CN114318039B - Element alloying preparation method of metal matrix composite material with three-peak grain structure - Google Patents
Element alloying preparation method of metal matrix composite material with three-peak grain structure Download PDFInfo
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Abstract
The invention discloses an element alloying preparation method of a metal matrix composite material with a trimodal grain structure, which comprises the following steps: dividing the nano reinforcing phase into three parts, wherein the two parts and the elementary substance powder divided into the two parts are respectively and uniformly mixed, and performing ball milling to obtain superfine crystal composite powder and fine crystal composite powder; mixing the residual nano reinforcing phase with the metal powder, mixing the mixture with the two composite powders in proportion, and performing densification and sintering treatment to obtain a composite ingot blank; and carrying out thermal deformation processing and thermal treatment on the composite ingot blank to obtain the nano reinforced metal matrix composite material with a matrix structure and a grain structure in a trimodal size distribution. Compared with the material with the grain structure of unimodal distribution or bimodal size distribution, the composite material can more effectively relieve stress-strain concentration and synchronously improve the strong plasticity of the material; meanwhile, the method does not need to use alloy powder, adopts metal element powder to realize alloying through a sintering densification process, and can design and regulate the alloy components of the substrate at will.
Description
Technical Field
The invention relates to a preparation method of a metal matrix composite material with a trimodal grain structure, belonging to the technical field of metal matrix composite materials.
Background
The nano reinforced metal matrix composite material has excellent mechanical, thermal and other functional characteristics of a metal matrix and a reinforcement, has the advantages of high strength, high modulus, high working temperature, wear resistance, good electric and heat conduction, stable size and the like, and can be widely applied to a plurality of fields of infrastructure, automation, automobile industry, aerospace and the like. However, the introduction of the nano reinforcement brings the problem of obviously reduced ductility and toughness, and the key problem of restricting the practical engineering application of the nano reinforced metal matrix composite is that how to improve the strong-plasticity inversion relationship in the nano reinforced metal matrix composite.
In response to this problem, researchers have conducted a number of conformational design studies. Initial configuration design research mainly focuses on regulating and controlling reinforcement distribution, such as a layered configuration, a reticular configuration, a micro-nano laminated configuration and the like, the plastic toughness is improved in the mode of an external toughening mechanism, such as crack deflection, passivation, bridging and the like, and the problem of poor intrinsic plasticity of a matrix cannot be effectively solved. In recent years, the formation of metal matrix is increasingly studied, and the principle is an internal toughening mechanism for improving the matrix work hardening capacity by regulating the dislocation behavior. Heterogeneous materials such as gradient grains, strip grains, bimodal grains and trimodal grains are widely concerned by virtue of good strong plasticity matching, wide design space, various preparation methods and other characteristics.
The key of the strong plasticity control mechanism of the heterogeneous material is to generate high-density geometric essential dislocations GNDs (Geometrically adjacent dislocations), which requires that: 1) a sufficient number of soft/hard heterointerfaces to provide a place and space for the generation and containment of GNDs; 2) on the premise that the soft region/hard region heterogeneous interface combination is good enough, the larger the performance difference between the soft region and the hard region is, the larger the generated strain gradient is, and the higher the density of GNDs is; 3) the hard regions should geometrically completely constrain the soft regions, causing the soft regions to develop a high strain gradient, while avoiding interconnection between the soft regions so that deformation is concentrated only in the soft regions. The trimodal grain structure in the heterogeneous metal well meets the conditions, so that the trimodal grain structure alloy composite material provides a good research direction. For example, patent "a nano-reinforced metal matrix composite material with trimodal characteristics" (CN111519073A) discloses a nano-reinforced metal matrix composite material with trimodal characteristics, which is characterized by comprising a nano-carbon reinforcement and a metal matrix, wherein the grain size distribution of the metal matrix has distinct trimodal distribution characteristics. However, the metal matrix is derived from metal powder and pre-alloyed powder, on one hand, the components and sources of the pre-alloyed powder are severely limited, and inconvenience is brought to the preparation of the nano reinforced metal matrix composite material with the trimodal characteristics; on the other hand, the strength and hardness of the prealloyed powder are higher than those of pure aluminum powder, the grain refining efficiency by ball milling is low, and the grain refining degree (grain size change) is limited.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a high-efficiency and controllable preparation method of a nanometer reinforced metal matrix composite material with a trimodal grain structure.
