CN110541142A - preparation method of modified graphene composite aluminum alloy - Google Patents
preparation method of modified graphene composite aluminum alloy Download PDFInfo
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- CN110541142A CN110541142A CN201910836069.0A CN201910836069A CN110541142A CN 110541142 A CN110541142 A CN 110541142A CN 201910836069 A CN201910836069 A CN 201910836069A CN 110541142 A CN110541142 A CN 110541142A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
- B21B1/24—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process
- B21B1/28—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process by cold-rolling, e.g. Steckel cold mill
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B13/00—Metal-rolling stands, i.e. an assembly composed of a stand frame, rolls, and accessories
- B21B13/02—Metal-rolling stands, i.e. an assembly composed of a stand frame, rolls, and accessories with axes of rolls arranged horizontally
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
- C23C8/44—Carburising
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B13/00—Metal-rolling stands, i.e. an assembly composed of a stand frame, rolls, and accessories
- B21B13/02—Metal-rolling stands, i.e. an assembly composed of a stand frame, rolls, and accessories with axes of rolls arranged horizontally
- B21B2013/021—Twin mills
Abstract
The invention discloses a preparation method of a modified graphene composite aluminum alloy, which comprises the following steps: 1) preparing a graphene additive solution: uniformly mixing 2-5 parts of nano-graphene and 80-100 parts of N-methyl-2-pyrrolidone in parts by weight, dispersing by a dispersion machine to form graphene dispersion liquid, and mixing with 400 parts of 300-fold ion water to prepare a graphene addition liquid; 2) and (3) rolling of the aluminum strip: carrying out n-pass rolling on the aluminum strip with the thickness of 4-8mm by an aluminum strip cold rolling machine until the thickness is 1-2 mm; in the process, adding graphene addition liquid on the mth rolling wheel of the first pass … … and the second pass … … respectively, wherein n is a positive integer greater than 3, n is a positive integer greater than 2, and m is less than or equal to n; in the calendering process, the aluminum strip heats, a thermal expansion effect is formed on the surface of the aluminum strip, pores are generated, the graphene additive solution permeates into the pores, and after the graphene is calendered and permeated in the previous m passes, energy spectrum analysis is performed to ensure that the graphene accounts for 10% -40% of the surface components of the aluminum strip.
Description
Technical Field
The invention relates to preparation of aluminum alloy, in particular to a preparation method of a modified graphene composite aluminum alloy.
Background
Graphene (Graphene) is a two-dimensional carbon nanomaterial composed of carbon atoms in sp hybridized orbitals into a hexagonal honeycomb lattice. The graphene has excellent optical, electrical and mechanical properties, and has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like. However, graphene is rarely applied to modification of aluminum bar products at present, and even if graphene is used, the modification process is generally the overall performance modification performed during aluminum alloy material smelting, the process is complex, the cost is high, and the modification effect is poor. Therefore, the existing preparation method of the graphene composite aluminum alloy has many unreasonable places, and needs to be improved and perfected.
disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a preparation method of a modified graphene composite aluminum alloy, which can perform graphene composite modification on the surface of an aluminum alloy in the subsequent aluminum strip calendering process, and has the advantages of scientific, reasonable, simple and feasible process flow, convenience for industrialization, low process cost, good modification effect and high cost performance.
the technical scheme adopted by the invention is as follows: the preparation method of the modified graphene composite aluminum alloy is characterized by comprising the following steps:
1) Preparing a graphene additive solution: uniformly mixing 2-5 parts of nano-graphene and 80-100 parts of N-methyl-2-pyrrolidone in parts by weight, dispersing by a dispersion machine to form graphene dispersion liquid, and mixing with 400 parts of 300-fold ion water to prepare a graphene addition liquid;
2) and (3) rolling of the aluminum strip: carrying out n-pass rolling on the aluminum strip with the thickness of 4-8mm by an aluminum strip cold rolling machine until the thickness is 1-2 mm; in the process, adding graphene addition liquid on the mth rolling wheel of the first pass … … and the second pass … … respectively, wherein n is a positive integer greater than 3, n is a positive integer greater than 2, and m is less than or equal to n; in the calendering process, the aluminum strip heats, a thermal expansion effect is formed on the surface of the aluminum strip, pores are generated, the graphene additive solution permeates into the pores, and after the graphene is calendered and permeated in the previous m passes, energy spectrum analysis is performed to ensure that the graphene accounts for 10% -40% of the surface components of the aluminum strip.
further, the step 1) also comprises the following steps: and adjusting the pH value of the graphene additive solution to 7-9 by adding liquid alkali, sodium hydroxide or potassium hydroxide.
