CN109338167B - Preparation method of carbon nano tube composite material - Google Patents
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Abstract
The invention discloses a preparation method of a carbon nano tube composite material, belonging to the field of metal matrix composite material development; mixing carbon nanotube powder and aluminum powder, and then carrying out ball milling for 10-30 h to obtain the Al-containing alloy4C3The 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-Al4C3A composite powder of/Al; CNTs-Al4C3the/Al composite powder is cold-pressed and molded at room temperature and sintered in an argon environment to obtain CNTs-Al4C3Performing hot extrusion on the sintered blank to obtain CNTs-Al4C3a/Al composite material. The nano aluminum carbide generated in situ in the method is well combined with an aluminum matrix, and the nano aluminum carbide and the CNTs play a role in synergistic reinforcement on the composite material; provides a preparation method of an aluminum matrix composite material with excellent comprehensive mechanical properties.
Description
Technical Field
The invention relates to a preparation method of a carbon nano tube composite material, belonging to the field of composite material development.
Background
The composite material is a material which has strong vitality and emerges according to the requirements of modern scientific development, and is compounded by two or more materials with different properties through various process means. The aluminum has many characteristics in manufacturing composite materials, such as light weight, small density, good plasticity, easy mastering of aluminum-based composite technology, easy processing and the like. In addition, the aluminum matrix composite has high specific strength and specific rigidity, good high-temperature performance, better fatigue resistance and wear resistance, good damping performance and low thermal expansion coefficient. Like other composites, it combines specific mechanical and physical properties to meet product needs. Therefore, aluminum-based composites have become one of the most common, most important materials in metal-based composites.
CNTs have been known for their excellent physicochemical properties since their discovery in 1991. The tensile strength of the CNTs reaches 50-200 GPa, the Young modulus is equivalent to that of diamond, the strength is 100 times that of steel, and the density is about 1.2-2.1 g/cm31/6-1/7 of steel only; CNTs have excellent electric and heat conductivity, low thermal expansion coefficient and very wide application prospect, and can be used as a material for the production of the carbon nanotubesComposite reinforcements are considered to be the most desirable. However, the mechanical properties and further applications of the composite material are limited by the dispersibility of the CNTs in the matrix and the interface bonding problem with the Al matrix. Among the methods for preparing CNT/Al composite materials, the ball milling method is widely applied due to simple and flexible process and strong controllability.
However, in the conventional ball milling process, when CNTs react with aluminum to generate aluminum carbide, the structure of the carbon nanotube is often seriously damaged, so that the load transfer effect of the carbon nanotube is greatly weakened, and therefore, the ball milling process is improved, so that the dispersion strengthening effect of the aluminum carbide and the load transfer effect of the carbon nanotube can be exerted, and the ball milling process is very beneficial to further improving the mechanical property of the aluminum matrix composite.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nano tube composite material, which specifically comprises the following steps:
(1) mixing carbon nanotube powder and aluminum powder, and then carrying out ball milling for 10-30 h to obtain the Al-containing alloy4C3The composite powder of (1); wherein the mass of the carbon nanotube powder is 1-2wt.% of the total mass of the mixed powder;
(2) mixing the carbon nano tube with the composite powder obtained in the step (1), ball-milling for 2-10 h, and uniformly dispersing in a matrix to obtain CNTs-Al4C3A composite powder of/Al; wherein the mass of the newly added carbon nanotube powder is 1-2wt.% of the total mass of the composite powder;
(3) CNTs-Al4C3the/Al composite powder is cold-pressed and molded at room temperature and sintered in an argon environment to obtain CNTs-Al4C3Performing hot extrusion on the sintered blank to obtain CNTs-Al4C3a/Al composite material.
Preferably, the carbon nanotubes in the step (1) of the invention have the length of 10-30 μm, the diameter of 20-30 nm and the particle size of 20-30 μm.
