CN109161709B - Preparation method of cracked carbon nanotube reinforced copper-based composite material - Google Patents
Preparation method of cracked carbon nanotube reinforced copper-based composite material Download PDFInfo
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- CN109161709B CN109161709B CN201810862025.0A CN201810862025A CN109161709B CN 109161709 B CN109161709 B CN 109161709B CN 201810862025 A CN201810862025 A CN 201810862025A CN 109161709 B CN109161709 B CN 109161709B
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- C22C1/00—Making non-ferrous alloys
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C22C2026/002—Carbon nanotubes
Abstract
The invention discloses a preparation method of a cracked carbon nanotube reinforced copper-based composite material, which comprises the steps of dispersing carbon nanotubes in concentrated sulfuric acid, adding concentrated phosphoric acid and potassium permanganate for magnetic stirring, heating, preserving heat, cooling to room temperature, adding deionized water containing hydrogen peroxide under the ice bath condition, cleaning to obtain cracked carbon nanotubes, preparing the prepared cracked carbon nanotubes and copper acetate into a solution to obtain a precursor, dripping glucose and hydrazine hydrate under magnetic stirring, carrying out suction filtration, drying and annealing to obtain composite powder, preparing the composite powder into a block material through SPS sintering, and carrying out hot extrusion and annealing to obtain the cracked carbon nanotube reinforced copper-based composite material; according to the invention, the carbon nano tube is subjected to oxidative cracking treatment to obtain the cracked carbon nano tube with adjustable length-width ratio, so that the strength of the composite material is improved, the plasticity of the material is considered, and the composite material has good comprehensive mechanical properties.
Description
Technical Field
The invention relates to a preparation method of a cracked carbon nanotube reinforced copper-based composite material, belonging to the technical field of composite material preparation.
Background
Due to their unique physical and chemical properties, Carbon Nanotubes (CNTs) have received considerable attention from researchers as reinforcements for composite materials. However, due to the nano-linear structure and chemical inertness of the surface of the Carbon Nanotubes (CNTs), the Carbon Nanotubes (CNTs) are very easy to agglomerate, and especially when used as a reinforcement in a composite material, the properties of each part of the composite material are not uniform. During the load transfer process, only the outer layer of defective Carbon Nanotubes (CNTs) plays a role in load transfer, and the inner layer is hardly utilized. Compared with Carbon Nanotubes (CNTs), Graphene Oxide (GO) with a two-dimensional structure has a larger specific surface area, so that the contact area between the Graphene oxide and a matrix is greatly increased, and the load transfer efficiency is improved. However, the aspect ratio of the commercialized graphene oxide GO is small, which is not enough to provide enough length to bear load transfer to the maximum, and a large amount of wrinkles exist on the surface of the industrially produced graphene oxide GO, which is not beneficial to the improvement of the comprehensive performance of the composite material. The large specific surface area enables graphene oxide GO to be easily damaged when the composite material is prepared, and the reinforcing efficiency of the graphene oxide GO is reduced.
At present, the commonly used process for preparing the Carbon Nano Tube (CNTs) reinforced copper-based composite material mainly comprises a powder metallurgy method, a spraying method, a chemical deposition method and the like. In the composite material prepared by the method, the strengthening efficiency of the reinforcement body has a large difference compared with a theoretical value, because the Carbon Nanotubes (CNTs) are poor in wettability with a metal matrix, the Carbon Nanotubes (CNTs) are difficult to be uniformly dispersed in the metal matrix, so that firm interface combination is difficult to form with the matrix, the strengthening efficiency is low, and the strengthening effect is far lower than that predicted by the theory.
Disclosure of Invention
Aiming at the problems, the invention adopts a molecular level blending method to prepare the cracked Carbon Nano Tube (CNTs) reinforced copper-based composite material, effectively realizes the uniform dispersion of the reinforcement in a matrix, and simultaneously keeps the structural integrity of the reinforcement.
