CN112030044B - Carbon nano tube reinforced aluminum matrix composite material and preparation method thereof - Google Patents

Carbon nano tube reinforced aluminum matrix composite material and preparation method thereof Download PDF

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CN112030044B
CN112030044B CN202010850184.6A CN202010850184A CN112030044B CN 112030044 B CN112030044 B CN 112030044B CN 202010850184 A CN202010850184 A CN 202010850184A CN 112030044 B CN112030044 B CN 112030044B
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stainless steel
composite material
base material
carbon nanotube
rolling
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CN112030044A (en
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李菊英
梅青松
张国栋
肖海天
王北海
王宇杰
侯健荣
付宇枭
杜禹琰
杜远飞
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Wuhan Polytechnic University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1084Alloys containing non-metals by mechanical alloying (blending, milling)
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/002Carbon nanotubes

Abstract

The invention belongs to the field of preparation of carbon nanotube reinforced aluminum matrix composite, and discloses a carbon nanotube reinforced aluminum matrix composite and a preparation method thereof, wherein the raw materials of the composite comprise carbon nanotubes and a matrix material in percentage by weight; the method comprises the following steps: respectively pretreating a base material and a stainless steel plate; folding the smooth surface of the pretreated stainless steel plate and pressing the stainless steel plate into a stainless steel envelope; placing the carbon nano tube on the pretreated base material, folding the base material in half to enable the base material to wrap the carbon nano tube, then sealing the periphery of the base material and placing the base material into a stainless steel envelope; and rolling the stainless steel seal sleeve, folding the stainless steel seal sleeve along the length direction of the stainless steel seal sleeve after each pass of rolling, and rolling the stainless steel seal sleeve for the next pass until the set pass is reached. The invention can prepare the CNTs/Al composite material with different content of the strengthening phase at room temperature, and the prepared CNTs/Al composite material has uniform strengthening phase distribution, obvious strengthening effect and no second phase.

Description

Carbon nano tube reinforced aluminum matrix composite material and preparation method thereof
Technical Field
The invention belongs to the field of preparation of carbon nanotube reinforced aluminum matrix composites, and particularly relates to a carbon nanotube reinforced aluminum matrix composite and a preparation method thereof.
Background
Carbon Nanotubes (CNTs) are a one-dimensional nanotube material, and have the characteristics of low density, good mechanical properties, excellent thermal and electrical conductivity, and the like, and are ideal reinforcements for various composite materials. The carbon nano tube reinforced aluminum-based (CNTs/Al) composite material has wide application prospect in the fields of aerospace, automobile manufacturing, electronic instruments, military and the like due to the characteristics of high specific strength, high specific stiffness, low expansion coefficient, high thermal conductivity and the like.
The common preparation process for the carbon nanotube reinforced aluminum matrix (CNTs/Al) composite material comprises the following steps: powder metallurgy, stir casting, powder metallurgy combined with hot rolling or hot extrusion; the powder metallurgy method is to sinter at a temperature close to the melting point of aluminum; the stirring casting method is to add carbon nanotubes into the aluminum liquid; powder metallurgy is combined with hot rolling or hot extrusion by sintering near the melting point of aluminum and then hot rolling or hot extrusion at high temperature. These preparation processes all have the disadvantages of long preparation time, high temperature, etc., which easily causes a second phase between the carbon nanotubes and the aluminum matrix, and breaks the structure of the carbon nanotubes, thereby weakening the reinforcing effect of the carbon nanotubes.