Preferably, the ball milling in step (1) of the present invention comprises the following specific processes: placing carbon nano tubes, pure aluminum powder and grinding balls in a ball milling tank under the protection of inert gas, and adding stearic acid as a process control agent; wherein the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the high-energy ball milling is accumulated for 10-30 h.
Preferably, the ball milling in step (2) of the present invention comprises the following specific processes: mixing carbon nanotube with nano Al4C3Placing the composite powder of the particles and the grinding ball in a ball milling tank under the protective atmosphere of inert gas, and adding stearic acid as a process control agent; wherein the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the ball milling is accumulated for 2-10 h.
Preferably, the cold pressing and sintering processes of the composite powder in the step (3) of the invention are as follows: and cold-pressing the composite powder into a blank at room temperature under the pressure of 300MPa, and sintering for 4 hours at the temperature of 600 ℃ under the argon environment.
Preferably, the hot extrusion in step (3) of the present invention comprises the following specific steps: CNTs-Al4C3Heating the/Al composite material sintered blank to 450 ℃ in a vacuum or inert gas protective atmosphere heating furnace, and preserving heat for 2 hours until the internal and external temperatures of the ingot blank are uniform; simultaneously preheating the extrusion die; the sintered compact was hot extruded into a composite material using an extrusion ratio of 36: 1.
The invention adopts a two-step ball milling method to prepare CNTs-Al4C3The preparation process of the/Al composite material generates aluminum carbide nano particles, the aluminum carbide nano particles play a role in dispersion strengthening in the composite material, appropriate amount of CNTs are added to enable the CNTs to be uniformly dispersed in an aluminum matrix, the load transfer function is played in the composite material, and the strength of the composite material is improved through the synergistic effect of nano aluminum carbide and carbon nano tubes in the composite material prepared through two-step ball milling.
The invention has the beneficial effects that: the CNTs-Al of the invention4C3the/Al composite material is prepared by adopting a two-step ball milling process, so that the composite material contains both a nanoparticle reinforcing phase and a carbon nanotube fiber reinforcing phase, and the synergistic effect of the nanoparticle reinforcing phase and the carbon nanotube fiber reinforcing phase is greatThe strength of the composite material is greatly improved; the problems of single reinforcing body and non-ideal performance of the traditional single-step ball milling are solved; the CNTs-Al of the invention4C3the/Al composite material has excellent light weight and high strength.
Drawings
FIG. 1 is a process flow diagram of the process of the present invention;
FIG. 2 shows CNTs-Al in the present invention4C3Raman spectrum of the/Al composite material;
FIG. 3 shows CNTs-Al in example 14C3Transmission electron microscope photos of the/Al composite material;
FIG. 4 shows CNTs-Al in example 14C3Vickers hardness histogram of/Al composite material and pure aluminum;
FIG. 5 shows CNTs-Al in example 14C3Tensile property curves of the/Al composite material and pure aluminum.
Detailed Description
The present invention will be further described with reference to the following detailed description, but the scope of the present invention is not limited to the description.
Example 1
The invention provides a CNTs-Al4C3The preparation method of the/Al composite material comprises the following steps;
(1) preparation of Al4C3Al composite powder: placing carbon nanotubes (with purity of 95%, 10 μm), pure aluminum powder (with purity of 99.5%, average particle size of 25 μm) and a certain number of grinding balls in a ball milling tank under inert gas protective atmosphere, wherein the mass of the carbon nanotube powder is 1 wt% of the total mass of the mixed powder, and adding a small amount of stearic acid as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated, and the high-energy ball milling is accumulated for 24 hours to ensure that the carbon nano tube and the pure aluminum powder react to generate the nano Al in situ4C3Particles; thereby obtaining the nano Al-containing4C3A composite powder of particles.