Further, in the step 2), each rolling of the aluminum strip cold rolling machine comprises an upper rolling wheel and a lower rolling wheel which are arranged in a matched manner, the upper rolling wheel and the lower rolling wheel are provided with rolling grooves, the rolling grooves of the upper rolling wheel and the lower rolling wheel are matched to form a rolling hole, the thickness of the rolling hole is gradually reduced along with each rolling, and specifically, the thickness of each rolling hole is 0.1-0.5 mm.
Further, in the step 2), the front m paths of rolling of the aluminum strip cold rolling machine are provided with a graphene additive liquid feeding device corresponding to the rolling path of the upper rolling wheel.
Further, the graphene additive liquid feeding device comprises a liquid feeding wheel and a liquid feeding funnel assembly, wherein the liquid feeding wheel is matched with the upper binding wheel.
further, in step 2), the aluminum strip is extruded and then stretch-formed through aluminum, and is degreased and oxidized film is removed through a cleaning tank.
The invention has the following advantages: the special graphene additive solution with extremely strong surface binding property is prepared, capillary pores generated by high-temperature thermal expansion in the aluminum strip calendering process are matched, and the graphene additive solution is combined in a penetration manner, so that the graphene composite modification can be carried out on the surface of the aluminum alloy in the subsequent aluminum strip calendering and forming process, the process flow is scientific, reasonable, concise and feasible, the industrialization is facilitated, the process cost is low, the modification effect is good, and the cost performance is extremely high.
The present invention will be further described with reference to the following description and embodiments in conjunction with the accompanying drawings.
drawings
FIG. 1 is a first schematic structural diagram of an aluminum strip cold rolling machine;
FIG. 2 is a second schematic structural view of an aluminum strip cold rolling machine;
FIG. 3 is a graph of energy spectrum analysis according to the first embodiment;
FIG. 4 is a graph of energy spectrum analysis of the second embodiment;
FIG. 5 is a graph of energy spectrum analysis of an unmodified conventional aluminum strip;
in the figure: a binding wheel 1 is arranged; and a rolling wheel 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that if directional indications (such as … …, which is up, down, left, right, front, back, top, bottom, inner, outer, vertical, transverse, longitudinal, counterclockwise, clockwise, circumferential, radial, axial) are provided in the embodiments of the present invention, the directional indications are only used for explaining the relative position relationship, motion condition, etc. of the components at a specific posture (as shown in the attached drawings), and if the specific posture is changed, the directional indications are changed accordingly.
In addition, if there is a description relating to "first" or "second", etc. in the embodiments of the present invention, the description of "first" or "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Example one
referring to fig. 1 to 3, the preparation method of the modified graphene composite aluminum alloy provided in this embodiment includes the following steps:
1) Preparing a graphene additive solution: uniformly mixing 2 parts of nano-graphene and 80 parts of N-methyl-2-pyrrolidone in parts by weight, dispersing by using a dispersion machine to form graphene dispersion liquid, mixing with 300 parts of deionized water, and adding liquid alkali, sodium hydroxide or potassium hydroxide to adjust the pH value to 7 to prepare a graphene addition liquid;
2) And (3) rolling of the aluminum strip: performing 10-pass rolling on the aluminum strip with the thickness of 4mm by an aluminum strip cold rolling machine until the thickness is 1 mm; in the process, adding graphene addition liquid on the binding grooves of the first binding wheel, the second binding wheel and the third binding wheel respectively; in the calendering process, the aluminum strip heats, a thermal expansion effect is formed on the surface of the aluminum strip, pores are generated, the graphene additive solution permeates into the pores, the graphene is calendered and permeated in the first three passes, then the graphene is calendered in the last seven passes, and energy spectrum analysis is performed, so that the graphene is guaranteed to account for 10% -40% of the surface components of the aluminum strip. Specifically, the aluminum strip is extruded and then stretch-formed through aluminum, and is degreased and an oxide film is removed through a cleaning tank. Specifically, each rolling of the aluminum strip cold rolling machine comprises an upper rolling wheel 1 and a lower rolling wheel 2 which are arranged in a matched mode, the upper rolling wheel 1 and the lower rolling wheel 2 are provided with rolling grooves, the rolling grooves of the upper rolling wheel and the lower rolling wheel are matched to form a rolling hole, the thickness of the rolling hole is gradually reduced along with each rolling, and specifically, the thickness of each rolling hole is 0.1-0.5 mm. It should be noted that, all the existing roller type aluminum strip cold rolling machines are applicable, and only the graphene additive solution needs to be added to the corresponding rollers. More specifically, a graphene additive liquid feeding device is arranged on the binding channel corresponding to the upper binding wheel. The graphene additive liquid feeding device comprises a liquid feeding wheel and a liquid feeding funnel assembly, wherein the liquid feeding wheel is matched with an upper binding wheel.
