CN113308630A - In-situ CNTs @ Ti hybrid reinforced aluminum matrix composite and preparation method thereof - Google Patents
In-situ CNTs @ Ti hybrid reinforced aluminum matrix composite and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4417—Methods specially adapted for coating powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses an in-situ CNTs @ Ti hybrid reinforced aluminum-based composite material and a preparation method thereof, and relates to the field of composite materials. The invention adopts a gas-permeable phase deposition method (CVD) to synthesize and distribute the Ti particles on the surface of the spherical Ti particles in situ, the tube diameters of the Ti particles are uniform and pureCNTs with high degree and good crystallinity are dispersed to an Al matrix through mechanical ball milling to obtain uniformly dispersed CNTs @ Ti/Al composite powder, and the composite material is prepared by Spark Plasma Sintering (SPS). The method for preparing the CNTs @ Ti hybrid reinforced phase by using the in-situ vapor deposition method is combined with a simple low-speed short-time ball milling method, so that the CNTs can be uniformly dispersed in an Al matrix, and Ti and the Al matrix react to generate TiAl under the action of high temperature and long time in the sintering process3CNTs and Al or Ti to form nanophase Al4C3And TiC, good interface bonding is formed, and the tensile strength and the ductility of the composite material are improved.
Description
Technical Field
The invention relates to an in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite and a preparation method thereof, belonging to the technical field of preparation of multiphase hybrid reinforced aluminum matrix composites.
Background
Aluminum metal has many advantages such as low density, good plasticity, good corrosion resistance, etc., and is widely used. However, pure aluminum and aluminum alloys generally have low strength, and development of aluminum-based composites is receiving much attention. The carbon nano tube reinforced aluminum-based composite material is expected to have the characteristics of light weight, high strength, good plasticity, good corrosion resistance and the like, and has good application prospects in the aspects of aerospace, precision instruments, transportation and the like. The ability of CNTs to fully exploit the previous properties of individual CNTs is a prerequisite for their improved overall performance of composites, which requires that the CNTs be sufficiently uniformly dispersed in the matrix. However, CNTs have Van der Waals force, nano-scale diameter and large specific surface area, and are easy to agglomerate in a metal composite material matrix, so that the strengthening effect is reduced. In addition, the poor wettability between CNTs and metals results in poor interfacial bonding of the composite material, which affects the properties of the composite material.
According to the difference of CNTs addition source, the method is divided into an external addition method and an internal in-situ generation method. The external addition method is to uniformly disperse the CNTs in a matrix to a certain extent by methods such as high-speed ball milling, casting or surface modification of the CNTs, and has the defects of high energy, high temperature or surface modification which damages the complete structure of the CNTs to a certain extent, weakens the strengthening effect of the CNTs and has limited dispersing capacity. Compared with an external method, the CNTs method generated by in-situ compounding is characterized in that chemical precipitation and deposition and gas cracking in-situ generation are utilized on a metal matrix, material pollution is avoided, the wettability of the matrix and an enhanced phase is improved, the bonding strength of an interface is improved, and meanwhile, the quantity and distribution of the CNTs can be effectively regulated and controlled by controlling process parameters. In-situ synthesis saves a separate preparation of a reinforcing phase, and reduces the preparation cost of the material. The in situ generation of CNTs reinforced metal matrix composites is now of increasing interest to researchers.
At present, with the higher requirements of industrial development on the performance of the composite material, the multiphase hybrid reinforced phase gradually replaces a single reinforced phase to reinforce the metal matrix composite material, and the multiphase hybrid reinforced body can make up for each other and perform synergistic reinforcement to obviously improve the performance of the composite material. Li and the like grow carbon nano tubes on the surfaces of SiC particles by a chemical vapor deposition method to prepare a novel SiCp-CNTs hybrid reinforcement, and the SiCp-CNTs hybrid reinforcement is uniformly dispersed in an aluminum matrix by a ball milling method. The results show that the elasticity modulus of the SiCp-CNTs/Al composite material reaches 93GPa, and the tensile strength is 202MPa, which is mainly because the CNTs are uniformly dispersed in the matrix by the aid of SiC and form a well-combined interface with the matrix. Based on the research, Li and the like further research the influence of the SiC particle size on the microstructure and the mechanical property of the SiCp-CNTs/6061Al composite material. When the size of SiCp is 7 mu m, the composite material has good comprehensive performance. Pure Ti powder is added into an aluminum matrix and reacts with aluminum to form an A1-Ti intermetallic compound dispersed phase, and the A1-Ti intermetallic compound is a high-temperature structural material and has the characteristics of high elastic modulus, high melting point, high temperature, high strength and the like. On the basis, the CNTs @ Ti hybrid reinforced aluminum matrix composite is prepared on the surface of Ti particles through in-situ synthesis of CNTs.
