m/K.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of preparation technology of the present invention;
Embodiment
Following examples are further described technical scheme of the present invention.
Embodiment 1
A preparation method for aluminium base graphene composite material, specifically comprises the following steps
1) by the Graphene of 0.1g, (diameter of Graphene is 10um, thered is provided by Chengdu is organic) and 0.4g dispersion agent Mierocrystalline cellulose mixing, then be added in 100ml ethanol, utilize ultrasonic disperse 1 hour, form graphene dispersing solution (Graphene is 1mg/ml in graphene dispersion liquid hold-up).
2) 4g communicating aperture foamed aluminium is placed in the dilute hydrochloric acid of 5wt% after cleaning removal zone of oxidation, oven dry.
3) by through step 2) handled by communicating aperture foamed aluminium be immersed in graphene dispersing solution, soak 2 hours, take out, dry in vacuum drying oven and obtain Graphene/foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
4) Graphene of oven dry/foamed aluminium complex body is placed in electric furnace is preheated to 300 degree, under rolling pressure is 300MPa, carry out continuous hot rolling repeatedly and obtain aluminium base graphene composite material, the aluminium base graphene composite material thermal conductivity of gained can reach 340W/m.K, and thermal expansivity is 8 × 10
-6m/K.
The difference of embodiment 2 the present embodiment and embodiment 1 is, step 1) in the Graphene that adds be 0.01g (Graphene content in graphene dispersing solution is 0.1mg/ml), the thermal conductivity of the aluminium base graphene composite material of gained is 180W/m.K, and thermal expansivity is 15 × 10
-6m/K.
The difference of embodiment 3 the present embodiment and embodiment 1 is, step 1) Graphene that adds is 0.2g (Graphene content in graphene dispersing solution is 2mg/ml), the thermal conductivity of the aluminium base graphene composite material of gained reaches 375W/m.K, and thermal expansivity is only 6 × 10
-6m/K.
The difference of embodiment 4 the present embodiment and embodiment 1 is, step 1) in the Graphene that adds be 0.3g (Graphene content in graphene dispersing solution is 3mg/ml), the thermal conductivity of the aluminium base graphene composite material of gained is 420W/m.K, and thermal expansivity is 4 × 10
-6m/K.
The difference of embodiment 5 the present embodiment and embodiment 1 is, step 1) do not add dispersion agent, the thermal conductivity of the aluminium base graphene composite material of gained is 190W/m.K, and thermal expansivity is 15 × 10
-6m/K.
The difference of embodiment 6 the present embodiment and embodiment 1 is, step 1) to add dispersion agent polyoxyethylene glycol be 0.78g, the thermal conductivity of the aluminium base graphene composite material of gained is 340W/m.K, and thermal expansivity is 8 × 10
-6m/K.
The difference of embodiment 7 the present embodiment and embodiment 1 is, step 2) 100g foamed aluminium is placed in the dilute sulphuric acid of 10wt% and carries out cleaning removal zone of oxidation, dry, the thermal conductivity of the aluminium base graphene composite material of gained is 190W/m.K, and thermal expansivity is 15 × 10
-6m/K.
The difference of embodiment 8 the present embodiment and embodiment 1 is, step 2) foamed aluminium of 1g is placed in the dilute acetic acid of 0.001wt% and carries out cleaning removal zone of oxidation, dry, the thermal conductivity of the aluminium base graphene composite material of gained is 345W/m.K, and thermal expansivity is 8 × 10
-6m/K.
The difference of embodiment 9 the present embodiment and embodiment 1 is, step 3) foamed aluminium is 0.5 hour in Graphene soak time, the thermal conductivity of the aluminium base graphene composite material of gained is 300W/m.K, and thermal expansivity is 10 × 10
-6m/K.
The difference of embodiment 10 the present embodiment and embodiment 1 is, step 3) foamed aluminium is 4 hours in Graphene soak time, the thermal conductivity of the aluminium base graphene composite material of gained is 345W/m.K, and thermal expansivity is 8 × 10
-6m/K.
The difference of embodiment 11 the present embodiment and embodiment 1 is, step 4) in preheating temperature be 200 degree, the thermal conductivity of the aluminium base graphene composite material of gained is 300W/m.K, and thermal expansivity is 9 × 10
-6m/K.
The difference of embodiment 12 the present embodiment and embodiment 1 is, step 4) in preheating temperature be 450 degree, the thermal conductivity of the aluminium base graphene composite material of gained is 350W/m.K, and thermal expansivity is 7 × 10
-6m/K.
The difference of embodiment 13 the present embodiment and embodiment 1 is, step 4) in mill rolling force be 100MPa, the thermal conductivity of the aluminium base graphene composite material of gained is 250W/m.K, and thermal expansivity is 10 × 10
-6m/K.
The difference of embodiment 14 the present embodiment and embodiment 1 is, step 4) in mill rolling force be 700MPa, the thermal conductivity of the aluminium base graphene composite material of gained is 360W/m.K, and thermal expansivity is 7 × 10
-6m/K.