The invention provides a preparation method of a cracked carbon nanotube reinforced copper-based composite material, which comprises the following specific steps:
(1) and (3) cracking of the carbon nanotubes:
adding carbon nanotubes into concentrated sulfuric acid, stirring for 1-2 hours, simultaneously adding concentrated phosphoric acid and potassium permanganate, stirring to obtain a suspension, then putting the suspension into a water bath kettle, heating to 70-80 ℃, keeping the temperature for 2-5 hours, cooling to room temperature, then pouring deionized water containing hydrogen peroxide under the condition of ice bath, respectively cleaning precipitates with hydrochloric acid and absolute ethyl alcohol, carrying out vacuum filtration, and drying at 70-80 ℃ for 24 hours to obtain cracked CNTs;
(2) preparing a precursor solution:
mixing the cracked CNTs prepared in the step (1) with copper acetate to prepare a precursor, wherein the volume fraction of the cracked CNTs in the precursor is 1-2%;
(3) and (3) sintering:
adding glucose into the precursor prepared in the step (2) under magnetic stirring, dropwise adding hydrazine hydrate until the solution is brownish, obtaining suspension, carrying out vacuum filtration on the suspension, drying at 70-80 ℃ for 24 hours to obtain composite powder, annealing the composite powder in a tubular furnace under inert atmosphere to obtain composite powder of cracked CNTs and copper, and finally carrying out SPS sintering on the annealed composite powder to obtain a block material;
(4) hot extrusion treatment:
heating the block material prepared in the step (3) to the temperature of 500-;
(5) and (3) subsequent processing treatment: and (4) annealing the composite bar extruded in the step (4) in a tube furnace under an inert atmosphere to obtain the cracked carbon nanotube reinforced copper-based composite material.
And (2) adding concentrated sulfuric acid into the CNTs in the step (1) according to the mass-volume ratio g: m L of the CNTs to the concentrated sulfuric acid of 1: 5-8.
Adding concentrated phosphoric acid in the step (1) according to the volume ratio of concentrated sulfuric acid to concentrated phosphoric acid of 1: 8-9.
The potassium permanganate in the step (1) is added according to the mass ratio of the CNTs to the potassium permanganate of 1: 5-8.
The volume fraction of the hydrogen peroxide in the deionized water containing the hydrogen peroxide in the step (1) is 2.5%.
The rotation speed of the magnetic stirring in the step (3) is 260-300 r/min.
And (3) adding the glucose according to the mass ratio of the CNTs to the glucose of 1: 10-20.
The SPS sintering process in the step (3) comprises the following specific steps: keeping the temperature at 700-750 ℃ for 10-15 minutes under the condition of 50 MPa.
And (4) in the step (3), the step (4) and the step (5), the inert atmosphere is argon atmosphere or argon-hydrogen atmosphere.
The annealing treatment process in the step (5) and the step (3) is the same, and specifically comprises the following steps: annealing at 300 ℃ for 3-5 hours at 250 ℃.
The concentrated sulfuric acid in the step (1) is sulfuric acid with the mass fraction of 98% purchased from the market, and the concentrated phosphoric acid is phosphoric acid with the mass fraction of 85% purchased from the market.
The SPS sintering is an abbreviation for spark plasma sintering.
The invention opens partial pipe wall of CNTs through oxidation reaction, obtains a complex body simultaneously having CNTs and GO structure, and uses the complex body for reinforcing copper-based composite material, the cracked CNTs well combines the advantages of CNTs and GO, the cracked outer pipe wall provides GO attribute, the uncracked inner pipe wall provides CNTs attribute, the cracked CNTs have high length-width ratio and flat edge, and simultaneously has the structure of CNTs and GO, thereby making up the defect that single CNTs or GO is used as a reinforcement body on a certain aspect, compared with the smaller length-width ratio of GO, the cracked CNTs have larger length-width ratio, therefore, enough length can be provided to bear larger load transfer in the load transfer process, in addition, the inner pipe wall of CNTs is exposed through cracking, the defect that CNTs only have outer structure function in the load transfer process is effectively improved, therefore, the cracked CNTs are used as a reinforcement body and added into the composite material to effectively improve the strength of the composite material, and simultaneously, the composite material keeps better plasticity.
The invention has the beneficial effects that:
according to the bionics principle, the CNTs are subjected to cracking treatment to obtain a leaf-shaped novel reinforcement body with the characteristics of the CNTs and GO, the outer GO structure of the novel reinforcement body can effectively increase the contact area with a metal matrix, the load transfer efficiency is improved, the CNTs structure of the inner layer is similar to veins, and the strength of the composite material can be effectively improved.
The method has the advantages of novel design, more reasonable reinforcement structure, capability of realizing the uniform dispersion of the reinforcement in the matrix, capability of obtaining the copper-based composite material with good comprehensive mechanical property, simple and convenient process, simple equipment, easiness in realization and capability of being popularized and applied to the preparation of other metal-based and polymer-based composite materials.
Drawings
FIG. 1 is a transmission electron micrograph of cleaved CNTs obtained in step (1) of example 1 of the present invention;
FIG. 2 is a scanning electron microscope photograph of the composite powder after the annealing treatment of step (3) in example 1 of the present invention;
FIG. 3 is a scanning electron microscope photograph of a bulk material obtained by SPS sintering in step (3) of example 1 of the present invention.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, but the scope of the invention is not limited thereto.
