CN114147214A - Preparation method of carbon nano tube reinforced magnesium-based composite material - Google Patents
Preparation method of carbon nano tube reinforced magnesium-based composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon nanotube reinforced magnesium-based composite material, which is implemented according to the following steps: step 1, weighing carbon nano tube and AZ91 magnesium alloy powder according to mass percentage, and ball-milling and mixing in a conical ball mill to obtain mixed powder; step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry; step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10‑3Vacuum degassing below pa, and tape casting; step 4, placing the blank formed by tape casting in a drying deviceDrying at 550 ℃ for 15-30min through upper and lower drying channels; and 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the material. The invention solves the problem of serious agglomeration phenomenon of CNTs in an alloy matrix in the existing preparation method.
Description
Technical Field
The invention belongs to the technical field of preparation methods of carbon nanotube reinforced magnesium-based composite materials, and particularly relates to a preparation method of a carbon nanotube reinforced magnesium-based composite material.
Background
The magnesium alloy has the advantages of good machinability, easy processing, high specific strength, specific stiffness, light weight, low density and the like, and is widely applied in the fields of new energy vehicles, aerospace, electronic communication, medical appliances and the like. In the application of light-weight engineering, when automobile parts or automobile body plates are manufactured, if magnesium alloy can be used for replacing original high-strength steel or aluminum alloy, the automobile quality is reduced, and great economic benefits can be brought. However, the magnesium alloy has the disadvantages of low tensile strength and hardness, poor wear resistance and the like, and the wide application of the magnesium alloy is limited. The carbon nano tube is a tubular nano-scale graphite crystal. The material has good mechanical property, the tensile strength reaches 50-200GPa, which is 100 times of that of steel, the density is only 1/6 of steel, the elastic modulus is equivalent to that of diamond, and 1TPa can be achieved; at the same time, CNTs have good flexibility, conductivity and heat conductivity. Due to the excellent mechanical and physical properties, the composite material can be used as an ideal reinforcement of a metal-based composite material and is uniformly approved by domestic and foreign scholars.
Domestic and foreign researches show that the grain refinement can be realized and the mechanical property of the magnesium alloy can be improved by adding the reinforcement, and the reinforcing phase materials of the magnesium-based composite material which is researched more mainly comprise SiC particles, crystal whiskers, Al2O3 particles, short fibers, TiC particles, graphite fibers and the like. However, the magnesium-based composite material is limited by the hcp structure of the Mg matrix, has poor plasticity, and particularly, when a reinforcement body with the size of micron or more is adopted, the defects of micron-sized reinforcement phase fracture, failure of an interface between the composite material and the matrix and the like often exist in the composite material. The plasticity is sharply reduced while the strength is improved, and the strength and the plasticity are inverted. Relevant studies show that if the reinforcement is reduced to a nano-scale and uniformly dispersed, the magnesium-based composite material can maintain the plasticity while improving the strength. Therefore, the nano reinforcement is a better choice for improving the toughness of the magnesium-based composite material.
At present, the preparation difficulty of the carbon nanotube reinforced magnesium-based composite material is that the agglomeration phenomenon of CNTs in an alloy matrix is serious, the wettability of the carbon nanotube and a magnesium alloy is poor, and the agglomeration and entanglement often cause air inclusion, generate air holes and other defects; and the carbon nano tube cluster and entanglement convert the one-dimensional reinforced phase into the particle-like reinforced phase, so that the advantage of high length-diameter ratio is lost, and the interfacial stress transfer efficiency is greatly reduced, therefore, the optimization of a good preparation process is necessary to improve the toughness of the CNTs/Mg composite material.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nano tube reinforced magnesium-based composite material, which solves the problem of serious agglomeration phenomenon of CNTs in an alloy matrix in the existing preparation method.
The invention adopts the technical scheme that the preparation method of the carbon nano tube reinforced magnesium-based composite material is implemented according to the following steps:
step 1, weighing carbon nano tube and AZ91 magnesium alloy powder according to mass percentage, and ball-milling and mixing in a conical ball mill to obtain mixed powder;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
step 4, placing the blank formed by tape casting into a drying device, and drying for 15-30min at the temperature of 500-;
and 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the material.
The invention is also characterized in that:
the carbon nano tube is a multi-wall carbon nano tube, the purity is more than 98%, the inner diameter is 5-10nm, the length is 10-20um, the purity of magnesium powder is 99%, and the particle size is 100 um.
In the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h.
The dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the dispersing agent and the leveling agent account for 3% of the mass of the mixed powder.
The alcohol in the step 2 is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank.
The diameters of the grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of the large balls to the small balls is 2: 1.