More than illustrate and above embodiment, the design philosophy surely of the present invention that is limited can not be resolved.Hold in technical field of the present invention identical know the knowledgeable can by technical thought of the present invention with various form improvement change, such improvement and change are interpreted as belonging in protection scope of the present invention.
Claims (9)
1. a preparation method for aluminium base graphene composite material, is characterized in that, specifically comprises the steps:
1) form graphene dispersing solution by graphene dispersion to organic solvent, described organic solvent is the organic solvent that chemical reaction does not occur with aluminium;
2) communicating aperture foamed aluminium acidification is removed the zone of oxidation post-drying on surface;
3) by through step 2) handled by communicating aperture foamed aluminium be placed in graphene dispersing solution and soak, then take out, after oven dry, obtain Graphene/foamed aluminium complex body;
4) by Graphene/foamed aluminium complex body preheating, then through the final matrix material of the shaping acquisition of mill milling.
Wherein, step 1) and step 2) in no particular order sequentially, the mass ratio 0.1wt%-10wt% of Graphene and communicating aperture foamed aluminium.
2. the preparation method of a kind of aluminium base graphene composite material according to claim 1, is characterized in that, described Graphene content in graphene dispersing solution is 0.1mg/ml-3mg/ml.
3. the preparation method of a kind of aluminium base graphene composite material according to claim 1, is characterized in that: described organic solvent is selected from the combination of a kind of of ethanol, ethylene glycol, glycerol, Virahol, butanols, acetone, butanone, hexanaphthene, heptane, ethyl acetate, toluene, dimethylbenzene, N methyl-2-pyrrolidone etc. or two or more arbitrary proportion.
4. the preparation method of a kind of aluminium base graphene composite material according to claim 1, it is characterized in that, by graphene dispersion to organic solvent time, first by Graphene and dispersant, this dispersion agent is selected from the combination of a kind of or two or more arbitrary proportion in Mierocrystalline cellulose, methylcellulose gum, Walocel MT 20.000PV, polyacrylic acid, Polyvinylpyrolidone (PVP), polysorbate, polyoxyethylene glycol, polypropylene glycol, alkylol amide, and described dispersion agent add-on is the 0.1-1wt% of organic solvent.
5. the preparation method of a kind of aluminium base graphene composite material according to claim 1, is characterized in that, the diameter of described Graphene is 200 nanometer-20 microns.
6. the preparation method of a kind of aluminium base graphene composite material according to claim 1, it is characterized in that, step 2) described in acidification acid used be selected from any one of hydrochloric acid, acetic acid, nitric acid, sulfuric acid, phosphoric acid etc., the concentration of acid is 0.001-10wt%.
7. the preparation method of a kind of aluminium base graphene composite material according to claim 1, is characterized in that, step 3) soak time is 0.5-4 hour, bake out temperature is 100-200 degree.
8. the preparation method of a kind of aluminium base graphene composite material according to claim 1; it is characterized in that; described drying course carries out under vacuum; vacuum tightness 0.01mbar-0.1bar; or carry out under protection of inert gas condition, rare gas element is selected from the one in nitrogen, argon gas.
9. the preparation method of a kind of aluminium base graphene composite material according to claim 1, it is characterized in that, step 4) preheating temperature of Graphene/foamed aluminium complex body is 250-600 degree, warm up time is 0.5-3 hour, and rolling pressure is 100MPa-700MPa.
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| CN105088111A (en) * | 2015-09-21 | 2015-11-25 | 国家电网公司 | Preparation method of carbon nanotube reinforced aluminum matrix composite |
| CN105349846A (en) * | 2015-11-02 | 2016-02-24 | 唐山建华科技发展有限责任公司 | Preparation method of graphene/aluminum composite material |
| CN105671387A (en) * | 2016-02-19 | 2016-06-15 | 广州市雷子克电气机械有限公司 | Aluminum-based compound material and preparation method thereof |
| CN105936992A (en) * | 2016-07-13 | 2016-09-14 | 蚌埠市时代电子有限公司 | Carbon monofluoride enhanced aluminum magnesium alloy material for automobile electronic packaging and preparing method thereof |
| CN105936988A (en) * | 2016-07-13 | 2016-09-14 | 安徽祈艾特电子科技股份有限公司 | Graphene enhanced aluminum magnesium alloy material for automobile electronic packaging and preparing method thereof |
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| CN111101112A (en) * | 2019-12-31 | 2020-05-05 | 新疆烯金石墨烯科技有限公司 | Graphene-aluminum composite material and preparation method thereof |
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| CN114069096A (en) * | 2021-11-12 | 2022-02-18 | 天津市捷威动力工业有限公司 | Composite film capable of regulating and controlling heat conduction and lithium ion battery |
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| US11878341B2 (en) | 2022-05-25 | 2024-01-23 | Wuhan Research Institute Of Materials Protection | Method for preparing aluminum carbon composite by using foam aluminum |
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