(2) Preparation of CNTs-Al4C3Al composite powder: mixing the carbon nano tube (purity 95%, 10 μm) with the Al-containing nano tube prepared in the step (1)4C3Placing the composite powder of the particles and a certain number of grinding balls in a ball-milling tank under the inert gas protective atmosphere, wherein the mass of the newly added carbon nanotube powder is 1 wt% of the total mass of the composite powder, and adding a small amount of stearic acid as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the ball milling is accumulated for 6 hours; CNTs-Al with uniformly dispersed carbon nanotubes is obtained after ball milling4C3a/Al composite powder.
(3) Pressing and sintering the composite powder: CNTs-Al is processed by a steel die4C3the/Al composite powder is cold-pressed into a cylinder blank with the diameter of 26 multiplied by 1.5 mm at the room temperature under the pressure of 300MPa, and sintered for 4 hours at the temperature of 600 ℃ under the argon environment.
(4) Hot extrusion of the sintered blank: CNTs-Al prepared in the step (3)4C3Heating the Al composite material sintered blank to 450 ℃ in a vacuum or inert gas protective atmosphere heating furnace, and preserving heat for 2 hours until the internal and external temperatures of the ingot blank are uniform; meanwhile, preheating an extrusion cylinder with the internal diameter phi of 28mm and an extrusion die with the internal diameter phi of 5 mm; then assembling an extrusion die and an extrusion cylinder, quickly transferring the hot ingot blank to the extrusion cylinder, and adopting an extrusion ratio of 36:1 to thermally extrude the sintered blank into CNTs-Al with the phi 5 mm4C3a/Al composite bar. The tensile strength and Vickers hardness of the composite material are improved compared with those of pure aluminum, as shown in figure 4, the hardness of the composite material in the embodiment is 82HV, the hardness of the pure aluminum is 63HV, and the hardness of the composite material in the embodiment is improved by 19HV compared with that of the pure aluminum. As shown in FIG. 5, the tensile strength of the composite material in this embodiment is 258MPa, the tensile strength of pure aluminum is 202MPa, and the tensile strength of the composite material in this embodiment is 56MPa higher than that of pure aluminum.
Example 2
(1) Preparation of Al4C3Al composite powder: mixing carbon nanotube (purity 95%, 20 μm) and pure aluminum powder (purity)99.5% with an average particle size of 30 μm) together with a certain number of grinding balls were placed in a ball milling jar under an inert gas atmosphere, wherein the mass of the carbon nanotube powder was 1.5wt.% of the total mass of the mixed powder, and a small amount of stearic acid was added as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated, and the high-energy ball milling is accumulated for 24 hours to ensure that the carbon nano tube and the pure aluminum powder react to generate the nano Al in situ4C3And (3) granules. Thereby obtaining the nano Al-containing4C3A composite powder of particles;
(2) preparation of CNTs-Al4C3Al composite powder: mixing the carbon nano tube (purity 95%, 20 μm) with the Al-containing nano tube prepared in the step (1)4C3Placing the composite powder of the particles and a certain number of grinding balls in a ball-milling tank under the inert gas protective atmosphere, wherein the mass of the newly added carbon nanotube powder is 2 wt% of the total mass of the composite powder, and a small amount of stearic acid is added to serve as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the ball milling is accumulated for 6 hours. CNTs-Al with uniformly dispersed carbon nanotubes is obtained after ball milling4C3a/Al composite powder.
(3) Pressing and sintering the composite powder: CNTs-Al is processed by a steel die4C3the/Al composite powder is cold-pressed into a cylinder blank with the diameter of 26 multiplied by 1.5 mm at the room temperature under the pressure of 300MPa, and sintered for 4 hours at the temperature of 600 ℃ under the argon environment.
(4) Hot extrusion of the sintered blank: CNTs-Al prepared in the step (3)4C3Heating the/Al composite material sintered blank to 450 ℃ in a vacuum or inert gas protective atmosphere heating furnace, and preserving heat for 2 hours until the internal and external temperatures of the ingot blank are uniform; meanwhile, preheating an extrusion cylinder with the internal diameter phi of 28mm and an extrusion die with the internal diameter phi of 5 mm; then assembling an extrusion die and an extrusion cylinder, quickly transferring the hot ingot blank to the extrusion cylinder, and adopting an extrusion ratio of 36:1 to thermally extrude the sintered blank into CNTs-A with phi 5 mml4C3a/Al composite bar.