it should be noted that the graphene additive solution is selectively infiltrated in the first few rolling passes, so that the subsequent rolling passes play a role in strengthening, and the stability of graphene on the surface of the aluminum strip is ensured. Of course, several rolling passes are selected in the middle or the later passes or at intervals to permeate the graphene additive solution, which can be used as an equivalent technical means and can also play a role in graphene composite modification, but the effect is far less than that of the previous rolling passes to permeate the graphene additive solution.
example two
Referring to fig. 4, the present embodiment is substantially the same as the first embodiment, except that: the preparation method of the modified graphene composite aluminum alloy comprises the following steps:
1) Preparing a graphene additive solution: uniformly mixing 5 parts of nano-graphene and 100 parts of N-methyl-2-pyrrolidone in parts by weight, dispersing by using a dispersion machine to form graphene dispersion liquid, mixing with 400 parts of deionized water, and adding liquid alkali, sodium hydroxide or potassium hydroxide to adjust the pH value to 9 to prepare a graphene addition liquid;
2) and (3) rolling of the aluminum strip: performing 20-pass rolling on the aluminum strip with the thickness of 8mm by an aluminum strip cold rolling machine until the thickness is 2 mm; in the process, adding graphene addition liquid on the binding grooves of the first binding wheel, the second binding wheel and the third binding wheel respectively; in the calendering process, the aluminum strip heats, a thermal expansion effect is formed on the surface of the aluminum strip, pores are generated, the graphene additive solution permeates into the pores, the graphene is calendered and permeated in the first three passes, then the graphene is calendered in the last seven passes, and energy spectrum analysis is performed, so that the graphene is guaranteed to account for 10% -40% of the surface components of the aluminum strip.
EXAMPLE III
The present embodiment is substantially the same as the first embodiment, except that: the preparation method of the modified graphene composite aluminum alloy comprises the following steps:
1) Preparing a graphene additive solution: uniformly mixing 3 parts of nano-graphene and 90 parts of N-methyl-2-pyrrolidone in parts by weight, dispersing by using a dispersion machine to form graphene dispersion liquid, mixing with 350 parts of deionized water, and adding liquid alkali, sodium hydroxide or potassium hydroxide to adjust the pH value to 8 to prepare graphene addition liquid;
2) And (3) rolling of the aluminum strip: performing 12-pass rolling on the aluminum strip with the thickness of 6mm by using an aluminum strip cold rolling machine until the thickness is 1.5 mm; in the process, adding graphene addition liquid on the binding grooves of the first binding wheel, the second binding wheel and the third binding wheel respectively; in the calendering process, the aluminum strip heats, a thermal expansion effect is formed on the surface of the aluminum strip, pores are generated, the graphene additive solution permeates into the pores, the graphene is calendered and permeated in the first three passes, then the graphene is calendered in the last seven passes, and energy spectrum analysis is performed, so that the graphene is guaranteed to account for 10% -40% of the surface components of the aluminum strip.
The surface of the modified graphene composite aluminum alloy strip obtained in the first and second embodiments is subjected to energy spectrum analysis and testing, and the component analysis is performed by utilizing different X-ray photon characteristic energies of different elements, so that the surface coating, the coating and the composite layer of the solid material can be analyzed. Wherein, the test content comprises: and (3) analyzing the components of the aluminum graphene composite material, and analyzing and observing the components of the surface material of the modified graphene composite aluminum alloy strip through EDS.
The detection method and the process are as follows:
1. Analytical test equipment and instrumentation: analytical testing EDS analysis was performed using a QUANTA200 model scanning electron microscope.
2. The testing process flow comprises the following steps: before EDS composition analysis, the sample is visually polished, immersed in acetone solution for ultrasonic vibration to remove oil, and then subjected to composition analysis.
3. Analyzing and detecting results: compared with an unmodified aluminum strip (shown in figure 5), the proportion of the graphene in the surface composition of the aluminum strip in the first embodiment and the second embodiment is obviously increased, and the proportions are as follows: 25.74 percent and 25.11 percent. The comprehensive properties of the alloy, such as conductivity, hardness, heat dispersion, bending rate, toughness, oxidation resistance and the like, are obviously optimized and improved.
The present invention is not limited to the above embodiments, and the preparation method of another modified graphene composite aluminum alloy obtained by using the same or similar technical features as those of the above embodiments of the present invention is within the protection scope of the present invention.