Example 1
A preparation method of a cracking carbon nano tube reinforced copper-based composite material comprises the following specific steps:
(1) and (3) cracking of the carbon nanotubes:
adding carbon nano tube CNTs into concentrated sulfuric acid according to the mass-volume ratio g of the CNTs to the concentrated sulfuric acid, wherein m L is 1:5, stirring for 1 hour, simultaneously adding concentrated phosphoric acid and potassium permanganate according to the volume ratio of the concentrated sulfuric acid to the concentrated phosphoric acid being 1:8, stirring to obtain a suspension, adding the potassium permanganate according to the mass ratio of the CNTs to the potassium permanganate being 1:5, then putting the suspension into a water bath kettle, heating to 70 ℃ for 5 hours, cooling to room temperature, pouring deionized water containing hydrogen peroxide according to the volume ratio of the suspension to the deionized water containing hydrogen peroxide being 1:5 under the ice bath condition, wherein the volume fraction of the hydrogen peroxide in the deionized water containing the hydrogen peroxide is 2.5%, then respectively cleaning the precipitate with hydrochloric acid and absolute ethyl alcohol for 5 times, carrying out vacuum filtration and drying at 70 ℃ for 24 hours to obtain cracked CNTs, wherein the concentrated sulfuric acid with the mass fraction of 98% and the concentrated phosphoric acid with the mass fraction of 85% are purchased from markets;
(2) preparing a precursor solution:
mixing the cracked CNTs prepared in the step (1) with copper acetate to prepare a precursor, wherein the volume fraction of the cracked CNTs in the precursor is 1%;
(3) and (3) sintering:
adding glucose into the precursor prepared in the step (2) under the magnetic stirring of 260 revolutions per minute according to the mass ratio of the cracked CNTs to the glucose of 1:10, dropwise adding hydrazine hydrate until the solution is brownish, stopping dropwise adding to obtain a suspension, carrying out vacuum filtration on the suspension, drying at 70 ℃ for 24 hours to obtain composite powder, annealing the composite powder in a tubular furnace at 250 ℃ for 5 hours under the nitrogen atmosphere to obtain composite powder of the cracked CNTs and copper, and finally carrying out SPS sintering on the annealed composite powder to obtain a block material, wherein the specific process of the SPS sintering is to heat the composite powder to 750 ℃ under the 50MPa condition and preserve heat for 10 minutes;
(4) hot extrusion treatment:
heating the block material prepared in the step (3) to 500 ℃ in a nitrogen atmosphere, preheating an extrusion cylinder and an extrusion die to 500 ℃, assembling the extrusion die and the extrusion cylinder, quickly transferring a hot ingot blank to the extrusion cylinder, and performing hot extrusion at 500 ℃ to obtain a composite bar;
(5) and (3) subsequent processing treatment: and (4) annealing the composite bar extruded in the step (4) for 5 hours at 250 ℃ in a tube furnace in the nitrogen atmosphere to obtain the cracked carbon nanotube reinforced copper-based composite material.
FIG. 1 is a transmission electron microscope image of the cracked carbon nanotube in step (1), from which it can be seen that the inner layer of the cracked carbon nanotube retains a tubular structure and the outer layer presents a graphene structure; FIG. 2 is a scanning electron microscope image of the composite powder after annealing treatment in step (3), in which the cracked carbon nanotubes are a composite of CNT and GO, and it can be seen that the cracked carbon nanotubes are well bonded to the matrix; FIG. 3 is a scanning electron microscope image of the bulk material obtained by SPS sintering in step (3), the cracked carbon nanotubes are a composite of CNT and GO, and it can be seen from the image that the cracked carbon nanotubes are uniformly dispersed in the matrix, which has a good reinforcing effect.
The tensile strength of the cracked carbon nanotube reinforced copper-based composite material obtained by the embodiment reaches 238MPa, and is increased by 25% compared with pure copper.