CNTs-Al prepared in this example4C3The hardness of the/Al composite material is 73HV, and the tensile strength is 243 MPa.
Example 3
(1) Preparation of Al4C3Al composite powder: placing carbon nanotubes (with purity of 95%, 30 μm), pure aluminum powder (with purity of 99.5%, average particle size of 20 μm) and a certain number of grinding balls in a ball milling tank under inert gas protective atmosphere, wherein the mass of the carbon nanotube powder is 2wt.% of the total mass of the mixed powder, and adding a small amount of stearic acid as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated, and the high-energy ball milling is accumulated for 24 hours to ensure that the carbon nano tube and the pure aluminum powder react to generate the nano Al in situ4C3Particles; thereby obtaining the nano Al-containing4C3A composite powder of particles;
(2) preparation of CNTs-Al4C3Al composite powder: mixing the carbon nano tube (purity 95%, 30 μm) with the Al-containing nano tube prepared in the step (1)4C3Placing the composite powder of the particles and a certain number of grinding balls in a ball-milling tank under the inert gas protective atmosphere, wherein the mass of the newly added carbon nanotube powder is 1.5 wt% of the total mass of the composite powder, and adding a small amount of stearic acid as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the ball milling is accumulated for 6 hours. CNTs-Al with uniformly dispersed carbon nanotubes is obtained after ball milling4C3a/Al composite powder.
(3) Pressing and sintering the composite powder: CNTs-Al is processed by a steel die4C3the/Al composite powder is cold-pressed into a cylinder blank with the diameter of 26 multiplied by 1.5 mm at the room temperature under the pressure of 300MPa, and sintered for 4 hours at the temperature of 600 ℃ under the argon environment.
(4) Hot extrusion of the sintered blank: subjecting the product of step (3)Prepared CNTs-Al4C3Heating the/Al composite material sintered blank to 450 ℃ in a vacuum or inert gas protective atmosphere heating furnace, and preserving heat for 2 hours until the internal and external temperatures of the ingot blank are uniform; meanwhile, preheating an extrusion cylinder with the internal diameter phi of 28mm and an extrusion die with the internal diameter phi of 5 mm; then assembling an extrusion die and an extrusion cylinder, rapidly transferring the hot ingot blank to the extrusion cylinder, and hot-extruding the sintered blank into a CNTs-Al4C3/Al composite bar with the phi 5 mm by adopting an extrusion ratio of 36: 1.
CNTs-Al prepared in this example4C3The hardness of the/Al composite material is 66HV, and the tensile strength is 232 MPa.
Comparative examples
(1) Placing carbon nanotubes (with purity of 95%, 10 μm), pure aluminum powder (with purity of 99.5%, average particle size of 25 μm) and a certain number of grinding balls in a ball milling tank under inert gas protection atmosphere, wherein the mass of the carbon nanotube powder is 2.5wt.% of the total mass of the mixed powder, and adding a small amount of stearic acid as a process control agent; the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the above steps are repeated in such a way, and the high-energy ball milling is accumulated for 30 hours.
(2) Pressing and sintering the composite powder: and (3) cold-pressing the composite powder in the step (1) into a phi 26 multiplied by 1.5 mm cylindrical blank at room temperature by using a steel die under the pressure of 300MPa, and sintering for 4 hours at the temperature of 600 ℃ in an argon environment.