Disclosure of Invention
The invention aims to provide an in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite, which not only has the special excellent performance of a metal matrix composite, but also has the unique characteristics of low density, light weight, high strength and the like, has important application prospects in the aspects of aerospace, precision instruments, transportation and the like, and comprises a spherical aluminum matrix and a hybrid reinforced phase, wherein the hybrid reinforced phase is CNTs @ Ti, the particle size of the spherical Ti is 1-25 mu m, and the particle size of the spherical aluminum matrix is 20-30 mu m.
Preferably, the total mass fraction of the spherical aluminum matrix and the hybrid reinforced phase CNTs @ Ti is 100%, wherein the mass fraction of the spherical aluminum matrix is 80-96 wt%, and the mass fraction of the hybrid reinforced phase CNTs @ Ti is 4-20 wt%.
The invention also aims to provide a preparation method of the in-situ CNTs @ Ti hybrid reinforced aluminum-based composite material, which solves the defect of uneven distribution of CNTs in the conventional hybrid reinforced aluminum-based composite material, improves the interface bonding performance, and specifically comprises the following steps:
(1) mixing Me (NO)3)2·6H2Adding O and spherical Ti powder into deionized water, and stirring to obtain Me (NO)3)2·6H2Dissolving O completely, and gradually dropping NaOH and Me (NO)3)2·6H2Fully reacting O, continuously stirring, standing to obtain Me (OH)2the/Ti binary colloid, wherein Me is Ni and Co.
(2) The Me (OH) obtained in the step (1)2Drying the/Ti binary colloid, and then putting the dried/Ti binary colloid into a tubular furnace to be calcined to obtain the catalystAnd MeO, introducing argon and hydrogen, heating, reducing, and coating the nano Me catalyst on the surface of the spherical Ti particles.
(3) C is to be2H2Introducing Ar into a tube furnace simultaneously for vapor deposition reaction to crack C on the surface of Ti particles2H2In-situ synthesis of CNTs, the CNTs are uniformly dispersed on the surface of spherical titanium particles, the tube diameter is uniform, the crystallinity is good, and H is finally turned off2And continuously calcining in argon atmosphere to remove TiH2And then cooling to room temperature to obtain the CNTs @ Ti hybrid reinforcement.
(4) Dispersing CNTs @ Ti into spherical Al powder by adopting mechanical ball milling to obtain composite powder, then sintering the composite powder by using discharge plasma to prepare a composite material, further processing the composite material by hot extrusion, and densifying the composite material to obtain the CNTs @ Ti hybrid reinforced aluminum-based composite material.
Preferably, the purity of the spherical aluminum powder is more than 99.95 percent, and the particle size is 20-30 mu m; the purity of the spherical titanium powder is more than 99.99 percent, and the particle size is 1-25 mu m; me (NO)3)2·6H2O is analytically pure.
Preferably, Me (NO) is used in step (1) of the present invention3)2·6H2The mass ratio of the O to the Ti powder is 0.07-0.5: 3.
Preferably, in the step (1) of the invention, the concentration of NaOH is 0.1-0.5 mol/L, the continuous stirring time is 1-4 h, and the standing time is 12-24 h.
Preferably, the drying conditions in step (2) of the present invention are: drying for 12-24 h in a vacuum drying oven at the temperature of 80-120 ℃, wherein the calcining condition is as follows: calcining for 2-4h at 400-500 ℃, wherein the reduction reaction conditions are as follows: reducing for 2h at the temperature of 430-550 ℃.
Preferably, the conditions of the vapor deposition reaction in step (3) of the present invention are: reducing at 500-600 deg.c for 30-60 min; removal of TiH2The conditions of (a) are as follows: calcining at 450-500 deg.C for 2-4h, wherein, C2H2And the volume ratio of Ar to Ar is 15: 1-35: 1.