201711198190.2 discloses an in-situ synthesized carbon nanotube reinforced aluminum matrix composite material, which adopts aluminum powder with purity of more than or equal to 99.0 percent and 200 meshes and CO (NO) with purity of more than or equal to 98.0 percent3)2·6H2And O is taken as a raw material, weighed and proportioned according to an experimental design scheme, poured into a hard alloy ball milling tank for wet milling after being prepared, and the prepared granules are subjected to vacuum drying and then added with a forming agent for granulation. And adding the prepared powder into a universal testing machine for pressing and forming, wherein the pressing pressure is 130 MPa. And putting the prepared pressed blank into a dewaxing-low pressure sintering integrated furnace for sintering, wherein the sintering temperature is 1200 ℃. 201610115738.1 discloses a method for preparing a carbon nanotube reinforced aluminum-based multilayer composite material. Uniformly dispersing carbon nanotubes into pure aluminum powder by adopting high-energy ball milling to obtain CNTs/Al precursor composite powder; filling the composite powder into a multi-layer pure aluminum casing pipe, tamping, vacuumizing and sealing; then, performing synchronous and asynchronous hot rolling and one-time cold rolling on the sheathed composite powder for multiple times; and (3) cutting the head and the tail of the CNTs/Al multilayer composite plate and cutting edges, and annealing to obtain the carbon nano tube reinforced aluminum-based multilayer composite material. 201811230060.7 discloses a method for preparing carbon nanotube composite material. Mixing carbon nanotube powder with aluminum powderThen ball milling is carried out for 10 h-30 h to obtain the product containing A14C3The composite powder of (1); mixing the carbon nano tube with the composite powder, ball-milling for 2-10 h, and uniformly dispersing in a matrix to obtain CNTs-A14C3A composite powder of/Al; CNTs-A14C3the/Al composite powder is cold-pressed and molded at room temperature and sintered in an argon environment to obtain CNTs-A14C3Performing hot extrusion on the sintered blank to obtain CNTs-A14C3a/Al composite material. 201610115737.7 discloses a method for preparing carbon nanotube reinforced aluminum matrix composite. Uniformly mixing carbon nano tubes and pure aluminum powder by adopting a high-energy ball milling method to obtain precursor composite powder of CNTs/Al, wherein the mass percent of the carbon nano tubes in the precursor composite powder is 0.5-5%, and the mass percent of the pure aluminum powder is 95-99.5%; pressing the CNTs/Al precursor composite powder into a cylindrical blank; then, sintering the cylindrical blank in vacuum or in the protective atmosphere of inert gas (such as nitrogen, argon and other common protective gases), wherein the sintering temperature is 500-620 ℃, and sintering is carried out for 2-8h to obtain a CNTs/Al composite material sintered blank; preparing a pure aluminum cylindrical blank with the same diameter as the sintering blank of the CNTs/Al composite material; and extruding the two ingots together by adopting a composite hot extrusion process to form a composite bar, then carrying out subsequent deformation processing on the composite bar by adopting drawing and rolling processes, and annealing to obtain the high-strength high-conductivity pure aluminum-coated carbon nano tube reinforced aluminum-based composite material. 201610115738.1, 201811230060.7 and 201610115737.7 all adopt a ball milling method to obtain precursor composite powder, and then the precursor composite powder is compounded with an aluminum tube, actually the obtained composite material of CNTs/Al + aluminum is obtained, and a part of aluminum matrix does not contain carbon nano tubes.
Disclosure of Invention
The invention aims to provide a carbon nano tube reinforced aluminum-based composite material and a preparation method thereof aiming at the defects of the prior art, and the carbon nano tube in the carbon nano tube reinforced aluminum-based (CNTs/Al) composite material can be uniformly and dispersedly distributed in a matrix material, so that the matrix material is effectively reinforced.
In order to achieve the above object, one aspect of the present invention provides a method for preparing a carbon nanotube reinforced aluminum matrix composite, wherein the raw materials of the composite comprise, by weight, 0.1-5% of carbon nanotubes and 95-99.9% of a matrix material;
the method comprises the following steps:
s1: respectively pretreating the base material and the stainless steel plate;
s2: folding the smooth surface of the pretreated stainless steel plate and pressing the stainless steel plate into a stainless steel envelope;
s3: placing the carbon nano tube on the pretreated base material, folding the base material with the carbon nano tube in half to enable the base material to wrap the carbon nano tube, and then sealing the periphery of the base material and placing the base material into the stainless steel envelope;
s4: and rolling the stainless steel envelope provided with the base material with the periphery sealed in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass.