(3) Hot extrusion of the sintered blank: heating the composite material sintered blank prepared in the step (2) to 450 ℃ in a vacuum or inert gas protective atmosphere heating furnace, and preserving heat for 2 hours until the internal and external temperatures of the ingot blank are uniform; meanwhile, preheating an extrusion cylinder with the internal diameter phi of 28mm and an extrusion die with the internal diameter phi of 5 mm; then assembling an extrusion die and an extrusion cylinder, rapidly transferring the hot ingot blank to the extrusion cylinder, and hot-extruding the sintered blank into a phi 5 mm composite bar by adopting an extrusion ratio of 36: 1.
The mechanical property test of the composite material obtained by the single-step ball milling shows that the tensile strength is 236MPa and the elongation is 14.3 percent. In example (1), the tensile strength of the composite material prepared by the two-step ball milling is not 258MPa, and the elongation is 19.5%, which shows that the tensile strength and the elongation of the composite material prepared by the two-step ball milling are superior to those of the composite material prepared by the single-step ball milling.
Claims (5)
1. The preparation method of the carbon nanotube composite material is characterized by comprising the following steps:
(1) mixing carbon nanotube powder and aluminum powder and then carrying out ball milling, wherein the mass of the carbon nanotube powder is 1-2 wt% of the total mass of the mixed powder, and the ball milling time is 10-30 h, so as to obtain the Al-containing powder4C3The composite powder of (1);
(2) mixing the carbon nano tube with the composite powder obtained in the step (1), ball-milling for 2-10 h, and uniformly dispersing in a matrix to obtain CNTs-Al4C3A composite powder of/Al; wherein the mass of the newly added carbon nanotube powder is 1-2wt.% of the mass of the composite powder;
(3) CNTs-Al4C3the/Al composite powder is cold-pressed and molded at room temperature and sintered in an argon environment to obtain CNTs-Al4C3Performing hot extrusion on the sintered blank to obtain CNTs-Al4C3a/Al composite material;
the length of the carbon nano tube in the step (1) is 10-30 mu m, the diameter is 20-30 nm, and the particle size of the aluminum powder is 20-30 mu m.
2. The method for producing a carbon nanotube composite material according to claim 1, wherein: the specific process of ball milling in the step (1) is as follows: placing carbon nano tubes, pure aluminum powder and grinding balls in a ball milling tank under the protection of inert gas, and adding stearic acid as a process control agent; wherein the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the high-energy ball milling is accumulated for 10-30 h.
3. The method for preparing a carbon nanotube composite material according to claim 1, wherein the carbon nanotube composite material is prepared by a method comprising a step of mixing the carbon nanotube composite material with a solventIn the following steps: the ball milling in the step (2) comprises the following specific processes: mixing carbon nanotube with nano Al4C3Placing the composite powder of the particles and the grinding ball in a ball milling tank under the protective atmosphere of inert gas, and adding stearic acid as a process control agent; wherein the ball-material ratio is 10:1, and the rotating speed of the ball mill is 250 r/min; in order to reduce the temperature rise of the composite powder in the ball milling process, the ball mill rotates forwards for 30min, then pauses for 30min, then rotates backwards for 30min, and the process is circulated in such a way, and the ball milling is accumulated for 2-10 h.
4. The method for producing a carbon nanotube composite material according to claim 1, wherein: the cold pressing and sintering process of the composite powder in the step (3) comprises the following specific steps: and cold-pressing the composite powder into a blank at room temperature under the pressure of 300MPa, and sintering for 4 hours at the temperature of 600 ℃ under the argon environment.
5. The method for producing a carbon nanotube composite material according to claim 1, wherein: the specific process of hot extrusion in the step (3) is as follows: CNTs-Al4C3Heating the/Al composite material sintered blank to 450 ℃ in a vacuum or inert gas protective atmosphere heating furnace, and preserving heat for 2 hours until the internal and external temperatures of the ingot blank are uniform; simultaneously preheating the extrusion die; the sintered compact was hot extruded into a composite material using an extrusion ratio of 36: 1.
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| CN101956149A (en) * | 2010-10-08 | 2011-01-26 | 昆明理工大学 | Process for preparing carbon nano-tube-enhanced aluminum-based composite material |
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