Preferably, the mechanical ball milling process of the present invention comprises the following steps:
(1) and (2) filling the mixed reinforcing phase of Al powder and CNTs @ Ti into a glove box to prepare powder, pouring the Al powder and the CNTs @ Ti into a ball milling tank, wherein the mass ratio of the composite powder to the steel ball is 10:1-20:1, fully filling high-purity argon, sealing the high-purity argon, and preventing the aluminum powder from being oxidized.
(2) Placing the mixture into a ball mill, and stopping ball milling for 15-30 min at the ball milling speed of 150-200r/min to avoid damaging the structure of the CNTs by high-speed ball milling; taking out the CNTs @ Ti/Al composite powder in an argon environment in a glove box.
Preferably, the conditions of spark plasma sintering according to the present invention are: the temperature is raised from the room temperature, the sintering temperature is 580-600 ℃, the temperature is kept for 40-50 min, and the pressure used in the sintering process is 30-50 MPa.
The invention has the beneficial effects that:
(1) according to the invention, CNTs (carbon nanotubes @ Ti powder) which are uniformly dispersed, uniform in pipe diameter and good in crystallinity are obtained on the surfaces of spherical titanium particles by taking Ni and Co as catalysts and acetylene as a carbon source gas; CNTs are uniformly dispersed on the surface of an Al matrix only by simple ball milling and taking Ti particles as a medium, no process control agent is used, and the complete structure of the CNTs is protected to a certain extent by cold welding generated in the ball milling process, so that the excellent performance of the CNTs is fully utilized; the uniformly dispersed CNTs @ Ti/Al mixed powder lays a good foundation for preparing composite materials (CNTs @ Ti/Al).
(2) After the CNTs @ Ti/Al mixed powder is sintered by SPS, a second phase TiAl which is dispersed relatively is formed in the CNTs @ Ti/Al composite material3A layer that acts as a pinning for the CNTs; in addition, in-situ grown nanophase TiC and Al are found at the interface4C3Thereby obtaining a large-area tightly-combined interface; the smaller the Ti particle diameter, the more easily TiAl is produced3The more obvious the strengthening effect, the tensile strength and the elongation of the 1-micron CNTs @ Ti hybrid reinforced phase reinforced aluminum matrix composite can reach 243MPa and more than 10 percent respectively.
(3) By changing the content of CNTs @ Ti, the CNTs @ Ti mixed reinforcing phase of 16wt.% is added, the tensile property of the CNTs @ Ti/Al composite material can reach 284MPa, the composite material has the elongation of about 10 percent and good comprehensive mechanical property, mainly because more second phases are generated to lock evenly dispersed CNTs on the interface of the composite material, the load of the CNTs is effectively exerted, in addition, the Olympic mechanism effect and the second phase dispersion strengthening are well exerted, and the comprehensive strengthening effect is achieved.
Drawings
FIG. 1 is a process flow diagram of the process of the present invention;
FIG. 2 is an SEM image of a CNTs @ Ti hybrid mixed powder obtained in example 1;
FIG. 3 is a transmission electron micrograph of the 12wt.% CNTs @ Ti/Al composite of example 3.
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
The raw materials used in this example were: pure aluminum powder (purity >99.95%, particle size 25 μm), titanium powder (purity >99.9 wt%; particle size 20 μm, spherical), wherein the pure aluminum powder is 96% by weight, and the hybrid reinforced phase CNTs @ Ti is 4% by weight, the specific steps are as follows:
(1) plating uniform 1.5wt.% catalyst metal Co particles on the Ti powder surface by a deposition-precipitation method; mixing Co (NO)3)2·6H2Placing O and Ti powders in a beaker containing deionized water, wherein Me (NO)3)2·6H2The mass of O is 0.2221g, and the mass of Ti powder is 3 g; then Co (NO)3)2·6H2Stirring by a magnetic stirrer to completely dissolve O in the deionized water; gradually dropping 0.1mol/L NaOH and Co (NO) into the beaker3)2·6H2Fully reacting O, continuously stirring for 1h, standing for 24h to obtain Co (OH)2a/Ti binary colloid.
