CN113151708B - Preparation method of high-conductivity graphene composite aluminum alloy for cable - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 51
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 66
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 62
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 46
- 239000007789 gas Substances 0.000 claims abstract description 38
- 238000000498 ball milling Methods 0.000 claims abstract description 37
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 33
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 33
- 239000011812 mixed powder Substances 0.000 claims abstract description 32
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 27
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 238000003801 milling Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 239000013598 vector Substances 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 230000002035 prolonged effect Effects 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 238000005273 aeration Methods 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 238000009749 continuous casting Methods 0.000 description 11
- 238000005096 rolling process Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/023—Alloys based on aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses a preparation method of a high-conductivity graphene composite aluminum alloy for cables, and belongs to the technical field of new materials. The preparation method comprises the following steps: s11, taking graphene and atomized aluminum powder, and performing ball milling by using a ball mill, wherein liquid nitrogen is used for immersing the milling balls during ball milling; s12, vacuum drying the mixed powder obtained in S11; s13, melting aluminum material under the condition of introducing mixed gas of nitrogen and carbon dioxide; s14, adding the dried mixed powder obtained in the step S12 into the molten aluminum obtained in the step S13, and mixing; s15, continuously introducing mixed gas of nitrogen and carbon dioxide; and S16, preparing an aluminum alloy ingot. According to the preparation method of the high-conductivity graphene composite aluminum alloy for the cable, the mixed powder which is suitable for being mixed with molten aluminum is obtained through ball milling of graphene and atomized aluminum powder; the graphene and the molten aluminum are mixed under the condition of introducing mixed gas of nitrogen and carbon dioxide, so that the strength and the conductivity of the obtained alloy composite material can be obviously improved.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a preparation method of a high-conductivity graphene composite aluminum alloy for cables.
Background
Graphene is widely introduced in the preparation of metal composite materials due to its mechanical properties, thermal conductivity and thermal expansion properties.
Aluminum alloys are common cable materials. In the preparation of graphene-aluminum alloy composite materials, the mixing process of graphene and molten aluminum metal is a key step, and important performance parameters such as strength and conductivity of the obtained composite materials are influenced.
Disclosure of Invention
In the research of the researchers of the invention, it is found that in the preparation method of the highly conductive graphene composite aluminum alloy for the cable, in the mixing process of the graphene and the molten aluminum metal, the strength and the conductivity of the obtained composite material are significantly influenced by parameters such as the particle state of the graphene material in the mixing process and the mixing conditions. The present invention is based on this finding.
The invention discloses a preparation method of a high-conductivity graphene composite aluminum alloy for cables, which comprises the following steps:
s11, taking graphene and atomized aluminum powder, and performing ball milling by using a ball mill, wherein liquid nitrogen is used for immersing the milling balls during ball milling;
s12, vacuum drying the mixed powder obtained in S11;
s13, melting aluminum material under the condition of introducing mixed gas of nitrogen and carbon dioxide;
s14, adding the dried mixed powder obtained in the step S12 into the molten aluminum obtained in the step S13, and mixing;
s15, continuously introducing mixed gas of nitrogen and carbon dioxide;
and S16, preparing an aluminum alloy ingot.
In some embodiments of the invention, in S11, the weight ratio of the graphene to the atomized aluminum powder is (1-3): (97-99).
In some embodiments of the invention, in S14, the weight ratio of the dry mixed powder to the molten aluminum is (90-110): (90-110).
In some embodiments of the invention, in S11, when the ball milling is performed by using the ball mill, the weight ratio of the milling balls to the material is (10-15):1, the rotation speed of the ball mill is 30-50rpm, and the ball milling is performed for 8-15 h.
In some embodiments of the invention, in S12, the temperature of vacuum drying is 80-90 ℃ for 1-2 h.
In some embodiments of the present invention, in S13, the volume ratio of nitrogen to carbon dioxide in the mixed gas is 1: (1-5), the flow rate of the mixed gas is (35-45)m 3/h。
In some preferred embodiments of the present invention, in S13, the volume ratio of nitrogen to carbon dioxide in the mixed gas is 1: (2-4), wherein the flow rate of the mixed gas is (35-45) m3/h。
In some further preferred embodiments of the present invention, in S13, the volume ratio of nitrogen to carbon dioxide in the mixed gas is 1:3, the flow rate of the mixed gas is 40m3/h。
In some embodiments of the invention, aeration is continued for 20-40min at S15.
In some embodiments of the invention, the nitrogen and carbon dioxide mixed gas is released into the molten aluminum through a serpentine tube provided at the bottom. The mixed gas released from the uniformly distributed exhaust ports of the coiled pipe can create an atmosphere environment, and can also drive nearby aluminum metal liquid to flow during bubbling, so that the graphene is favorably mixed with molten aluminum after being added.