Another aspect of the present invention provides a carbon nanotube-reinforced aluminum matrix composite prepared by the method.
The invention has the following beneficial effects:
the invention can prepare the CNTs/Al composite material with different content of the strengthening phase at room temperature, and the prepared CNTs/Al composite material has uniform distribution of the strengthening phase and obvious strengthening effect. The adopted equipment is a common double-roller cold rolling mill, the preparation process flow is simple, high temperature is not needed, the structure of the carbon nano-tube cannot be damaged, and no second phase is generated between the matrix material and the carbon nano-tube.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
Fig. 1 shows a process diagram of a method for preparing a carbon nanotube reinforced aluminum matrix composite provided by the invention.
Fig. 2 shows a CNTs/Al composite metallographic microscopic image with multi-walled carbon nanotubes of 3% prepared by the method for preparing a carbon nanotube reinforced aluminum matrix composite according to embodiment 3 of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The invention provides a preparation method of a carbon nano tube reinforced aluminum matrix composite, which comprises the following steps of (by weight percentage) preparing a composite material, wherein the raw materials of the composite material comprise 0.1-5% of carbon nano tubes and 95-99.9% of a matrix material; preferably 1.5-4.5% of the carbon nanotubes and 95.5-98.5% of the matrix material, and further preferably 2.5-3.5% of the carbon nanotubes and 96.5-97.5% of the matrix material;
the method comprises the following steps:
s1: respectively pretreating the base material and the stainless steel plate;
s2: folding the smooth surface of the pretreated stainless steel plate and pressing the stainless steel plate into a stainless steel envelope;
s3: placing the carbon nano tube on the pretreated base material, folding the base material with the carbon nano tube in half to enable the base material to wrap the carbon nano tube, and then sealing the periphery of the base material and placing the base material into the stainless steel envelope;
s4: and rolling the stainless steel envelope provided with the base material with the periphery sealed in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass.
The method of the present invention is suitable for both multi-wall carbon nanotubes and single-wall carbon nanotubes. From the viewpoint of cost and availability, the carbon nanotubes are preferably multi-walled carbon nanotubes.
According to the invention, preferably, the multi-walled carbon nanotubes have a purity of 99% to 99.99%, a diameter of 10 to 40nm, an aspect ratio of 1 to 100: 1-1000, tensile strength of 100-150 GPa.
According to the invention, the base material is preferably an industrially pure aluminum plate.
According to the present invention, preferably, the purity of the industrial pure aluminum plate is 99-99.99%, and the thickness is 0.2-0.5 mm.
According to the present invention, preferably, in step S1, the preprocessing step is: treating the base material by using sand paper, absolute ethyl alcohol and acetone; and (3) treating the stainless steel plate by using absolute ethyl alcohol and acetone.
According to the invention, the surface of the industrial pure aluminum plate is polished by using sand paper, the polishing aims at removing a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then the surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
According to the present invention, preferably, the stainless steel plate has a thickness of 0.4 to 0.6 mm.
According to the present invention, preferably, in step S4, the set pass is 10 to 20.
According to the invention, preferably, in step S2 and step S4, the pressing and rolling are performed by a double-roller cold rolling mill, the rotation speed of a motor of the double-roller cold rolling mill is 1400-1500r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 10-20m/min, and the reduction of the thickness of the rolled sample in each pass is 35-40%.
Another aspect of the present invention provides a carbon nanotube-reinforced aluminum matrix composite prepared by the method.
The method for preparing the carbon nanotube reinforced aluminum matrix composite according to the present invention will be described in detail with reference to fig. 1.
