CN115074560B - Titanium particle reinforced magnesium matrix composite material and preparation method thereof - Google Patents
Titanium particle reinforced magnesium matrix composite material and preparation method thereof Download PDFInfo
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- CN115074560B CN115074560B CN202210772648.5A CN202210772648A CN115074560B CN 115074560 B CN115074560 B CN 115074560B CN 202210772648 A CN202210772648 A CN 202210772648A CN 115074560 B CN115074560 B CN 115074560B
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Abstract
The invention discloses a titanium particle reinforced magnesium matrix composite material and a preparation method thereof, belonging to the technical field of magnesium alloy. The method comprises the following steps: mixing the magnesium alloy melt with TiH under stirring 2 Mixing the particles; wherein, tiH 2 The mass ratio of the particles to the magnesium alloy matrix is 1. TiH 2 After entering the melt, the particles are heated to be rapidly decomposed to generate titanium particles and release hydrogen. The hydrogen firstly forms a layer of gas film on the particle surface, and under the action of the gas film, the titanium particles which are agglomerated together are separated, so that overlapping agglomeration is avoided, the agglomeration problem of the micron-scale titanium particles in a melt can be effectively solved, and the magnesium-based composite material with uniform dispersion is prepared.
Description
Technical Field
The invention relates to the technical field of magnesium alloy, in particular to a titanium particle reinforced magnesium matrix composite material and a preparation method thereof.
Background
At present, a stirring casting method is adopted to prepare the titanium particle reinforced magnesium-based composite material, and the added titanium particles are mainly micron titanium particles. The micron-sized titanium particles are influenced by Van der Waals force, electrostatic force and the like, and the particles are adhered to each other and are easy to agglomerate together and are difficult to disperse uniformly. When the magnesium-based composite material is prepared by adopting a stirring casting method, a stirring mechanism needs to stir at a high rotating speed for a long time, and agglomeration is easy to occur even in the way, so that the density and the mechanical property of the composite material are reduced, and the application of the magnesium-based composite material is limited.
In view of this, the invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of a titanium particle reinforced magnesium matrix composite material, which can prepare the magnesium matrix composite material with uniformly dispersed particles and no agglomeration.
The second purpose of the invention is to provide a titanium particle reinforced magnesium-based composite material prepared by the preparation method.
The application can be realized as follows:
in a first aspect, the invention provides a method for preparing a titanium particle reinforced magnesium matrix composite, which comprises the following steps: mixing the magnesium alloy matrix melt with TiH under stirring 2 Mixing the particles;
wherein, tiH 2 The mass ratio of the particles to the magnesium alloy matrix is 1.
In an alternative embodiment, tiH 2 The mass ratio of the particles to the magnesium alloy matrix is 1.
In an alternative embodiment, tiH 2 The average particle size of the particles is 0.5 to 10 μm.
In an alternative embodiment, tiH 2 The purity of the particles is more than or equal to 99.9 percent.
In an alternative embodiment, the magnesium alloy melt is alloyed with TiH 2 The mixing of the particles comprises: firstly adding TiH into the magnesium alloy melt under the condition that the rotating speed is 300-500rpm 2 Particles of TiH 2 After the particles are added, the magnesium alloy and TiH are added 2 The mixed melt of the granules is mixed for 3-30min under the condition that the rotating speed is 600-1000rpm.
In an alternative embodiment, the magnesium alloy and TiH 2 The mixed melt of the granules is mixed for 3-5min under the condition that the rotating speed is 600-1000rpm.
In an alternative embodiment, the mixing temperature is 550-650 ℃.
In an alternative embodiment, the TiH is treated prior to mixing with the magnesium alloy matrix melt 2 The particles are preheated.
In an alternative embodiment, the preheating time is 30-120min.
In alternative embodiments, preheating includes vacuum preheating or preheating in a non-vacuum environment. Wherein the vacuum preheating temperature is 80-350 ℃, and the preheating temperature is 80-300 ℃ in a non-vacuum environment.
In an alternative embodiment, the temperature of the vacuum preheat is 80-200 ℃.
In an alternative embodiment, the magnesium alloy melt is formed from a magnesium alloy melt.
In an alternative embodiment, the magnesium alloy is melted under the condition that the vacuum degree is less than or equal to 10 Pa.