In some embodiments of the present invention, the step of S11 further includes the step of determining the weight ratio of the grinding balls to the material:
s21, setting the weight ratio range of the grinding balls to the materials as (a, b), the rotating speed of the ball mill as c, and the ball milling time as d in the ball milling step;
s22, respectively taking x1, x2 and x3 from small to large between a and b, c and d are fixed, 3 mixed powder samples are prepared, and the percentage of the particle size of the largest part of the particle size distribution is determined
S23, taking x4 as a new sample;
s24, neutralizing with x1, x2 and x3
The two values that are close are the end values of the preferred weight ratio range of the grinding balls to the materials;
s25, repeating S22-S24 until the percentage of the difference value of the two end values of the weight ratio range of the grinding balls and the materials to the smaller end value is less than 5%, and taking the middle value of the end values as the weight ratio of the final grinding balls and the materials;
wherein a is more than or equal to 3, b is less than or equal to 20, c is more than or equal to 60rpm at 10rpm, d is more than or equal to 20h at 5 h; when the particle size is counted, the particle size distribution range is less than 3um, 3-5um, 5-10um, 10-20um and more than 20 um.
In some embodiments of the present invention, the step of S13 further comprises a step of checking the uniformity of the dried powder:
s21, taking a samples of the mixed powder with fixed drying time and a sample of the mixed powder with 15-25% prolonged drying time at the same drying temperature, wherein a is more than 10, and testing the flowability of the powder and recording the flowability as vectors X1 and X2;
s22, calculating the stability of the vector using the following formula:
the vector X1 has a stability of
The vector X2 has a stability of
Wherein,
s24, if
If the drying time is less than 3.02, determining the fixed drying time as the drying time;
if it is not
If the drying time is more than 3.02, the drying time is prolonged by 15 to 25 percent to obtain a new drying time, and the steps S21 to S22 are repeated until the drying time is increased to be more than 3.02
Less than 3.02.
The beneficial technical effects of the invention are as follows:
(1) according to the preparation method of the high-conductivity graphene composite aluminum alloy for the cable, the mixed powder which is suitable for being mixed with molten aluminum is obtained through ball milling of graphene and atomized aluminum powder;
(2) according to the preparation method of the high-conductivity graphene composite aluminum alloy for the cable, disclosed by the invention, the graphene and the molten aluminum are mixed under the condition of introducing the mixed gas of nitrogen and carbon dioxide, so that the strength and the conductivity of the obtained alloy composite material can be obviously improved compared with the single nitrogen or carbon dioxide;
(3) the aluminum alloy rod material prepared by the preparation method of the high-conductivity graphene composite aluminum alloy for the cable has excellent conductivity and strength performance, the conductivity is higher than 60.0% IACS, and the strength is higher than 180 MPa.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The experimental procedures used in the following examples and comparative examples are conventional ones unless otherwise specified. The graphene is prepared by a Hummer's method; atomized aluminum powder is N2Atomization, 60-80um. The aluminum material is a 6061 aluminum plate, which is provided by Rongchu metal materials Co., Ltd. The continuous casting and rolling are carried out by adopting conventional steps and parameters, and are not limited specifically. In the following examples and comparative examples, unless otherwise specified, parallel tests were conducted with the same components, contents, operating procedures and parameters.
Example 1
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:2 (40 m) and introduced at a flow rate of3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 2
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 15:1, the rotating speed of the ball mill is 20rpm, and the ball milling is carried out for 15 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 90 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:2 (40 m) and introduced at a flow rate of3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 3
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 50rpm, and the ball milling is carried out for 8 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 2 hours in vacuum at the temperature of 80 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:2 (40 m) and introduced at a flow rate of3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 4
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:3, and the flow rate of air was 40m3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 5
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:4, and the flow rate of air was 40m3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 6
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:1, and the flow rate of air was 40m3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 7
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:5, and the flow rate of air was 40m3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Example 8
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
the difference from the embodiment 1 is that in the step of S11, the method further comprises the step of determining the weight ratio of the grinding balls to the material:
s21, setting the weight ratio range of the grinding balls to the materials as (a, b), the rotating speed of the ball mill as c, and the ball milling time as d in the ball milling step;
s22, respectively taking x1, x2 and x3 from small to large between a and b, c and d are fixed, 3 mixed powder samples are prepared, and the percentage of the particle size of the largest part of the particle size distribution is determined
S23, taking x4 as a new sample;
s24, neutralizing with x1, x2 and x3
The two values that are close are the end values of the preferred weight ratio range of the grinding balls to the materials;
s25, repeating S22-S24 until the percentage of the difference value of the two end values of the weight ratio range of the grinding balls and the materials to the smaller end value is less than 5%, and taking the middle value of the end values as the weight ratio of the final grinding balls and the materials;
wherein a is more than or equal to 3, b is less than or equal to 20, c is more than or equal to 60rpm at 10rpm, d is more than or equal to 20h at 5 h; when the particle size is counted, the particle size distribution range is less than 3um, 3-5um, 5-10um, 10-20um and more than 20 um.