In the following examples, the multi-walled carbon nanotubes are obtained from Mitsui New Material science and technology, Inc. in Beijing, the multi-walled carbon nanotubes have a purity of 99-99.99%, a diameter of 10-40nm, and an aspect ratio of 1-100: 1-1000, tensile strength of 100-150 GPa. The purity of the industrial pure aluminum plate is 99-99.99%, and the size of the industrial pure aluminum plate is 50mm multiplied by 200mm multiplied by 0.5 mm.
Example 1
The raw materials of the composite material comprise 1 percent of multi-wall carbon nano-tube and 99 percent of industrial pure aluminum plate in percentage by weight; specifically, 0.136 grams of multi-walled carbon nanotubes were weighed.
The method comprises the following steps:
s1: respectively pretreating the industrial pure aluminum plate and the stainless steel plate with the thickness of 0.5 mm; the pretreatment steps are as follows: the surface of the industrial pure aluminum plate is polished by using abrasive paper, the purpose of polishing is to remove a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
S2: folding the smooth surface of the pretreated stainless steel plate with the thickness of 0.5mm in half and pressing the stainless steel plate into a stainless steel envelope by adopting a double-roller cold rolling mill; the motor rotating speed of the double-roller cold rolling mill is 1480r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 15m/min, and the reduction of the thickness of a rolled sample in each pass is 36%.
S3: placing the multi-walled carbon nanotube on the pretreated industrial pure aluminum plate, folding the industrial pure aluminum plate with the multi-walled carbon nanotube placed thereon in half, so that the industrial pure aluminum plate wraps the multi-walled carbon nanotube, and then sealing the periphery of the industrial pure aluminum plate and placing the industrial pure aluminum plate into the stainless steel envelope.
S4: and rolling the stainless steel envelope provided with the industrial pure aluminum plate with the sealed periphery in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass. The set pass is 20 times, the equipment that rolling adopted is the double-roller cold rolling mill, the motor speed of double-roller cold rolling mill is 1480r/min, the two-roller rolling speed of double-roller cold rolling mill is 15m/min, and the reduction of rolling sample thickness of each pass is 36%.
Example 2
The raw materials of the composite material comprise 2 percent of multi-wall carbon nano-tube and 98 percent of industrial pure aluminum plate in percentage by weight; specifically, 0.272 grams of multi-walled carbon nanotubes were weighed.
The method comprises the following steps:
s1: respectively pretreating the industrial pure aluminum plate and the stainless steel plate with the thickness of 0.5 mm; the pretreatment steps are as follows: the surface of the industrial pure aluminum plate is polished by using abrasive paper, the purpose of polishing is to remove a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
S2: folding the smooth surface of the pretreated stainless steel plate with the thickness of 0.5mm in half and pressing the stainless steel plate into a stainless steel envelope by adopting a double-roller cold rolling mill; the motor rotating speed of the double-roller cold rolling mill is 1480r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 15m/min, and the reduction of the thickness of a rolled sample in each pass is 38%.
S3: placing the multi-walled carbon nanotube on the pretreated industrial pure aluminum plate, folding the industrial pure aluminum plate with the multi-walled carbon nanotube placed thereon in half, so that the industrial pure aluminum plate wraps the multi-walled carbon nanotube, and then sealing the periphery of the industrial pure aluminum plate and placing the industrial pure aluminum plate into the stainless steel envelope.
S4: and rolling the stainless steel envelope provided with the industrial pure aluminum plate with the sealed periphery in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass. The set pass is 20 times, the equipment that rolling adopted is the double-roller cold rolling mill, the motor speed of double-roller cold rolling mill is 1480r/min, the two-roller rolling speed of double-roller cold rolling mill is 15m/min, and the reduction of rolling sample thickness of each pass is 38%.
Example 3
The raw materials of the composite material comprise 3 percent of multi-wall carbon nano-tube and 97 percent of industrial pure aluminum plate in percentage by weight; specifically, 0.408 grams of multi-walled carbon nanotubes were weighed.