(2) Placing the static binary colloid in a suction filter for suction filtration, and drying the obtained powder in a vacuum drying oven at 80 ℃ for 24 hours; obtaining dry Co (OH)2Calcining Ti in a tube furnace at 460 ℃ for 4h to obtain a catalyst CoO, introducing argon and hydrogen to increase the temperature to 480 ℃ for reduction for 2h, and reducing the CoO into Co catalyst particlesCoating the nano Co catalyst on the surface of the spherical Ti particles; subsequently, the temperature is increased to 550 ℃ continuously according to V (Ar): C2H2) Ratio of = 30:12H2Introducing Ar into the tube furnace gas phase deposition reaction for 50min, synthesizing CNTs on the surface of Ti particles in situ, and finally turning off H2And continuously calcining at 450 ℃ for 4h in an argon environment to remove TiH2And then cooling to room temperature to obtain the CNTs @ Ti hybrid reinforcement body, wherein an SEM image of the CNTs @ Ti hybrid reinforcement body is shown in figure 2, and the CNTs on the surface of Ti particles are uniform in pipe diameter, uniform in direction and uniform in dispersion and wrap the Ti particles.
(3) The Al powder and the CNTs @ Ti mixed reinforced phase are filled in a glove box to be prepared into powder; pouring Al powder and CNTs @ Ti into a ball milling tank, wherein the total mass is 30 g; the mass ratio of the composite powder to the steel ball (diameter is 10 mm) is 10:1, the composite powder and the steel ball are filled with high-purity argon, and the composite powder and the steel ball are sealed to prevent aluminum powder from being oxidized; then putting the powder into a ball mill, avoiding overheating aluminum powder due to long-time ball milling, stopping ball milling for 15min, wherein the ball milling speed is 200r/min, and avoiding damaging the structure of the CNTs by high-speed ball milling; taking out the CNTs @ Ti/Al composite powder in an argon environment in a glove box.
(4) Preparing a blocky composite material from the prepared CNTs-Ti/Al composite powder by SPS sintering; the diameter of the die used in the experiment is 26.4mm, the temperature is raised from room temperature in the sintering process, the sintering temperature is 590 ℃, the temperature is kept for 40min, and the pressure used in the sintering process is 50 MPa; after cooling, the resultant was taken out to obtain a cylindrical block composite material having a diameter of 26 mm.
And (3) analyzing an experimental result: at room temperature, the tensile mechanical property and the micro vickers hardness of the aluminum-based composite material are tested, and the tensile strength and the elongation of the composite material reach 162 +/-4 MPa and 70.99HV respectively.
Example 2
The raw materials used in this example were: pure aluminum powder (purity >99.95%, particle size 25 μm), titanium powder (purity >99.9 wt%; particle size 10 μm, spherical), wherein the pure aluminum powder is 92% by weight, and the hybrid reinforced phase CNTs @ Ti is 8% by weight, the specific steps are as follows:
(1) by depositing-precipitating on Ti powderThe end surface was plated with uniform 0.5wt.% catalyst metal Ni particles; mixing Ni (NO)3)2·6H2Placing O and Ti powders in a beaker containing deionized water, wherein Ni (NO)3)2·6H2The mass of O is 0.74g, and the mass of Ti powder is 3 g; then Ni (NO)3)2·6H2Stirring by a magnetic stirrer to completely dissolve O in the deionized water; gradually dropping 0.4mol/L NaOH and Ni (NO) into the beaker3)2·6H2Fully reacting O, continuously stirring for 1h, standing for 24h to obtain Ni (OH)2a/Ti binary colloid.
(2) Then placing the static binary colloid in a suction filter for suction filtration, and drying the obtained powder in a vacuum drying oven at 120 ℃ for 12 hours; obtaining dried Ni (OH)2Putting Ti in a tube furnace at 480 ℃, calcining for 3h to obtain a catalyst NiO, introducing argon and hydrogen to increase the temperature to 550 ℃, reducing for 2h, and reducing the NiO into Ni catalyst particles; subsequently, the temperature is increased further to 600 ℃ in the range of V (Ar): C2H2) Ratio of = 30:12H2Introducing Ar into the tube furnace gas phase deposition reaction for 30min, synthesizing CNTs on the surface of Ti particles in situ, and finally turning off H2And continuously calcining at 500 ℃ for 2h in an argon environment to remove TiH2And then cooling to room temperature to obtain the CNTs @ Ti hybrid reinforcement.