In an alternative embodiment, the magnesium alloy is melted at 650-750 ℃, cooled to 550-650 ℃, and then mixed with TiH 2 And (4) mixing the particles.
In an alternative embodiment, the method further comprises the step of melting the magnesium alloy matrix and TiH 2 The mixed melt of particles is subjected to dehydrogenation.
In an alternative embodiment, the hydrogen removal comprises: to mix with TiH 2 And introducing inert gas into the magnesium alloy melt of the particles.
In an alternative embodiment, the inert gas is argon.
In an alternative embodiment, the hydrogen removal is carried out under stirring conditions.
In an alternative embodiment, the stirring speed during dehydrogenation is 600-1000rpm.
In an alternative embodiment, the material of the stirring mechanism is graphite, ceramic, titanium alloy or stainless steel.
In an alternative embodiment, the stirring mechanism used for stirring has an aperture in the middle.
In an alternative embodiment, the inert gas is introduced into the magnesium alloy and TiH through the pores of the stirring mechanism 2 In a mixed melt of the granules.
In an alternative embodiment, the pressure of the inert gas is from 0.01 to 0.06MPa.
In an alternative embodiment, casting is further included after hydrogen removal.
In an alternative embodiment, the casting temperature is 650-750 ℃.
In an alternative embodiment, the heating to the predetermined casting temperature after the hydrogen removal is performed at a stirring speed of 800 to 1200 rpm.
In a second aspect, the present application provides a titanium particle reinforced magnesium-based composite material prepared by the preparation method of any one of the foregoing embodiments.
In an alternative embodiment, the titanium particle reinforced Mg-based composite has a porosity of 1% or less.
In an alternative embodiment, the reinforcing phase in the titanium particle reinforced magnesium-based composite material is elemental titanium.
The beneficial effect of this application includes:
TiH for this application 2 The particles replace the scheme of directly adding titanium particles to prepare the magnesium-based composite material in the prior art; when TiH 2 After the particles enter the melt, the particles are heated and rapidly decomposed to generate titanium particles and release hydrogen. The hydrogen firstly forms a layer of gas film on the particle surface, and the titanium particles which are agglomerated together are separated under the action of the gas film, so that the overlapping agglomeration is avoided. That is, the present application incorporates TiH 2 The particles, the titanium particles generated by the reaction are used as the reinforcement, so that the problems that the particles are adhered and aggregated to each other, are easy to agglomerate together and are difficult to disperse uniformly due to the influence of van der Waals force, electrostatic acting force and the like when the micron-scale titanium particles are directly used as the reinforcement in the prior art can be effectively avoided. The scheme provided by the application can be used for preparing the magnesium-based composite material with uniform dispersion.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is TiH in example 1 2 Scanning electron micrographs of the particles;
fig. 2 to 9 are SEM photographs of the titanium particle-reinforced mg-based composite materials prepared in examples 1 to 8 of the present application in sequence;
fig. 10 to 17 are SEM photographs of the titanium particle-reinforced mg-based composite materials prepared in comparative examples 1 to 8 of the present application, in order.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The titanium particle-reinforced magnesium-based composite material and the preparation method thereof provided by the present application are specifically described below.
The application provides a preparation method of a titanium particle reinforced magnesium matrix composite, which comprises the following steps: mixing the magnesium alloy melt with TiH under stirring 2 Mixing the particles;
wherein, tiH 2 The mass ratio of the particles to the magnesium alloy is 1.
Referenced ground, tiH 2 The mass ratio of the particles to the magnesium alloy may be, for example, 1.
In some preferred embodiments, tiH 2 The mass ratio of the particles to the magnesium alloy is 1.
It is noted that if TiH 2 The mass ratio of the particles to the magnesium alloy is more than 1 (for example, 1 2 The mass ratio of the particles to the magnesium alloy matrix melt is less than 1 (such as 1. According to the preferable mass ratio of 1The obtained material has high mechanical property and lower density and has engineering application value.
In this application, tiH 2 The particles may be irregularly shaped, or may be spherical or nearly spherical. TiH 2 The average particle size of the particles is 0.5 to 10 μm. If TiH 2 The particles are irregularly shaped, the "particle size" refers to the TiH 2 The average size of the particles; if TiH 2 The particles are spherical or nearly spherical, and the "particle size" refers to the TiH 2 The average particle size of the particles. TiH used as described above 2 The particles can have nano-scale TiH 2 Particles, provided all TiH 2 The average particle size of the particles is 0.5-10 μm.