The method comprises the following steps:
s1: respectively pretreating the industrial pure aluminum plate and the stainless steel plate with the thickness of 0.5 mm; the pretreatment steps are as follows: the surface of the industrial pure aluminum plate is polished by using abrasive paper, the purpose of polishing is to remove a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
S2: folding the smooth surface of the pretreated stainless steel plate with the thickness of 0.5mm in half and pressing the stainless steel plate into a stainless steel envelope by adopting a double-roller cold rolling mill; the motor rotating speed of the double-roller cold rolling mill is 1480r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 15m/min, and the reduction of the thickness of a rolled sample in each pass is 38%.
S3: placing the multi-walled carbon nanotube on the pretreated industrial pure aluminum plate, folding the industrial pure aluminum plate with the multi-walled carbon nanotube placed thereon in half, so that the industrial pure aluminum plate wraps the multi-walled carbon nanotube, and then sealing the periphery of the industrial pure aluminum plate and placing the industrial pure aluminum plate into the stainless steel envelope.
S4: and rolling the stainless steel envelope provided with the industrial pure aluminum plate with the sealed periphery in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass. The set pass is 20 times, the equipment that rolling adopted is the double-roller cold rolling mill, the motor speed of double-roller cold rolling mill is 1480r/min, the two-roller rolling speed of double-roller cold rolling mill is 15m/min, and the reduction of rolling sample thickness of each pass is 38%.
Example 4
The raw materials of the composite material comprise 4 percent of multi-wall carbon nano-tube and 96 percent of industrial pure aluminum plate in percentage by weight; specifically, 0.544 g of multi-walled carbon nanotubes was weighed.
The method comprises the following steps:
s1: respectively pretreating the industrial pure aluminum plate and the stainless steel plate with the thickness of 0.5 mm; the pretreatment steps are as follows: the surface of the industrial pure aluminum plate is polished by using abrasive paper, the purpose of polishing is to remove a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
S2: folding the smooth surface of the pretreated stainless steel plate with the thickness of 0.5mm in half and pressing the stainless steel plate into a stainless steel envelope by adopting a double-roller cold rolling mill; the motor rotating speed of the double-roller cold rolling mill is 1480r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 15m/min, and the reduction of the thickness of a rolled sample in each pass is 38%.
S3: placing the multi-walled carbon nanotube on the pretreated industrial pure aluminum plate, folding the industrial pure aluminum plate with the multi-walled carbon nanotube placed thereon in half, so that the industrial pure aluminum plate wraps the multi-walled carbon nanotube, and then sealing the periphery of the industrial pure aluminum plate and placing the industrial pure aluminum plate into the stainless steel envelope.
S4: and rolling the stainless steel envelope provided with the industrial pure aluminum plate with the sealed periphery in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass. The set pass is 20 times, the equipment that rolling adopted is the double-roller cold rolling mill, the motor speed of double-roller cold rolling mill is 1480r/min, the two-roller rolling speed of double-roller cold rolling mill is 15m/min, and the reduction of rolling sample thickness of each pass is 38%.
Example 5
The raw materials of the composite material comprise 2 percent of multi-wall carbon nano-tube and 98 percent of industrial pure aluminum plate in percentage by weight; specifically, 0.272 grams of multi-walled carbon nanotubes were weighed.
The method comprises the following steps:
s1: respectively pretreating the industrial pure aluminum plate and the stainless steel plate with the thickness of 0.5 mm; the pretreatment steps are as follows: the surface of the industrial pure aluminum plate is polished by using abrasive paper, the purpose of polishing is to remove a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
S2: folding the smooth surface of the pretreated stainless steel plate with the thickness of 0.5mm in half and pressing the stainless steel plate into a stainless steel envelope by adopting a double-roller cold rolling mill; the motor speed of the double-roller cold rolling mill is 1480r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 15m/min, and the reduction of the thickness of a rolled sample in each pass is 39%.