In order to solve the technical problems, the invention adopts the following technical scheme:
an element alloying preparation method of a metal matrix composite material with a trimodal grain structure is characterized by comprising the following steps:
step 1): weighing a nano reinforcing phase and required elemental element powder according to the design requirements of material components, dividing the nano reinforcing phase into three parts, respectively adding, dividing all the elemental element powder into A, B parts, respectively and uniformly mixing the part A and the part B with the nano reinforcing phase to obtain mixed powder I and mixed powder II correspondingly, and uniformly mixing the nano reinforcing phase with metal powder to obtain mixed powder III;
step 2): respectively carrying out different ball milling processes on the mixed powder I and the mixed powder II of the part A and the part B obtained in the step 1) to obtain superfine crystal composite powder, namely the composite powder I and fine crystal composite powder, namely the composite powder II;
step 3): mixing the composite powder I and the composite powder II with non-ball-milled mixed powder III, namely micron coarse crystal metal powder, according to a ratio to obtain composite powder III;
step 4): carrying out densification and sintering treatment on the composite powder III to obtain a composite ingot blank;
step 5): and carrying out thermal deformation processing and thermal treatment on the composite ingot blank to obtain the nano reinforced metal matrix composite material with a matrix structure and a grain structure in a trimodal size distribution.
Preferably, the nano reinforcing phase is carbon nano tube, carbon nano sphere, carbon nano fiber, carbon nano sheet, graphene oxide, redox graphene, nano diamond, nano SiC, nano B4C, nano Al 2 O 3 Nano ZnO and nano TiO 2 Any one or more of nanometer AlN and nanometer TiN.
Preferably, the elemental element powder is any one or more of Al, Cu, Mg, Ti, Fe, Ni, Zn, Si, Zr, Cr, Co, Nb and W.
Preferably, in the mixed powder I, the mixed powder II and the mixed powder III, the volume contents of the nano reinforcing phase are respectively 1-20%, 0.1-10% and 0.001-5%.
Preferably, the ball milling process is variable speed ball milling, and specifically comprises the following steps: firstly, ball milling at a low rotating speed, wherein the rotating speed of the ball milling at the low rotating speed is 10-300 r/min, the ball milling time at the low rotating speed is 2-96h, ball milling at a high rotating speed is carried out after the ball milling at the low rotating speed, the rotating speed of the ball milling at the high rotating speed is 100-1000 r/min, and the ball milling time at the high rotating speed is 0.5-5 h.
Preferably, a process control agent is added in the process of the ball milling process, and the process control agent is any one or more of methanol, ethanol, titanate, silicone oil, oleic acid, imidazoline, paraffin, cellulose and stearic acid.
Preferably, the grain size of the ultra-fine grain composite powder is 0.05 to 0.5 μm.
Preferably, the grain size of the fine-grain composite powder is 0.5-3 μm.
Preferably, the grain size of the non-ball-milled micron coarse-grained metal powder is 3-100 μm.
Preferably, the densification treatment is cold pressing or cold isostatic pressing; the sintering process is atmosphere sintering, vacuum hot pressing sintering, spark plasma sintering or hot isostatic pressing sintering.
Preferably, the hot deformation process includes at least one of hot forging, hot rolling, and hot extrusion.
Compared with the material with the crystal grain structure of unimodal distribution (traditional uniform distribution) or bimodal size distribution, the nano reinforced metal matrix composite material with the matrix structure and the crystal grain structure of trimodal size distribution can more effectively relieve stress-strain concentration and synchronously improve the strong plasticity of the material; meanwhile, the method does not need to use alloy powder, realizes alloying by completely adopting metal element powder through a sintering densification process, can regulate and control the alloy components of the matrix according to design, has wide application range, and can realize the macro-quantitative preparation of large-size composite materials.
The invention provides an element alloying preparation method of a metal matrix composite with a trimodal grain structure, which can obtain a nano reinforced metal matrix composite with a matrix structure and a grain structure in trimodal size distribution. Compared with the traditional nanometer reinforced metal-based composite material with a double-peak size grain structure, the nanometer reinforced metal-based composite material prepared by the method can effectively relieve the stress concentration of the interface between the coarse crystal region and the fine crystal region, and provides enough heterogeneous interfaces so as to generate high-density geometric essential dislocation GNDs in the deformation process, which is also the key for breaking through the strong plasticity inversion relation. Compared with other preparation methods of nano reinforced metal matrix composite materials with three-peak size crystal grain structures, the method has the advantages of simple operation, stronger controllability and wide application range, and can be used for the macro-quantitative preparation of large-size composite materials.
Compared with the prior art, the invention has the following technical effects:
(1) alloy powder is not used, and wider grain size design and alloy component regulation can be realized by regulating and controlling the type and content of the added simple substance powder;
(2) the method is simple to operate, high in efficiency and good in process stability, and can be used for large-scale production of large-size composite materials;
(3) the grain size becomes obvious trimodal distribution, and the synchronous promotion of strong plasticity can be realized.