Referenced ground, tiH 2 The average particle size of the particles may illustratively be 0.5 μm, 1 μm, 2 μm, 5 μm, 8 μm, 10 μm, or the like, and may also be any other value in the range of 0.5 to 10 μm.
It is noted that if TiH 2 The average particle size of the particles is too small, the dispersion difficulty of the particles is high, and micro-agglomeration is easy to form; if TiH 2 The too large average particle size of the particles reduces the strengthening effect and is prone to sedimentation during the preparation process, leading to density segregation.
The above TiH 2 The purity of the particles is more than or equal to 99.9 percent.
Bearing, tiH for this application 2 The particles replace the scheme of directly adding titanium particles to prepare the magnesium-based composite material in the prior art; when TiH 2 After the particles enter the melt, the particles are heated and rapidly decomposed to generate titanium particles and release hydrogen. The hydrogen firstly forms a layer of gas film on the particle surface, and the titanium particles which are agglomerated together are separated under the action of the gas film, so that the overlapping agglomeration is avoided. That is, the present application is directed to the incorporation of TiH 2 The particles replace directly added titanium particles, so that the problems that in the prior art, the particles are adhered and aggregated to each other due to the influence of van der Waals force, electrostatic acting force and the like when the micron-sized titanium particles are directly used as a reinforcement, the particles are easily agglomerated together and are difficult to disperse uniformly can be effectively solved. The scheme provided by the application can be used for preparing the magnesium-based composite material with uniform dispersion and no agglomeration.
Need to emphasizeThat is, tiH in the present application 2 The particles do not play a foaming role, but play a role in dispersing the particles by utilizing hydrogen and generating simple substance titanium as a reinforcing phase.
By reference, the magnesium alloy matrix melt and TiH in this application 2 The mixing of the particles may include: adding TiH into the magnesium alloy matrix melt under the condition of the rotation speed of 300-500rpm (such as 300rpm, 350rpm, 400rpm, 450rpm or 500rpm and the like) 2 Particles of TiH 2 After the particles are added, the magnesium alloy matrix melt and TiH are added 2 The mixed melt of the particles is mixed for 3-30min (such as 3min, 5min, 10min, 15min, 20min, 25min or 30 min) at a rotation speed of 600-1000rpm (such as 600rpm, 650rpm, 700rpm, 750rpm, 800rpm, 850rpm, 900rpm, 950rpm or 1000 rpm).
In some preferred embodiments, the magnesium alloy matrix melt and TiH 2 Mixing the mixed melt of the granules at 600-1000rpm for 3-5min (such as 3min, 3.5min, 4min, 4.5min or 5 min).
The above magnesium alloy matrix melt and TiH 2 The remixing time of the mixed melt of the particles at 600-1000rpm is not less than 3min, otherwise, the gas film is not favorable for pushing away and dispersing the agglomerated particles.
In an alternative embodiment, the magnesium alloy matrix melt is alloyed with TiH 2 The temperature during the mixing process of the granules can be 550-650 deg.C, such as 550 deg.C, 560 deg.C, 570 deg.C, 580 deg.C, 590 deg.C, 600 deg.C, 610 deg.C, 620 deg.C, 630 deg.C, 640 deg.C or 650 deg.C, etc., or any other value within 550-650 deg.C.
In this application, the TiH may be treated prior to mixing with the magnesium alloy matrix melt 2 The particles are preheated to reduce adsorption to TiH 2 Water vapor on the particles.
Preheating may include vacuum preheating or preheating in a non-vacuum environment.
Wherein the vacuum preheating temperature is 80-350 deg.C, such as 80 deg.C, 100 deg.C, 150 deg.C, 200 deg.C, 250 deg.C, 300 deg.C or 350 deg.C, or other arbitrary values within the range of 80-350 deg.C, preferably 80-200 deg.C.
It is emphasized thatThe temperature of the vacuum preheating exceeds 350 ℃, which can result in TiH 2 The particles undergo decomposition reactions.
The preheating temperature in non-vacuum environment is not more than 300 deg.C, such as 300 deg.C, 280 deg.C, 250 deg.C, 220 deg.C or 200 deg.C, preferably 80-300 deg.C.