Example 2
A preparation method of a cracking carbon nano tube reinforced copper-based composite material comprises the following specific steps:
(1) and (3) cracking of the carbon nanotubes:
adding carbon nano tube CNTs into concentrated sulfuric acid according to the mass-volume ratio g of the CNTs to the concentrated sulfuric acid, wherein m L is 1:6, stirring for 1.5 hours, simultaneously adding concentrated phosphoric acid and potassium permanganate, stirring to obtain a suspension, adding the concentrated phosphoric acid according to the volume ratio of the concentrated sulfuric acid to the concentrated phosphoric acid, adding the potassium permanganate according to the mass ratio of the CNTs to the potassium permanganate of 1:7, then putting the suspension into a water bath kettle, heating to 75 ℃ for 3 hours, cooling to room temperature, pouring deionized water containing hydrogen peroxide according to the volume ratio of 1:5 of the suspension to the deionized water containing hydrogen peroxide under the ice bath condition, wherein the volume fraction of the hydrogen peroxide in the deionized water containing the hydrogen peroxide is 2.5%, then respectively cleaning precipitates with hydrochloric acid and absolute ethyl alcohol for 6 times, carrying out vacuum filtration and drying at 75 ℃ for 24 hours to obtain cracked CNTs, wherein the sulfuric acid with the mass fraction of 98% is purchased, and the concentrated phosphoric acid with the mass fraction of 85% is purchased;
(2) preparation of precursor solution
Mixing the cracked CNTs prepared in the step (1) with copper acetate to prepare a precursor, wherein the volume fraction of the cracked CNTs in the precursor is 1.5%;
(3) and (3) sintering:
adding the cracked CNTs and glucose according to the mass ratio of 1:12, adding glucose into the precursor prepared in the step (2) under magnetic stirring at 280 revolutions per minute, dropwise adding hydrazine hydrate until the solution is brownish, stopping dropwise adding to obtain a suspension, performing vacuum filtration on the suspension, drying at 75 ℃ for 24 hours to obtain composite powder, annealing the composite powder in a tubular furnace at 280 ℃ for 4 hours under the nitrogen atmosphere to obtain composite powder of the cracked CNTs and copper, and performing SPS sintering on the annealed composite powder to obtain a block material, wherein the specific process of the SPS sintering is to heat the composite powder to 720 ℃ for 13 minutes under the 50MPa condition;
(4) hot extrusion treatment:
heating the block material prepared in the step (3) to 600 ℃ in a nitrogen atmosphere, preheating an extrusion cylinder and an extrusion die to 600 ℃, assembling the extrusion die and the extrusion cylinder, quickly transferring a hot ingot blank to the extrusion cylinder, and performing hot extrusion at 600 ℃ to obtain a composite bar;
(5) and (3) subsequent processing treatment: and (4) annealing the composite bar extruded in the step (4) for 4 hours at 280 ℃ in a tubular furnace in the nitrogen atmosphere to obtain the cracked carbon nanotube reinforced copper-based composite material.
The tensile strength of the cracked carbon nanotube reinforced copper-based composite material obtained by the embodiment reaches 270MPa, and is improved by 42% compared with pure copper.
Example 3
A preparation method of a cracking carbon nano tube reinforced copper-based composite material comprises the following specific steps:
(1) and (3) cracking of the carbon nanotubes:
adding carbon nano tube CNTs into concentrated sulfuric acid according to the mass-volume ratio g of the CNTs to the concentrated sulfuric acid, wherein m L is 1:8, stirring for 2 hours, simultaneously adding concentrated phosphoric acid and potassium permanganate, stirring to obtain a suspension, adding the concentrated phosphoric acid according to the volume ratio of the concentrated sulfuric acid to the concentrated phosphoric acid being 1:9, adding the potassium permanganate according to the mass ratio of the CNTs to the potassium permanganate being 1:8, then putting the suspension into a water bath kettle, heating to 80 ℃, keeping the temperature for 2 hours, cooling to room temperature, pouring deionized water containing hydrogen peroxide according to the volume ratio of the suspension to the deionized water containing the hydrogen peroxide being 1:5 under the ice bath condition, wherein the volume fraction of the hydrogen peroxide in the deionized water containing the hydrogen peroxide is 2.5%, then respectively cleaning precipitates with hydrochloric acid and absolute ethyl alcohol for 6 times, carrying out vacuum filtration, and drying at 80 ℃ for 24 hours to obtain cracked CNTs, wherein the concentrated sulfuric acid with the mass fraction of 98% and the concentrated phosphoric acid with the mass fraction of 85% are purchased from markets;
(2) preparing a precursor solution:
mixing the cracked CNTs prepared in the step (1) with copper acetate to prepare a precursor, wherein the volume fraction of the cracked CNTs in the precursor is 2%;
(3) and (3) sintering:
adding the cracked CNTs and glucose according to the mass ratio of 1:20, adding glucose into the precursor prepared in the step (2) under the magnetic stirring of 300 revolutions per minute, dropwise adding hydrazine hydrate until the solution is brownish, stopping dropwise adding to obtain a suspension, carrying out vacuum filtration on the suspension, drying at 80 ℃ for 24 hours to obtain composite powder, then annealing the composite powder in a tubular furnace at 300 ℃ for 3 hours under the nitrogen atmosphere to obtain composite powder of the cracked CNTs and copper, and finally carrying out SPS sintering on the annealed composite powder to obtain a block material, wherein the specific process of the SPS sintering is to heat the composite powder to 700 ℃ under the condition of 50MPa and preserve heat for 15 minutes;
(4) hot extrusion treatment:
heating the block material prepared in the step (3) to 700 ℃ in a nitrogen atmosphere, preheating an extrusion cylinder and an extrusion die to 700 ℃, assembling the extrusion die and the extrusion cylinder, quickly transferring a hot ingot blank to the extrusion cylinder, and performing hot extrusion at 700 ℃ to obtain a composite bar;
(5) and (3) subsequent processing treatment: and (4) annealing the composite bar extruded in the step (4) for 3 hours at 300 ℃ in a tube furnace in the nitrogen atmosphere to obtain the cracked carbon nanotube reinforced copper-based composite material.