Drawings
FIG. 1 is a process flow diagram of the preparation method provided by the present invention.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
A 1.5% CNT/Al-4.2Cu-1.4Mg composite was prepared, wherein the final material composition included: the mass fraction of the carbon nanotubes is 1.5%, the mass fraction of Cu is 4.2%, the mass fraction of Mg is 1.4%, and the mass fraction of Al is 92.9%.
Mixing 91.2 wt% of pure Al powder with the particle size of 300 meshes, 5 wt% of Cu powder, 2 wt% of Mg powder and 1.80 wt% of CNT in a mixer for 5 hours to obtain mixed powder I; 89.37 wt% pure Al powder with a particle size of 300 mesh, 7 wt.% Cu powder, 2 wt.% Mg powder, and 1.63 wt.% CNT were mixed in a blender mixer for 5h to obtain mixed powder ii. 99 wt% pure Al powder with a particle size of 300 mesh and 1 wt.% CNT were mixed in a blender for 5h to give mixed powder iii.
Putting the mixed powder I into a ball mill, taking a stainless steel ball as a ball milling medium, adding 1 wt.% of stearic acid as a process control agent, and ball-milling at a ball-material ratio of 20:1 at a rotating speed of 120 r/min for 16h, and then at a rotating speed of 300 r/min for 2h to obtain ultrafine crystal composite powder (composite powder I).
Putting the mixed powder II into a ball mill, taking a stainless steel ball as a ball milling medium, adding 1 wt.% of stearic acid as a process control agent, wherein the ball-material ratio is 20:1, firstly carrying out ball milling for 8 hours at a rotating speed of 120 revolutions per minute, and then carrying out ball milling for 2 hours at a rotating speed of 250 revolutions per minute to obtain fine-grain composite powder (composite powder II).
Mixing 35% of composite powder I, 35% of composite powder II and 30 wt% of non-ball-milled mixed powder III in a ball mill at a ball-to-material ratio of 20:1 and a rotating speed of 200 rpm for 1h to obtain composite powder III.
The composite powder III is firstly pressed into a blank with the diameter of 40mm under the pressure of 400MPa, then the blank is placed in a vacuum sintering furnace to be sintered for 2h at the temperature of 570 ℃, and then the sintered blank is heated to 450 ℃ and is kept warm for 1h, and then is extruded into a round rod with the diameter of 8mm at the extrusion ratio of 25:1 and the extrusion rate of 2 mm/min.
And (3) performing solid solution on the extruded round bar at 500 ℃ for 2h, and aging at 150 ℃ for 12h to finally obtain the nano reinforced metal matrix composite material with the grain structure characteristic of trimodal size distribution, wherein the nano reinforced metal matrix composite material is 1.5% of CNT/Al-4.2Cu-1.4 Mg.
Example 2
A 1.5% CNT/Al-4.2Cu-1.4Mg composite was prepared, wherein the final material composition included: the mass fraction of the carbon nanotube was 1.5%, the mass fraction of Cu was 4.2%, the mass fraction of Mg was 1.4%, and the mass fraction of Al was 92.9%.
89.22 wt% of pure Al powder with the particle size of 300 meshes, 6 wt% of Cu powder, 3 wt% of Mg powder and 1.78 wt% of CNT are mixed in a mixer for 5 hours to obtain mixed powder I; 91.1 wt% pure Al powder with a particle size of 300 mesh, 6 wt.% Cu powder, 1.25 wt.% Mg powder and 1.65 wt.% CNT were mixed in a blender mixer for 5h to obtain mixed powder ii. 99 wt% pure Al powder with a particle size of 300 mesh and 1 wt.% CNT were mixed in a blender for 5h to give mixed powder iii.
Putting the mixed powder I into a ball mill, taking a stainless steel ball as a ball milling medium, adding 1 wt.% of stearic acid as a process control agent, and ball-milling at a ball-material ratio of 20:1 at a rotating speed of 120 r/min for 16h, and then at a rotating speed of 300 r/min for 2h to obtain ultrafine crystal composite powder (composite powder I).
And putting the mixed powder II into a ball mill, taking stainless steel balls as a ball milling medium, adding 1 wt.% of stearic acid as a process control agent, and performing ball milling for 8 hours at a ball-material ratio of 20:1 at a rotating speed of 120 revolutions per minute, and then performing ball milling for 2 hours at a rotating speed of 250 revolutions per minute to obtain fine-grain composite powder (composite powder II).
Mixing 50% of composite powder I, 40% of composite powder II and 10 wt% of non-ball-milled mixed powder III in a ball mill at a ball-to-material ratio of 20:1 and a rotating speed of 200 rpm for 1h to obtain composite powder III.
The composite powder III is firstly pressed into a blank with the diameter of 40mm under the pressure of 400MPa, then the blank is placed in a vacuum sintering furnace to be sintered for 2h at the temperature of 570 ℃, and then the sintered blank is heated to 450 ℃ and is kept warm for 1h, and then is extruded into a round rod with the diameter of 8mm at the extrusion ratio of 25:1 and the extrusion rate of 2 mm/min.