(3) The Al powder and the CNTs @ Ti mixed reinforced phase are filled in a glove box to be prepared into powder; pouring Al powder and CNTs @ Ti into a ball milling tank, wherein the total mass is 30 g; the mass ratio of the composite powder to the steel ball (diameter is 10 mm) is 10:1, the composite powder and the steel ball are filled with high-purity argon, and the composite powder and the steel ball are sealed to prevent aluminum powder from being oxidized; then putting the powder into a ball mill, avoiding overheating aluminum powder due to long-time ball milling, stopping ball milling for 15min, wherein the ball milling speed is 200r/min, and avoiding damaging the structure of the CNTs by high-speed ball milling; taking out the CNTs @ Ti/Al composite powder in an argon environment in a glove box.
(4) Preparing a blocky composite material from the prepared CNTs @ Ti/Al composite powder by SPS sintering; the diameter of the die used in the experiment is 26.4mm, the temperature is raised from room temperature in the sintering process, the sintering temperature is 580 ℃, the temperature is kept for 50min, and the pressure used in the sintering process is 30 MPa; after cooling, the resultant was taken out to obtain a cylindrical block composite material having a diameter of 26 mm.
And (3) analyzing an experimental result: at room temperature, the tensile mechanical property and the elongation of the aluminum matrix composite material are tested, and the tensile strength and the micro Vickers hardness of the composite material reach 200 +/-2 MPa and 81.17HV respectively.
Example 3
The raw materials used in this example were: pure aluminum powder (purity >99.95%, particle size 25 μm), particle size 1 μm, spherical), 30g in total, wherein the weight ratio of the pure aluminum powder is 88%, the weight percentage of the hybrid reinforced phase CNTs @ Ti is 12%, and the specific steps are as follows:
(1) plating uniform catalyst metal Ni particles on the surface of Ti powder by a deposition-precipitation method; mixing Ni (NO)3)2·6H2Placing O and Ti powders in a beaker containing deionized water, wherein Ni (NO)3)2·6H2The mass of O is 0.2228g, and the mass of Ti powder is 3 g; then Ni (NO)3)2·6H2Stirring by a magnetic stirrer to completely dissolve O in the deionized water; gradually dripping 0.3mol/L NaOH and Ni (NO) into the beaker3)2·6H2Fully reacting O, continuously stirring for 1h, standing for 24h to obtain Ni (OH)2a/Ti binary colloid.
(2) Then placing the static binary colloid in a suction filter for suction filtration, and drying the obtained powder in a vacuum drying oven at 100 ℃ for 18 h; obtaining dried Ni (OH)2Placing Ti in a tube furnace at 400 ℃, calcining for 4h to obtain a catalyst NiO, introducing argon and hydrogen to increase the temperature to 430 ℃ for reduction for 2h, and reducing the NiO into Ni catalyst particles; subsequently, the temperature is increased further to 500 ℃ in the range of V (Ar): C2H2) Ratio of = 30:12H2Introducing Ar into the tube furnace gas phase deposition reaction for 60min, synthesizing CNTs on the surface of Ti particles in situ, and finally turning off H2And continuously calcining at 480 ℃ for 3h in an argon environment to remove TiH2And then cooling to room temperature to obtain the CNTs @ Ti hybrid reinforcement.
(3) The Al powder and the CNTs @ Ti mixed reinforced phase are filled in a glove box to be prepared into powder; pouring Al powder and CNTs @ Ti into a ball milling tank, wherein the total mass is 30 g; the mass ratio of the composite powder to the steel ball (diameter is 10 mm) is 10:1, the composite powder and the steel ball are filled with high-purity argon, and the composite powder and the steel ball are sealed to prevent aluminum powder from being oxidized. Then putting the powder into a ball mill, avoiding overheating aluminum powder due to long-time ball milling, stopping ball milling for 15min, wherein the ball milling speed is 200r/min, and avoiding damaging the structure of the CNTs by high-speed ball milling; taking out the CNTs @ Ti/Al composite powder in an argon environment in a glove box, and then adding Al powder to the powder, wherein the total amount of the powder is 30 g.