In the step 3, the aperture of the nanofiltration membrane is 1-2nm, the blank forming speed is 2mm/s and the blank thickness is 2mm in the tape casting process.
The heat treatment temperature in the step 5 is 200 ℃, and the treatment time is 12 h.
And 5, cutting the dried blank into plates of 60mm by 2 mm.
The mass ratio of the carbon nano tubes in the step 1 to the mixed powder is not more than 10%.
The invention has the beneficial effects that:
1. the invention can effectively obtain the carbon nano tube with better dispersity and integrity by dispersing the carbon nano tube.
2. The invention utilizes the tape casting process method to improve the interface bonding property of the carbon nano tube and the magnesium matrix to a certain extent.
3. The CNTs/AZ91 magnesium-based composite material prepared by the method has the advantages of obviously improved tensile strength and toughness.
Drawings
FIG. 1 shows the morphology of CNTs before dispersion in the method for preparing a carbon nanotube reinforced Mg-based composite according to the present invention;
FIG. 2 shows the morphology of the dispersed CNTs in the method for preparing the carbon nanotube reinforced Mg-based composite.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The preparation method of the carbon nanotube reinforced magnesium-based composite material is specifically implemented according to the following steps:
step 1, weighing carbon nano tubes and AZ91 magnesium alloy powder according to mass percentage, and ball-milling and mixing in a conical ball mill to obtain mixed powder, wherein the mass of the carbon nano tubes in the step 1 accounts for no more than 10% of the mass of the mixed powder.
The carbon nano tube is a multi-wall carbon nano tube, the purity is more than 98%, the inner diameter is 5-10nm, the length is 10-20um, the purity of magnesium powder is 99%, and the particle size is 100 um;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry;
the dispersant is specifically: mixing phosphatidylethanolamine, fatty acid polyglycerol and methylpentanol according to a weight ratio of 1: 1.5: 2, mixing, and keeping for 15 days in a dark place, wherein the dispersing agent is used for dispersing the aggregated CNTs;
the leveling agent is specifically as follows: methyl isopropylbenzene, flower hydrocarbon, m-methyl propylbenzene and 2-methyl pentane in the weight ratio of 1: 1.5: 1: 2, mixing, and keeping away from light for 15 days, wherein a leveling agent is used for uniformly distributing the dispersed CNTs in a magnesium matrix, and the leveling agent is used for improving the wettability of the CNTs matrix;
the dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the dispersing agent and the leveling agent account for 3% of the mass of the mixed powder;
the alcohol is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank;
the diameters of stainless steel grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of large balls to small balls is 2: 1;
in the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
the aperture of the nanofiltration membrane is 1-2nm, the speed of forming a blank is 2mm/s in the tape casting process, and the thickness of the blank is 2 mm;
step 4, placing the blank formed by tape casting into a drying device, and drying for 15-30min at the temperature of 500-;
step 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the finished product;
the heat treatment temperature is 200 ℃, and the treatment time is 12 hours;
and cutting the dried blank into plates of 60mm by 2 mm.
Example 1
The preparation method of the carbon nano tube reinforced magnesium-based composite material is implemented according to the following steps:
step 1, preparing 0.5 wt.% of CNTs/AZ91 magnesium-based composite material, weighing 597g of magnesium powder and 3g of CNTs, and ball-milling and mixing in a conical ball mill to obtain mixed powder;
the carbon nano tube is a multi-wall carbon nano tube, the purity is more than 98%, the inner diameter is 5nm, the length is 10um, the purity of magnesium powder is 99%, and the particle size is 100 um;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry; the dispersing agent is used for dispersing the agglomerated CNTs, and the homogenizing agent is used for uniformly distributing the dispersed CNTs in the magnesium matrix and improving the wettability of the CNTs matrix;
the dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the mass of the dispersing agent and the leveling agent is 18 g;
the alcohol is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank;
the diameters of stainless steel grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of large balls to small balls is 2: 1;
in the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
the aperture of the nanofiltration membrane is 1-2nm, the speed of forming a blank is 2mm/s in the tape casting process, and the thickness of the blank is 2 mm;
step 4, placing the blank formed by tape casting into a drying device, and drying for 15min through an upper drying channel and a lower drying channel at 500 ℃;
step 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the finished product;
the heat treatment temperature is 200 ℃, and the treatment time is 12 hours;
and cutting the dried blank into plates of 60mm by 2 mm.