S3: placing the multi-walled carbon nanotube on the pretreated industrial pure aluminum plate, folding the industrial pure aluminum plate with the multi-walled carbon nanotube placed thereon in half, so that the industrial pure aluminum plate wraps the multi-walled carbon nanotube, and then sealing the periphery of the industrial pure aluminum plate and placing the industrial pure aluminum plate into the stainless steel envelope.
S4: and rolling the stainless steel envelope provided with the industrial pure aluminum plate with the sealed periphery in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass. The set pass is 10 times, the equipment that rolling adopted is two roller cold rolling mills, the motor speed of two roller cold rolling mills is 1480r/min, two roller rolling speed of two roller cold rolling mills is 15m/min, and the rolling reduction of rolling sample thickness of each pass is 39%.
Comparative example 1
The composite material comprises the following raw materials in percentage by weight: the raw materials of the composite material comprise 15% of multi-wall carbon nano-tubes and 85% of industrial pure aluminum plates; specifically, 2.04 grams of multi-walled carbon nanotubes were weighed.
The method comprises the following steps:
s1: respectively pretreating the industrial pure aluminum plate and the stainless steel plate with the thickness of 0.5 mm; the pretreatment steps are as follows: the surface of the industrial pure aluminum plate is polished by using abrasive paper, the purpose of polishing is to remove a compact oxide film which is easily formed in the air of the industrial pure aluminum plate, after polishing is finished, the surface is cleaned by using absolute ethyl alcohol, and then surface grease is removed by using acetone. For the stainless steel plate, the surface is wiped clean by the same absolute ethyl alcohol, and then the surface grease is wiped by acetone.
S2: folding the smooth surface of the pretreated stainless steel plate with the thickness of 0.5mm in half and pressing the stainless steel plate into a stainless steel envelope by adopting a double-roller cold rolling mill; the motor rotating speed of the double-roller cold rolling mill is 1480r/min, the rolling speed of two rollers of the double-roller cold rolling mill is 15m/min, and the reduction of the thickness of a rolled sample in each pass is 38%.
S3: placing the multi-walled carbon nanotube on the pretreated industrial pure aluminum plate, folding the industrial pure aluminum plate with the multi-walled carbon nanotube placed thereon in half, so that the industrial pure aluminum plate wraps the multi-walled carbon nanotube, and then sealing the periphery of the industrial pure aluminum plate and placing the industrial pure aluminum plate into the stainless steel envelope.
S4: and rolling the stainless steel envelope provided with the industrial pure aluminum plate with the sealed periphery in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass. The equipment that rolling adopted is two roller cold rolling mills, the motor speed of two roller cold rolling mills is 1480r/min, two roller rolling speed of two roller cold rolling mills is 15m/min, and the rolling reduction of rolling sample thickness of each pass is 38%. When the rolling pass reaches 10 times, the composite material is crushed into powder but not into blocks, because the carbon nano tube powder is more, the composite material cannot be bonded, and in addition, the wettability of the carbon nano tube particles and pure aluminum is poor, the composite material is very easy to crush. With the further increase of the rolling pass, the composite material still can not be bonded into blocks, and the whole composite material is dark gray black and has no metallic luster. Therefore, at 15% by weight of the multi-walled carbon nanotubes, CNTs/Al composite material could not be obtained, and Vickers hardness could not be measured.
Test example
The CNTs/Al composite material prepared in example 3 was subjected to sample embedding in the vertical rolling direction, and the microstructure of the CNTs/Al composite material prepared in example 3 was analyzed by a metallographic microscope, as shown in FIG. 2.
The CNTs/Al composite materials prepared in examples 1, 2, 3, 4, and 5 and comparative example 1 were each mounted in a parallel rolling direction and a perpendicular rolling direction, respectively, to measure the Vickers fiber hardness, and the Vickers hardness of the CNTs/Al composite materials prepared in examples 1, 2, 3, 4, and 5 and comparative example 1, which were measured in the parallel rolling direction and the perpendicular rolling direction using a 100 g load and a 10-second dwell time, is shown in Table 1.