(4) Preparing a blocky composite material from the prepared CNTs @ Ti/Al composite powder by SPS sintering; the diameter of the die used in the experiment is 26.4mm, the temperature is raised from room temperature in the sintering process, the sintering temperature is 590 ℃, the temperature is kept for 45min, and the pressure used in the sintering process is 40 MPa; cooling and taking out to obtain a cylindrical block composite material with the diameter of 26mm, wherein a transmission electron microscope picture of the block composite material is shown in figure 3, and a second phase TiAl can be seen from the picture3The CNTs are locked at the interface, and in addition, nanophase Al is also arranged4C3And TiC, suggesting that the composite has a good interface.
And (3) analyzing an experimental result: at room temperature, the tensile mechanical property and the micro Vickers hardness of the aluminum matrix composite material are tested, and the tensile strength and the elongation of the composite material reach 246 +/-3 MPa and 108.63HV respectively.
Example 4
The raw materials used in this example were: pure aluminum powder (purity >99.95%, particle size 25 μm), titanium powder (purity >99.9 wt%; particle size 1 μm, spherical), 30g in total, wherein the weight ratio of pure aluminum powder is 84%, the weight percentage of hybrid reinforced phase CNTs @ Ti is 16%, and the concrete steps are as follows:
(1) the Ti powder surface was coated with uniform 1.5wt% catalyst metal Co particles by a deposition-precipitation method. Mixing Co (NO)3)2·6H2Placing O and Ti powders in a beaker containing deionized water, wherein Co (NO)3)2·6H2The mass fraction of O is 0.2962g, and the mass of Ti powder is 3 g; then Co (NO)3)2·6H2The O is stirred by a magnetic stirrerFully dissolving in deionized water; gradually dropping 0.5mol/L NaOH and Co (NO) into the beaker3)2·6H2Fully reacting O, continuously stirring for 1h, standing for 24h to obtain Co (OH)2a/Ti binary colloid.
(2) Then placing the static binary colloid in a suction filter for suction filtration, and drying the obtained powder in a vacuum drying oven at 110 ℃ for 16 h; obtaining dry Co (OH)2Placing Ti in a tube furnace at 500 ℃, calcining for 2h to obtain a catalyst CoO, then introducing argon and hydrogen to increase the temperature to 450 ℃ for reduction for 2h, and reducing the CoO into Co catalyst particles; subsequently, the temperature is increased further to 600 ℃ in the range of V (Ar): C2H2) Ratio of = 30:12H2Introducing Ar into the tube furnace gas phase deposition reaction for 30min, synthesizing CNTs on the surface of Ti particles in situ, and finally turning off H2And continuously calcining at 460 ℃ for 4h in an argon environment to remove TiH2And then cooling to room temperature to obtain the CNTs @ Ti hybrid reinforcement.
(3) The Al powder and the CNTs @ Ti mixed reinforced phase are filled in a glove box to be prepared into powder; al powder and CNTs @ Ti are poured into a ball milling tank, and the total mass is 30 g. The mass ratio of the composite powder to the steel ball (diameter is 10 mm) is 10:1, the composite powder and the steel ball are filled with high-purity argon, and the composite powder and the steel ball are sealed to prevent aluminum powder from being oxidized; and then putting the powder into a ball mill, avoiding overheating the aluminum powder due to long-time ball milling, stopping ball milling for 15min, wherein the ball milling speed is 200r/min, and avoiding damaging the structure of the CNTs by high-speed ball milling. Taking out the CNTs @ Ti/Al composite powder in an argon environment in a glove box, and then adding Al powder to the powder, wherein the total amount of the powder is 30 g.
(4) Preparing a blocky composite material from the prepared CNTs-Ti/Al composite powder by SPS sintering; the diameter of the die used in the experiment is 26.4mm, the temperature is raised from room temperature in the sintering process, the sintering temperature is 590 ℃, the temperature is kept for 55min, and the pressure used in the sintering process is 50 MPa; after cooling, the resultant was taken out to obtain a cylindrical block composite material having a diameter of 26 mm.
And (3) analyzing an experimental result: at room temperature, the tensile mechanical property and the micro vickers hardness of the aluminum-based composite material are tested, and the tensile strength and the elongation of the composite material reach 280 +/-4 MPa and 168.27HV respectively.