Example 2
The preparation method of the carbon nano tube reinforced magnesium-based composite material is implemented according to the following steps:
step 1, preparing 1.0 wt.% of CNTs/AZ91 magnesium-based composite material, weighing 594g of magnesium powder and 6g of CNTs, and ball-milling and mixing in a conical ball mill to obtain mixed powder;
the carbon nano tube is a multi-wall carbon nano tube, the purity is more than 98%, the inner diameter is 10nm, the length is 20um, the purity of magnesium powder is 99%, and the particle size is 100 um;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry; the dispersing agent is used for dispersing the aggregated CNTs, the leveling agent is used for enabling the dispersed CNTs to be uniformly distributed in the magnesium matrix, and the leveling agent is used for improving the wettability of the CNTs matrix;
the dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the mass of the dispersing agent and the leveling agent is 18 g;
the alcohol is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank;
the diameters of stainless steel grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of large balls to small balls is 2: 1;
in the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
the aperture of the nanofiltration membrane is 2nm, the speed of forming a blank is 2mm/s in the tape casting process, and the thickness of the blank is 2 mm;
step 4, placing the blank formed by tape casting into a drying device, and drying for 30min through an upper drying channel and a lower drying channel at 550 ℃;
step 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the finished product;
the heat treatment temperature is 200 ℃, and the treatment time is 12 hours;
and cutting the dried blank into plates of 60mm by 2 mm.
Example 3
The preparation method of the carbon nano tube reinforced magnesium-based composite material is implemented according to the following steps:
step 1, preparing 1.5 wt.% of CNTs/AZ91 magnesium-based composite material, weighing 591g of magnesium powder and 9g of CNTs, and ball-milling and mixing in a conical ball mill to obtain mixed powder;
the carbon nano tube is a multi-wall carbon nano tube, the purity is more than 98%, the inner diameter is 7nm, the length is 15um, the purity of magnesium powder is 99%, and the particle size is 100 um;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry; the dispersing agent is used for dispersing the aggregated CNTs, the leveling agent is used for enabling the dispersed CNTs to be uniformly distributed in the magnesium matrix, and the leveling agent is used for improving the wettability of the CNTs matrix;
the dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the mass of the dispersing agent and the leveling agent is 18 g;
the alcohol is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank;
the diameters of stainless steel grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of large balls to small balls is 2: 1;
in the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
the aperture of the nanofiltration membrane is 1.5nm, the speed of forming a blank is 2mm/s in the tape casting process, and the thickness of the blank is 2 mm;
step 4, placing the blank formed by tape casting into a drying device, and drying for 30min through an upper drying channel and a lower drying channel at 520 ℃;
step 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the finished product;
the heat treatment temperature is 200 ℃, and the treatment time is 12 hours;
and cutting the dried blank into plates of 60mm by 2 mm.
Example 4
The preparation method of the carbon nano tube reinforced magnesium-based composite material is implemented according to the following steps:
step 1, preparing 2.0 wt.% of CNTs/AZ91 magnesium-based composite material, weighing 498g of magnesium powder and 12g of CNTs, and ball-milling and mixing in a conical ball mill to obtain mixed powder;
the carbon nano tube is a multi-wall carbon nano tube, the purity is more than 98%, the inner diameter is 7nm, the length is 15um, the purity of magnesium powder is 99%, and the particle size is 100 um;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry; the dispersing agent is used for dispersing the aggregated CNTs, the leveling agent is used for enabling the dispersed CNTs to be uniformly distributed in the magnesium matrix, and the leveling agent is used for improving the wettability of the CNTs matrix;
the dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the mass of the dispersing agent and the leveling agent is 18 g;
the alcohol is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank;
the diameters of stainless steel grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of large balls to small balls is 2: 1;
in the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
the aperture of the nanofiltration membrane is 1.5nm, the speed of forming a blank is 2mm/s in the tape casting process, and the thickness of the blank is 2 mm;
step 4, placing the blank formed by tape casting into a drying device, and drying for 30min through an upper drying channel and a lower drying channel at 520 ℃;
step 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the finished product;
the heat treatment temperature is 200 ℃, and the treatment time is 12 hours;
and cutting the dried blank into plates of 60mm by 2 mm.