According to the preparation method of the high-conductivity graphene composite aluminum alloy for the cable, the particle size of the mixed powder particles after ball milling directly influences the performance of the obtained alloy. The weight ratio of the grinding balls to the material in this example was determined quickly by taking the diameter of the body portion as an indication parameter.
Example 9
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
the difference from the example 1 is that the step of S13 further includes a step of checking the uniformity of the dried powder:
s21, taking a samples of the mixed powder with fixed drying time and a sample of the mixed powder with 15-25% prolonged drying time at the same drying temperature, wherein a is more than 10, and testing the flowability of the powder and recording the flowability as vectors X1 and X2;
s22, calculating the stability of the vector using the following formula:
the vector X1 has a stability of
The vector X2 has a stability of
Wherein,
s24, if
Less than 3.02, the fixed drying time is determined to be dryDrying time;
if it is not
If the drying time is more than 3.02, the drying time is prolonged by 15 to 25 percent to obtain a new drying time, and the steps S21 to S22 are repeated until the drying time is increased to be more than 3.02
Less than 3.02.
According to the preparation method of the high-conductivity graphene composite aluminum alloy for the cable, the mixed powder needs to be thoroughly dried in vacuum, and the drying degree influences the flowability of the powder and the mixing of the powder and molten aluminum metal. The uniformity test of the powder determined in the embodiment ensures the uniformity of the mixed powder and eliminates the system error of the aluminum alloy ingot casting performance caused by drying.
Comparative example 1
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in a nitrogen gas atmosphere at a flow rate of 40m3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing nitrogen gas for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Comparative example 2
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and ball-milled by a ball mill. The weight ratio of the grinding balls to the materials is 10:1, the rotating speed of the ball mill is 30rpm, and the ball milling is carried out for 10 hours. During ball milling, the milling balls are immersed by liquid nitrogen.
(2) The ball-milled mixed powder is dried for 1 hour in vacuum at the temperature of 85 ℃;
(3) 98g of an aluminum material was melted in an atmosphere of carbon dioxide gas at a flow rate of 40m3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing carbon dioxide gas for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Comparative example 3
A preparation method of a high-conductivity graphene composite aluminum alloy for cables comprises the following steps:
(1) 2g of graphene and 98g of atomized aluminum powder are taken and mixed uniformly.
(2) Vacuum drying the mixed powder at 85 deg.C for 1 h;
(3) 98g of an aluminum material was melted in a mixed gas atmosphere of nitrogen and carbon dioxide at a volume ratio of 1:2 (40 m) and introduced at a flow rate of3/h；
(4) Adding the powder obtained in the step (2), and uniformly mixing;
(5) continuously introducing the mixed gas of nitrogen and carbon dioxide for 30 min;
(6) and carrying out continuous casting and continuous rolling to obtain the aluminum alloy ingot.
Examples of the experiments
The aluminum alloy ingots prepared in the examples were observed by SEM, and it was found that graphene was uniformly dispersed in the aluminum alloy ingots.
The aluminum alloy ingots obtained in examples and comparative examples were rolled into rods (5 to 8mm in diameter), and the strength and electric conductivity of the rods were measured.
The strength test adopts a method of GB/T3954-2014 electrical round aluminum rod, and the conductivity test adopts a method of Q/GDW 1815-2012 aluminum alloy core high-conductivity aluminum stranded wire. The results are shown in Table 1.
TABLE 1 Effect on Strength and conductivity
In the same column of data, marked with different lower case letters, the representation has significant difference, and P is less than 0.05
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (9)
1. A preparation method of a high-conductivity graphene composite aluminum alloy for cables is characterized by comprising the following steps:
s11, taking graphene and atomized aluminum powder, and performing ball milling by using a ball mill, wherein liquid nitrogen is used for immersing the milling balls during ball milling;
s12, vacuum drying the mixed powder obtained in S11;
s13, melting aluminum material under the condition of introducing mixed gas of nitrogen and carbon dioxide;
s14, adding the dried mixed powder obtained in the step S12 into the molten aluminum obtained in the step S13, and mixing;
s15, continuously introducing mixed gas of nitrogen and carbon dioxide;
s16, preparing an aluminum alloy ingot;
wherein, in the step of S13, the method further comprises the step of checking the uniformity of the dried powder:
s21, taking a samples of the mixed powder with fixed drying time and a sample of the mixed powder with 15-25% prolonged drying time at the same drying temperature, wherein a is more than 10, and testing the flowability of the powder and recording the flowability as vectors X1 and X2;
s22, calculating the stability of the vector using the following formula:
the vector X1 has a stability of
The vector X2 has a stability of
Wherein,
s24, if
If the drying time is less than 3.02, determining the fixed drying time as the drying time;
if it is not
If the drying time is more than 3.02, the drying time is prolonged by 15 to 25 percent to obtain a new drying time, and the steps S21 to S22 are repeated until the drying time is increased to be more than 3.02
Less than 3.02.