It is emphasized that preheating temperatures in a non-vacuum environment in excess of 300 ℃ will result in TiH 2 The particles forming TiO during heating 2 And TiN.
The preheating time may be 30-120min, such as 30min, 50min, 80min, 100min or 120min, or any other value within the range of 30-120min.
In the present application, the magnesium alloy melt is obtained by melting a magnesium alloy.
The magnesium alloy is melted under the condition that the vacuum degree is less than or equal to 10Pa, and can be specifically carried out in a vacuum furnace.
By carrying out the melting under the above-mentioned conditions, tiH can be avoided 2 The particles are heated to react with oxygen and nitrogen in the air to produce TiO 2 And TiN.
In some alternative embodiments, the magnesium alloy matrix can be melted at 650-750 ℃, cooled to 550-650 ℃, and then mixed with TiH 2 And (4) mixing the particles.
After melting, the temperature is reduced to 550-650 ℃ and then the molten material is mixed with TiH 2 The particles are mixed because: 1) Under vacuum, tiH 2 The decomposition speed in the temperature interval can quickly separate out hydrogen; 2) In the temperature range, the magnesium alloy melt has high viscosity, which is beneficial to avoiding the generated Ti particles from settling.
Further, the method also comprises the step of melting the magnesium alloy matrix and TiH 2 The mixed melt of particles is subjected to dehydrogenation.
By reference, dehydrogenation includes: to mix with TiH 2 Inert gas, preferably argon, is introduced into the magnesium alloy melt of the particles.
Preferably, the dehydrogenation stage is also carried out under stirring conditions. The stirring speed during the hydrogen removal process can be 600-1000rpm, such as 600rpm, 700rpm, 800rpm, 900rpm or 1000rpm, and the like, and can also be any other value within the range of 600-1000rpm.
In some preferred embodiments, the stirring mechanism used for stirring is a structure with a hole in the middle, and the material of the stirring mechanism can be graphite, ceramic, stainless steel, titanium alloy or the like.
Under the condition, inert gas is introduced into the magnesium alloy and the TiH through the pores of the stirring mechanism 2 In a mixed melt of the granules.
The pressure of the inert gas introduced is 0.01-0.06MPa, such as 0.01MPa, 0.02MPa, 0.03MPa, 0.04MPa, 0.05MPa or 0.06MPa, and may be any other value within the range of 0.01-0.06MPa.
It should be noted that if the argon pressure is lower than 0.01MPa, hydrogen in the melt is not easily released, and the pore defect is easily formed in the cast material; if the argon pressure is higher than 0.06MPa, the titanium particles will be carried out of the melt when the gas escapes.
In summary, the above dehydrogenation principle can be referred to as follows: and during stirring, introducing argon gas into the melt through a hole in the middle of the stirring mechanism, wherein the argon gas forms small bubbles under the action of the stirring head and escapes from the melt upwards, and in the escaping process, hydrogen in the melt diffuses into the bubbles under the action of partial pressure difference and escapes along with the bubbles, so that the aim of removing hydrogen from the melt is fulfilled.
The dehydrogenation time can be 3-10min.
Further, casting was performed after hydrogen removal.
The casting temperature may, by reference, be 650-750 c, such as 650 c, 660 c, 670 c, 680 c, 690 c, 700 c, 710 c, 720 c, 730 c, 740 c, 750 c, etc., or any other value within the range of 650-750 c.
After the hydrogen removal, the temperature is raised to the predetermined casting temperature under the condition that the stirring speed is 800-1200rpm (such as 800rpm, 900rpm, 1000rpm, 1100rpm or 1200 rpm).
It should be noted that the process is also carried out under stirring conditions, which avoids the titanium particles settling in the melt.
Correspondingly, the application also provides a titanium particle reinforced magnesium matrix composite material prepared by the preparation method.
The porosity of the titanium particle reinforced magnesium-based composite material is less than or equal to 1 percent.
It is emphasized that the reinforcing phase in the titanium particle reinforced magnesium matrix composite material of the present application is titanium simple substance, but not Ti-Al intermediate compound or TiC and TiB 2 And the like. The simple substance of titanium and the magnesium alloy matrix have good wettability, metal particles such as Al or Mg and the like do not need to be mixed in the particles, namely, the metal particles do not need to be added and subjected to ball milling, so that a corresponding metal layer is generated on the surface of the reinforcement body, and the purpose of improving the wettability of the reinforcement body is achieved.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a titanium particle reinforced magnesium matrix composite material, and a preparation method thereof comprises the following steps:
s1, preheating TiH 2 And (3) particles.