TABLE 1
Figure BDA0002644462360000111
Figure BDA0002644462360000121
As can be seen from table 1 and fig. 2, the carbon nanotube reinforced aluminum matrix (CNTs/Al) composite prepared by the method of the present invention has significantly higher hardness, and the reinforcing phase is uniformly distributed, and no second phase is formed between the matrix material and the carbon nanotubes. In addition, the composite material prepared under the optimized conditions has better strengthening effect.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.

Claims (12)

1. A preparation method of a carbon nano tube reinforced aluminum matrix composite material is characterized in that,
the raw materials of the composite material comprise 0.1 to 5 weight percent of carbon nano tube and 95 to 99.9 weight percent of base material;
the method comprises the following steps:
s1: respectively pretreating the base material and the stainless steel plate;
s2: folding the smooth surface of the pretreated stainless steel plate and pressing the stainless steel plate into a stainless steel envelope;
s3: placing the carbon nano tube on the pretreated base material, folding the base material with the carbon nano tube in half to enable the base material to wrap the carbon nano tube, and then sealing the periphery of the base material and placing the base material into the stainless steel envelope;
s4: and rolling the stainless steel envelope provided with the base material with the periphery sealed in the step S3, folding the stainless steel envelope in half along the length direction of the stainless steel envelope after each rolling pass, and rolling the stainless steel envelope for the next pass until the set pass.
2. The method for preparing a carbon nanotube-reinforced aluminum-based composite material according to claim 1, wherein the raw materials of the composite material comprise, in weight percent, 1.5 to 4.5% of the carbon nanotubes and 95.5 to 98.5% of a matrix material.
3. The method for preparing a carbon nanotube-reinforced aluminum-based composite material according to claim 1, wherein the raw materials of the composite material comprise, in weight percent, 2.5 to 3.5% of the carbon nanotubes and 96.5 to 97.5% of a matrix material.
4. The method of claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes or single-walled carbon nanotubes.
5. The method for preparing a carbon nanotube-reinforced aluminum-based composite material according to claim 4, wherein the multi-walled carbon nanotube has a purity of 99-99.99%, a diameter of 10-40nm, an aspect ratio of 1-100: 1-1000, tensile strength of 100-150 GPa.
6. The method for producing a carbon nanotube-reinforced aluminum-based composite material according to claim 4, wherein the matrix material is an industrially pure aluminum sheet.
7. The method for preparing a carbon nanotube-reinforced aluminum-based composite material according to claim 6, wherein the purity of the industrial pure aluminum plate is 99-99.99%, and the thickness is 0.2-0.5 mm.
8. The method for producing a carbon nanotube-reinforced aluminum-based composite material as claimed in claim 1, wherein the step of pretreating in step S1 is: treating the base material by using sand paper, absolute ethyl alcohol and acetone; and (3) treating the stainless steel plate by using absolute ethyl alcohol and acetone.
9. The method for producing a carbon nanotube-reinforced aluminum-based composite material according to claim 8, wherein the stainless steel plate has a thickness of 0.4 to 0.6 mm.
10. The method for producing a carbon nanotube-reinforced aluminum-based composite material according to claim 9, wherein the set pass is 10 to 20 passes in step S4.
11. The method for preparing carbon nanotube reinforced aluminum-based composite material as claimed in claim 10, wherein in step S2 and step S4, the pressing and rolling are performed by a two-roll cold rolling mill, the rotation speed of the motor of the two-roll cold rolling mill is 1400-1500r/min, the rolling speed of the two rolls of the two-roll cold rolling mill is 10-20m/min, and the reduction of the thickness of the sample in each rolling pass is 35-40%.
12. A carbon nanotube reinforced aluminum matrix composite material prepared by the method of any one of claims 1 to 11.
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