And (3) performing solid solution on the extruded round bar at 500 ℃ for 2h, and aging at 150 ℃ for 12h to finally obtain the nano reinforced metal matrix composite material with the grain structure characteristic of trimodal size distribution, wherein the nano reinforced metal matrix composite material is 1.5% of CNT/Al-4.2Cu-1.4 Mg.
Comparative example 1
The comparative example adopts the same powder metallurgy method as that of example 1, pure Al powder, Cu powder, Mg powder, 2024 alloy powder and CNT which are the same as those in example 1 are respectively taken and mixed in a mixer for 5 hours, then ball milling, sintering, deformation processing and heat treatment are carried out according to the same ball milling process as that in example 1, and finally the nano reinforced metal matrix composite material 1.5% CNT/Al-4.2Cu-1.4Mg with the grain structure characteristic of trimodal size distribution is obtained.
Comparative example 2
In the comparative example, pure Al powder, Cu powder, Mg powder and CNT which are the same as those in example 1 were mixed in a mixer for 5 hours by the same powder metallurgy method as in example 1, and then ball-milled, sintered, deformed and heat-treated by the same ball-milling process as in example 1, so as to obtain a nano-reinforced metal matrix composite material 1.5% CNT/Al-4.2Cu-1.4Mg with uniform grain size.
TABLE 1 Components, preparation methods, texture and Room temperature mechanical Properties of the composite materials
Note: the number before the element is the mass percent thereof
Claims (4)
1. An element alloying preparation method of a metal matrix composite material with a trimodal grain structure is characterized by comprising the following steps:
step 1): weighing a nano reinforcing phase and required elemental element powder according to the material components, dividing the nano reinforcing phase into three parts, dividing all the elemental element powder into A, B two parts, then respectively and uniformly mixing the part A and the part B with the nano reinforcing phase to correspondingly obtain mixed powder I and mixed powder II, and uniformly mixing the nano reinforcing phase with metal powder to obtain mixed powder III; in the mixed powder I, the mixed powder II and the mixed powder III, the volume contents of the nano reinforcing phase are respectively 1-20%, 0.1-10% and 0.001-5%;
step 2): respectively carrying out different ball milling processes on the mixed powder I and the mixed powder II of the part A and the part B obtained in the step 1) to obtain superfine crystal composite powder, namely the composite powder I and fine crystal composite powder, namely the composite powder II; the ball milling process is variable speed ball milling, and specifically comprises the following steps: firstly, ball milling at a low rotating speed, wherein the rotating speed of the ball milling at the low rotating speed is 10-300 r/min, the ball milling time at the low rotating speed is 5-96h, ball milling at a high rotating speed is carried out after the ball milling at the low rotating speed, the rotating speed of the ball milling at the high rotating speed is 100-; the grain size of the superfine crystal composite powder is 0.05-0.5 mu m; the grain size of the fine-grain composite powder is 0.5-3 mu m;
and step 3): mixing the composite powder I and the composite powder II with non-ball-milled mixed powder III, namely micron coarse crystal metal powder, according to a ratio to obtain composite powder III;
step 4): carrying out densification and sintering treatment on the composite powder III to obtain a composite ingot blank;
step 5): carrying out thermal deformation processing and thermal treatment on the composite ingot blank to obtain a nano reinforced metal matrix composite material with a matrix structure and a grain structure in a trimodal size distribution;
in the nano-reinforced metal matrix composite, the metal matrix composite is an Al-4.2Cu-1.4Mg composite, and the nano-reinforced phase is a carbon nano tube, a carbon nano sphere, a carbon nano fiber, a carbon nano flake, graphene oxide, redox graphene, nano diamond, nano SiC, nano B4C, nano Al 2 O 3 Nano ZnO and nano TiO 2 Any one or more of nanometer AlN and nanometer TiN.
2. The elemental alloying method for preparing a metallic matrix composite with a trimodal grain structure as claimed in claim 1, wherein the process control agent is added during the ball milling process, and the process control agent is any one or more of methanol, ethanol, titanate, silicone oil, oleic acid, imidazoline, paraffin, cellulose and stearic acid.
3. The method for preparing the metal matrix composite material with the trimodal grain structure through elemental alloying according to the claim 1, wherein the densification treatment is cold pressing or cold isostatic pressing; the sintering treatment is atmosphere sintering, vacuum hot-pressing sintering, spark plasma sintering or hot isostatic pressing sintering.
4. The method of elemental alloying of claim 1 wherein the hot deformation process comprises at least one of hot forging, hot rolling, and hot extrusion.
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