Will TiH 2 The granules were preheated for 60min at 200 ℃ under vacuum.
Wherein, tiH 2 The average particle size of the particles is 10 mu m, and the purity is more than or equal to 99.9 percent.
And S2, melting the magnesium alloy.
Heating the AZ91 magnesium alloy to 700 ℃ in a vacuum furnace with the vacuum degree less than or equal to 10Pa, and cooling the temperature to 580 ℃ after the magnesium alloy is melted.
And S3, starting stirring.
Starting a stirring mechanism in the vacuum furnace, setting the stirring speed to be 400rpm, and preheating the TiH in the stirring state 2 The granules are added to the melt.
TiH 2 The mass ratio of the particles to the AZ91 magnesium alloy matrix is 1.
The stirring mechanism is made of graphite and is provided with a hole for introducing inert gas.
And S4, stirring and mixing.
TiH 2 After the addition of the particles was complete, the stirring phase was continued at 800rpm for 5min, the temperature of the stirring phase being maintained at 550-600 ℃.
And S5, removing hydrogen.
And after the stirring stage is finished, entering a dehydrogenation stage. In the stage, the stirring is continued at the rotating speed of 800rpm, and argon with the pressure of 0.05MPa is introduced into the melt through a hole in the middle of the stirring mechanism while stirring. The dehydrogenation time was 3min.
And S6, casting.
And (3) heating the melt obtained after the dehydrogenation to 700 ℃ (the stirring speed is 1000rpm in the heating stage) and casting to obtain the titanium particle reinforced magnesium-based composite material.
Example 2
The embodiment provides a titanium particle reinforced magnesium matrix composite material, and a preparation method thereof comprises the following steps:
s1, preheating TiH 2 And (3) granules.
Mix TiH 2 The granules were preheated at 80 ℃ for 120min under vacuum.
Wherein, tiH 2 The average grain diameter of the grains is 0.5 mu m, and the purity is more than or equal to 99.9 percent.
And S2, melting the magnesium alloy matrix.
In a vacuum furnace with the vacuum degree less than or equal to 10Pa, the temperature of the magnesium alloy is raised to 650 ℃, and after the magnesium alloy is completely melted, the temperature is lowered to 590 ℃.
And S3, starting stirring.
Starting a stirring mechanism in the vacuum furnace, setting the stirring speed to 300rpm, and preheating the TiH in the stirring state 2 The particles are added to the melt.
TiH 2 The mass ratio of the particles to the AZ91 magnesium alloy matrix is 1.
The stirring mechanism is made of ceramic and is provided with a hole for introducing inert gas.
And S4, stirring and mixing.
TiH 2 After the addition of the particles was completed, the stirring phase was continued at 600rpm for 30min, the temperature of the stirring phase being maintained at 550-600 ℃.
And S5, removing hydrogen.
And after the stirring stage is finished, entering a dehydrogenation stage. In the stage, stirring is continued at a rotating speed of 600rpm, and argon with a pressure of 0.01MPa is introduced into the melt through a hole in the middle of the stirring mechanism while stirring. The dehydrogenation time was 5min.
And S6, casting.
And heating the melt obtained after the dehydrogenation to 650 ℃ (the stirring speed is 800rpm in the heating stage) and casting to obtain the titanium particle reinforced magnesium matrix composite.
Example 3
The embodiment provides a titanium particle reinforced magnesium matrix composite material, and a preparation method thereof comprises the following steps:
s1, preheating TiH 2 And (3) granules.
Mix TiH 2 The granules were preheated at 350 ℃ for 30min under vacuum.
Wherein, tiH 2 The particles are spherical particles with the average particle size of 5 mu m, and the purity is more than or equal to 99.9 percent.
And S2, melting the magnesium alloy matrix.
Heating the AZ91 magnesium alloy to 750 ℃ in a vacuum furnace with the vacuum degree less than or equal to 10Pa, and cooling to 600 ℃ after the AZ91 magnesium alloy is completely melted.
And S3, starting stirring.
Starting a stirring mechanism in the vacuum furnace, setting the stirring speed to be 500rpm, and preheating the TiH in the stirring state 2 The granules are added to the melt.