The tensile strength of the cracked carbon nanotube reinforced copper-based composite material obtained by the embodiment reaches 323MPa, and is improved by 70% compared with pure copper.
Claims (7)
1. A preparation method of a cracked carbon nanotube reinforced copper-based composite material is characterized by comprising the following specific steps:
(1) and (3) cracking of the carbon nanotubes:
adding a carbon nano tube into concentrated sulfuric acid, stirring for 1-2 hours, simultaneously adding concentrated phosphoric acid and potassium permanganate, stirring to obtain a suspension, heating the suspension to 70-80 ℃, preserving heat for 2-5 hours, cooling to room temperature, adding deionized water containing hydrogen peroxide under the condition of ice bath, respectively cleaning precipitates with hydrochloric acid and absolute ethyl alcohol, carrying out vacuum filtration, and drying at 70-80 ℃ for 24 hours to obtain a cracked carbon nano tube;
the mass volume ratio g: m L of the carbon nano tube to the concentrated sulfuric acid is 1: 5-8;
the volume ratio of the concentrated sulfuric acid to the concentrated phosphoric acid is 1: 8-9;
the mass ratio of the carbon nano tube to the potassium permanganate is 1: 5-8;
(2) preparing a precursor solution:
mixing the cracked carbon nano tube prepared in the step (1) with copper acetate to prepare a precursor, wherein the volume fraction of the cracked carbon nano tube in the precursor is 1-2%;
(3) and (3) sintering:
adding glucose into the precursor prepared in the step (2) under magnetic stirring, dropwise adding hydrazine hydrate until the solution is brownish, obtaining a suspension, carrying out vacuum filtration on the suspension, drying at 70-80 ℃ for 24 hours to obtain composite powder, annealing the composite powder under an inert atmosphere to obtain composite powder, and then carrying out SPS sintering to obtain a block material;
(4) hot extrusion treatment:
heating the block material prepared in the step (3) to the temperature of 500-;
(5) and (3) subsequent processing treatment: and (4) annealing the composite bar obtained in the step (4) in an inert atmosphere to obtain the cracked carbon nanotube reinforced copper-based composite material.
2. The method for preparing the cracked carbon nanotube reinforced copper-based composite material according to claim 1, wherein the volume fraction of hydrogen peroxide in the deionized water containing hydrogen peroxide in the step (1) is 2.5%.
3. The method as claimed in claim 1, wherein the magnetic stirring speed in step (3) is 260-300 rpm.
4. The method for preparing the cracked carbon nanotube reinforced copper-based composite material according to claim 1, wherein the glucose in the step (3) is added in a mass ratio of the carbon nanotubes to the glucose of 1: 10-20.
5. The method for preparing the cracked carbon nanotube reinforced copper-based composite material as claimed in claim 1, wherein the SPS sintering in the step (3) comprises the following specific processes: keeping the temperature at 700-750 ℃ for 10-15 minutes under the condition of 50 MPa.
6. The method for preparing the cracked carbon nanotube reinforced copper-based composite material according to claim 1, wherein the inert atmosphere in the step (3), the step (4) or the step (5) is an argon atmosphere or an argon-hydrogen atmosphere.
7. The method for preparing the cracked carbon nanotube reinforced copper-based composite material according to claim 1, wherein the annealing treatment in the step (5) and the step (3) is the same in process, and specifically comprises the following steps: annealing at 300 ℃ for 3-5 hours at 250 ℃.
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