Example 5
The preparation method of the carbon nano tube reinforced magnesium-based composite material is implemented according to the following steps:
step 1, weighing magnesium powder with the purity of 99 percent and the particle size of 100um, and ball-milling the magnesium powder in a conical ball mill;
step 2, adding a dispersing agent, a homogenizing agent and alcohol in the step 1, and continuing ball milling to obtain mixed slurry;
the dispersing agent and the leveling agent are mixed and added according to the mass ratio of 2:1, and the mass of the dispersing agent and the leveling agent is 18 g;
the alcohol is over the grinding balls and the materials, and the volume of the alcohol does not exceed 1/2 of the ball milling tank;
the diameters of stainless steel grinding balls in the ball-milling tank are respectively 5mm and 12mm, and the number ratio of large balls to small balls is 2: 1;
in the step 1 and the step 2, the rotating speed of the conical ball mill is 300r/min, and the ball milling time is 10 h;
step 3, filtering the mixed slurry in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry in a vacuum degree of 9 multiplied by 10-3Vacuum degassing below pa, and tape casting;
the aperture of the nanofiltration membrane is 1.5nm, the speed of forming a blank is 2mm/s in the tape casting process, and the thickness of the blank is 2 mm;
step 4, placing the blank formed by tape casting into a drying device, and drying for 30min through an upper drying channel and a lower drying channel at 520 ℃;
step 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the finished product;
the heat treatment temperature is 200 ℃, and the treatment time is 12 hours;
and cutting the dried blank into plates of 60mm by 2 mm.
FIG. 2 is a high power SEM observation of the morphology of dispersed carbon nanotubes, which clearly shows that CNTs are elongated and intertwined, indicating that CNTs are significantly dispersed after ball milling and chemical dispersion.
Table 1 shows the room temperature tensile property test results of CNTs/AZ91 composite materials with different CNTs contents
It is found by comparing example 5 with examples 1 to 4 that the tensile strength, the reduction of area and the elongation of examples 1 to 4 are superior to those of example 5, wherein the mechanical properties of example 3 are most excellent, the tensile strength reaches 190MPa, and is improved by about 24% compared with example 5.
Claims (10)
1. The preparation method of the carbon nanotube reinforced magnesium-based composite material is characterized by comprising the following steps:
step 1, weighing carbon nano tubes and AZ91 magnesium alloy powder according to mass percentage, and ball-milling and mixing the carbon nano tubes in a conical ball mill to obtain mixed powder;
step 2, adding a dispersing agent, a homogenizing agent and alcohol into the mixed powder in the step 1, and continuing ball milling to obtain mixed slurry;
3, filtering the mixed slurry obtained in the step 2 by using a nanofiltration membrane, and then filtering the mixed slurry under the vacuum degree of 9 x 10-3Vacuum degassing below pa, and tape casting;
step 4, placing the blank formed by tape casting into a drying device, and drying for 15-30min at the temperature of 500-;
and 5, cutting the blank dried in the step 4, and then placing the cut blank in a box-type resistance furnace for homogenization heat treatment to obtain the material.
2. The method of claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes having a purity of greater than 98%, an inner diameter of 5-10nm, a length of 10-20um, a purity of 99% of magnesium powder, and a particle size of 100 um.
3. The method for preparing a carbon nanotube reinforced magnesium-based composite material as claimed in claim 1, wherein the rotation speed of the ball cone mill in step 1 and step 2 is 300r/min, and the ball milling time is 10 h.
4. The method for preparing a carbon nanotube reinforced magnesium-based composite material as claimed in claim 1, wherein the dispersing agent and the leveling agent are mixed and added in a mass ratio of 2:1, and the dispersing agent and the leveling agent account for 3% of the mass of the mixed powder.
5. The method for preparing carbon nanotube reinforced Mg-based composite material as claimed in claim 1, wherein the alcohol in step 2 is higher than the milling balls and the materials and has a volume not exceeding 1/2 of the ball milling pot.
6. The method for preparing a carbon nanotube reinforced magnesium-based composite material as claimed in claim 1, wherein the diameters of the grinding balls in the ball mill pot are 5mm and 12mm, respectively, and the number ratio of the large balls to the small balls is 2: 1.
7. The method for preparing a carbon nanotube reinforced magnesium-based composite material as claimed in claim 1, wherein the pore diameter of the nanofiltration membrane in the step 3 is 1-2nm, the speed of forming the blank during tape casting is 2mm/s, and the thickness of the blank is 2 mm.
8. The method of claim 1, wherein the heat treatment temperature in the step 5 is 200 ℃ and the treatment time is 12 hours.
9. The method of claim 1, wherein the step 5 comprises cutting the dried blank into sheets of 60mm by 2 mm.
10. The method for preparing a carbon nanotube reinforced magnesium-based composite material as claimed in claim 1, wherein the mass of the carbon nanotubes in the step 1 is not more than 10% of the mass of the mixed powder.
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Cited By (2)
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| CN114682798A (en) * | 2022-03-31 | 2022-07-01 | 贵州航天风华精密设备有限公司 | Forming method of magnesium-based carbon nanotube composite material |
| CN114990370A (en) * | 2022-05-11 | 2022-09-02 | 山东商业职业技术学院 | High-biocompatibility magnesium alloy composite material and preparation method thereof |
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