Claims (10)
1. An in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite is characterized by comprising a spherical aluminum matrix and a hybrid reinforced phase, wherein the hybrid reinforced phase is CNTs @ Ti.
2. The in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite as claimed in claim 1, wherein: the total mass fraction of the spherical aluminum matrix and the hybrid reinforced phase CNTs @ Ti is 100%, wherein the mass fraction of the spherical aluminum matrix is 80-96 wt%, and the mass fraction of the hybrid reinforced phase CNTs @ Ti is 4-20 wt%.
3. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material as recited in claim 1, is characterized by comprising the following steps:
(1) mixing Me (NO)3)2·6H2Adding O and spherical Ti powder into deionized water, and stirring to obtain Me (NO)3)2·6H2Dissolving O completely, and gradually dropping NaOH and Me (NO)3)2·6H2Fully reacting O, continuously stirring, standing to obtain Me (OH)2the/Ti binary colloid is prepared from Me, Co and Ni;
(2) the Me (OH) obtained in the step (1)2Drying the/Ti binary colloid, then putting the dried/Ti binary colloid into a tubular furnace to calcine the dried/Ti binary colloid to obtain a catalyst MeO, then introducing argon and hydrogen to heat the catalyst to reduce the catalyst, and coating the nano Me catalyst on the surface of the spherical Ti particles;
(3) c is to be2H2Introducing Ar into a tube furnace simultaneously for vapor deposition reaction to crack C on the surface of Ti particles2H2In situ synthesis of CNTs, and finally turning off H2And continuously calcining in argon atmosphere to remove TiH2Then cooling to room temperature to obtain a CNTs @ Ti hybrid reinforcement;
(4) dispersing CNTs @ Ti into spherical Al powder by adopting mechanical ball milling to obtain composite powder, then sintering the composite powder by using discharge plasma to prepare a composite material, further processing the composite material by hot extrusion, and densifying the composite material to obtain the CNTs @ Ti hybrid reinforced aluminum-based composite material.
4. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, is characterized in that: the purity of the spherical aluminum powder is more than 99.95 percent, and the particle size is 20-30 mu m; the purity of the spherical titanium powder is more than 99.99 percent, and the particle size is 1-25 mu m; me (NO)3)2·6H2O is analytically pure.
5. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, is characterized in that: me (NO) in step (1)3)2·6H2The mass ratio of the O to the Ti powder is 0.07-0.5: 3.
6. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, is characterized in that: in the step (1), the concentration of NaOH is 0.1-0.5 mol/L, the continuous stirring time is 1-4 h, and the standing time is 12-24 h.
7. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, is characterized in that: the drying conditions in the step (2) are as follows: drying for 12-24 h in a vacuum drying oven at the temperature of 80-120 ℃, wherein the calcining condition is as follows: calcining for 2-4h at 400-500 ℃, wherein the reduction reaction conditions are as follows: reducing for 2h at the temperature of 430-550 ℃.
8. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, is characterized in that: the conditions of the gas phase deposition reaction in the step (3) are as follows: the synthesis time is 30min-60min at 500-600 ℃; removal of TiH2The conditions of (a) are as follows: calcining at 450-500 deg.C for 2-4h, wherein, C2H2And the volume ratio of Ar to Ar is 15: 1-35: 1.
9. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, is characterized in that the mechanical ball milling comprises the following specific steps:
(1) the method comprises the following steps of (1) filling Al powder and CNTs @ Ti mixed reinforced phase into a glove box to prepare powder, pouring the Al powder and the CNTs @ Ti into a ball milling tank, wherein the mass ratio of composite powder to steel balls is 10:1-20:1, filling high-purity argon into the ball milling tank, sealing the ball milling tank, and preventing aluminum powder from being oxidized;
(2) placing the mixture into a ball mill, and stopping ball milling for 15-30 min at the ball milling speed of 150-200r/min to avoid damaging the structure of the CNTs by high-speed ball milling; taking out the CNTs @ Ti/Al composite powder in an argon environment in a glove box.
10. The method for preparing the in-situ CNTs @ Ti hybrid reinforced aluminum matrix composite material according to claim 3, wherein the conditions of spark plasma sintering are as follows: the temperature is raised from the room temperature, the sintering temperature is 580-600 ℃, the temperature is kept for 40-50 min, and the pressure used in the sintering process is 30-50 MPa.
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