2. The preparation method according to claim 1, wherein in S11, the weight ratio of the graphene to the atomized aluminum powder is (1-3): (97-99).
3. The method according to claim 1, wherein in S14, the weight ratio of the dry mixed powder to the molten aluminum is (90-110): (90-110).
4. The preparation method according to claim 1, wherein in S11, when the ball milling is carried out by using the ball mill, the weight ratio of the milling balls to the material is (10-15):1, the rotation speed of the ball mill is 30-50rpm, and the ball milling is carried out for 8-15 h.
5. The method according to claim 1, wherein the vacuum drying in S12 is carried out at 80-90 ℃ for 1-2 h.
6. The method according to claim 1, wherein in S13, the volume ratio of nitrogen to carbon dioxide in the mixed gas is 1: (1-5), wherein the flow rate of the mixed gas is (35-45) m3/h。
7. The method according to claim 1, wherein in S13, the volume ratio of nitrogen to carbon dioxide in the mixed gas is 1: (2-4), wherein the flow rate of the mixed gas is (35-45) m3/h。
8. The method according to claim 1, wherein the aeration is continued for 20 to 40min at S15.
9. The method as claimed in claim 1, wherein the step of S11 further comprises the step of determining the weight ratio of grinding balls to material:
s21, setting the weight ratio range of the grinding balls to the materials as (a, b), the rotating speed of the ball mill as c, and the ball milling time as d in the ball milling step;
s22, respectively taking x1, x2 and x3 from small to large between a and b, c and d are fixed, 3 mixed powder samples are prepared, and the percentage of the particle size of the largest part of the particle size distribution is determined
S23, taking x4 as a new sample;
s24, neutralizing with x1, x2 and x3
The two values that are close are the end values of the preferred weight ratio range of the grinding balls to the materials;
s25, repeating S22-S24 until the percentage of the difference value of the two end values of the weight ratio range of the grinding balls and the materials to the smaller end value is less than 5%, and taking the middle value of the end values as the weight ratio of the final grinding balls and the materials;
wherein a is more than or equal to 3, b is less than or equal to 20, c is more than or equal to 60rpm at 10rpm, d is more than or equal to 20h at 5 h; when the particle size is counted, the particle size distribution range is less than 3um, 3-5um, 5-10um, 10-20um and more than 20 um.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498223A (en) * | 2016-11-16 | 2017-03-15 | 银邦金属复合材料股份有限公司 | A kind of modified graphene reinforced aluminum matrix composites and preparation method thereof |
| CN106756263A (en) * | 2016-11-14 | 2017-05-31 | 安徽名杰净化科技有限公司 | A kind of purification of air pretreatment chamber aluminium alloy preparation method |
| CN107675028A (en) * | 2017-09-25 | 2018-02-09 | 广州埃米石墨烯投资管理有限公司 | A kind of single-layer graphene/aluminium composite material and preparation method thereof |
| 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 |
| CN112453386A (en) * | 2020-11-23 | 2021-03-09 | 安徽竣阳信息技术有限公司 | Graphene aluminum-based composite material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4504914B2 (en) * | 2005-12-19 | 2010-07-14 | 株式会社神戸製鋼所 | Aluminum ingot manufacturing method, aluminum ingot, and protective gas for manufacturing aluminum ingot |
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2021
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756263A (en) * | 2016-11-14 | 2017-05-31 | 安徽名杰净化科技有限公司 | A kind of purification of air pretreatment chamber aluminium alloy preparation method |
| CN106498223A (en) * | 2016-11-16 | 2017-03-15 | 银邦金属复合材料股份有限公司 | A kind of modified graphene reinforced aluminum matrix composites and preparation method thereof |
| CN107675028A (en) * | 2017-09-25 | 2018-02-09 | 广州埃米石墨烯投资管理有限公司 | A kind of single-layer graphene/aluminium composite material and preparation method thereof |
| 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 |
| CN112453386A (en) * | 2020-11-23 | 2021-03-09 | 安徽竣阳信息技术有限公司 | Graphene aluminum-based composite material and preparation method thereof |
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