Claims (6)
1. The preparation method of the modified graphene composite aluminum alloy is characterized by comprising the following steps:
1) Preparing a graphene additive solution: uniformly mixing 2-5 parts of nano-graphene and 80-100 parts of N-methyl-2-pyrrolidone in parts by weight, dispersing by a dispersion machine to form graphene dispersion liquid, and mixing with 400 parts of 300-fold ion water to prepare a graphene addition liquid;
2) And (3) rolling of the aluminum strip: carrying out n-pass rolling on the aluminum strip with the thickness of 4-8mm by an aluminum strip cold rolling machine until the thickness is 1-2 mm; in the process, adding graphene addition liquid on the mth rolling wheel of the first pass … … and the second pass … … respectively, wherein n is a positive integer greater than 3, n is a positive integer greater than 2, and m is less than or equal to n; in the calendering process, the aluminum strip heats, a thermal expansion effect is formed on the surface of the aluminum strip, pores are generated, the graphene additive solution permeates into the pores, and after the graphene is calendered and permeated in the previous m passes, energy spectrum analysis is performed to ensure that the graphene accounts for 10% -40% of the surface components of the aluminum strip.
2. The method for preparing the modified graphene composite aluminum alloy according to claim 1, wherein the step 1) further comprises the following steps: and adjusting the pH value of the graphene additive solution to 7-9 by adding liquid alkali, sodium hydroxide or potassium hydroxide.
3. The method for preparing the modified graphene composite aluminum alloy according to claim 1, wherein in the step 2), each rolling of the aluminum strip cold rolling machine includes an upper rolling wheel and a lower rolling wheel which are arranged in a matching manner, the upper rolling wheel and the lower rolling wheel are provided with rolling grooves, the rolling grooves of the upper rolling wheel and the lower rolling wheel are matched to form a rolling hole, and the thickness of the rolling hole is gradually reduced along with each rolling, specifically, the thickness of each rolling hole is 0.1-0.5 mm.
4. The preparation method of the modified graphene composite aluminum alloy according to claim 3, wherein in the step 2), the front m lines of the aluminum strip cold rolling machine are rolled, and a graphene additive liquid feeding device is arranged corresponding to the rolling line of the upper rolling wheel.
5. the preparation method of the modified graphene composite aluminum alloy according to claim 3, wherein the graphene additive solution feeding device comprises a solution feeding wheel and a solution feeding funnel assembly, wherein the solution feeding wheel is matched with the rolling wheel.
6. The method for preparing the modified graphene composite aluminum alloy according to claim 1, wherein in the step 2), the aluminum strip is formed by aluminum extrusion and then stretching, and is subjected to oil removal and oxide film removal through a cleaning tank.
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Citations (6)
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| CN102962418A (en) * | 2012-12-11 | 2013-03-13 | 武汉钢铁(集团)公司 | Cast-rolling compound production method and device for thin high-silicon steel band |
| CN105845942A (en) * | 2016-06-20 | 2016-08-10 | 山东建筑大学 | Preparation method of nano graphene copper foil |
| CN106163227A (en) * | 2015-05-13 | 2016-11-23 | 蔡承恩 | Heat radiation lamination structure and manufacture method thereof |
| WO2018080475A1 (en) * | 2016-10-26 | 2018-05-03 | Hewlett-Packard Development Company, L.P. | Substrates with patterned surfaces |
| CN109628789A (en) * | 2019-01-31 | 2019-04-16 | 中国科学院过程工程研究所 | Graphene Al-alloy, wire rod, preparation method and the purposes prepared by it |
| CN110125181A (en) * | 2018-02-09 | 2019-08-16 | 常州第六元素材料科技股份有限公司 | Roll-bonding prepares the method and its alkene alloy of alkene alloy |
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2019
- 2019-09-05 CN CN201910836069.0A patent/CN110541142B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102962418A (en) * | 2012-12-11 | 2013-03-13 | 武汉钢铁(集团)公司 | Cast-rolling compound production method and device for thin high-silicon steel band |
| CN106163227A (en) * | 2015-05-13 | 2016-11-23 | 蔡承恩 | Heat radiation lamination structure and manufacture method thereof |
| CN105845942A (en) * | 2016-06-20 | 2016-08-10 | 山东建筑大学 | Preparation method of nano graphene copper foil |
| WO2018080475A1 (en) * | 2016-10-26 | 2018-05-03 | Hewlett-Packard Development Company, L.P. | Substrates with patterned surfaces |
| CN110125181A (en) * | 2018-02-09 | 2019-08-16 | 常州第六元素材料科技股份有限公司 | Roll-bonding prepares the method and its alkene alloy of alkene alloy |
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