TiH 2 The mass ratio of the particles to the AZ91 magnesium alloy matrix is 1.
The stirring mechanism is made of graphite and is provided with a hole for introducing inert gas.
And S4, stirring and mixing.
TiH 2 After the addition of the particles is completed, the stirring stage is started, the stirring is continued for 10min at the rotating speed of 800rpm, and the temperature of the stirring stage is kept between 550 and 600 ℃.
And S5, removing hydrogen.
And after the stirring stage is finished, entering a dehydrogenation stage. In the stage, the stirring is continued at the rotating speed of 800rpm, and argon with the pressure of 0.06MPa is introduced into the melt through a hole in the middle of the stirring mechanism while stirring. The dehydrogenation time was 10min.
And S6, casting.
And heating the melt obtained after the dehydrogenation to 750 ℃ (the stirring speed is 1200rpm in the heating stage) and casting to obtain the titanium particle reinforced magnesium matrix composite.
Example 4
The present example differs from example 1 in that: tiH 2 The particles were spherical particles having an average particle diameter of 1 μm.
Example 5
This example differs from example 1 in that: tiH 2 The mass ratio of the particles to the AZ91 magnesium alloy matrix is 1.
Example 6
This example differs from example 1 in that: tiH 2 The ratio of the particles to the AZ91 magnesium alloy matrix is 1.
Example 7
The present example differs from example 1 in that: and the stirring and mixing time in the step S4 is 3min.
Example 8
This example differs from example 1 in that: in step S1, tiH 2 The particles were preheated for 100min at 200 ℃ in a non-vacuum environment.
Comparative example 1
This comparative example differs from example 1 in that: tiH 2 The particles are not preheated and are directly mixed with the magnesium alloy melt.
Comparative example 2
The comparative example differs from example 1 in that: tiH 2 The granules were preheated at 380 ℃ for 60min under vacuum.
Comparative example 3
This comparative example differs from example 8 in that: tiH 2 The granules were preheated at 320 ℃ for 60min in a non-vacuum environment.
Comparative example 4
This comparative example differs from example 1 in that: tiH 2 The average particle size of the particles was 0.1. Mu.m.
Comparative example 5
This comparative example differs from example 1 in that: tiH 2 Average of particlesThe particle size was 50 μm.
Comparative example 6
The comparative example differs from example 1 in that: tiH 2 The mass ratio of particles to melt was 1.
Comparative example 7
This comparative example differs from example 1 in that: tiH 2 The mass ratio of the particles to the melt was 1.
Comparative example 8
This comparative example differs from example 1 in that: the argon pressure was 0.005MPa.
Test example 1
Example 1, the TiH used 2 The SEM electron microscope scanning results of the particles are shown in fig. 1, and the SEM electron microscope scanning results of the prepared titanium particle-reinforced magnesium-based composite material are shown in fig. 2.
As can be seen from fig. 1 and 2 in combination: the titanium particles are uniformly distributed in the magnesium alloy matrix, and the agglomeration phenomenon does not occur among the particles.
The titanium particle-reinforced Mg-based composite materials obtained in examples 2 to 8 were also subjected to SEM scanning, and the results are shown in FIGS. 3 to 9. The titanium particles in the prepared composite material are also shown to have no agglomeration phenomenon and to be well combined with the magnesium alloy matrix.
In fig. 3, because titanium particles are small and the adsorption force between the particles is strong, the particles are close to each other but still have a certain distance and are not completely agglomerated together. As can be seen in fig. 4, there is a distance between the titanium particles and no agglomeration occurs.
Similarly, the results of SEM electron microscope scanning of the titanium particle-reinforced Mg-based composite materials obtained in comparative examples 1 to 8 are shown in FIGS. 10 to 17.
Among them, in the case of FIG. 10, due to TiH 2 The particles are not preheated and the moisture contained forms pores in the composite material. In the case of FIG. 11, tiH 2 The particles are preheated in a vacuum environment at 380 ℃, reaction occurs, and hydrogen is released in advance, so that the titanium particles are agglomerated after the magnesium alloy melt is added. In the case of FIG. 12, tiH 2 Preheating the granules at 320 deg.C in non-vacuum environment, reacting, and producingTitanium compounds, which wet poorly with the substrate, do not form a good bonding surface. For FIG. 13, tiH 2 The particles had an average particle diameter of 0.1 μm and easily formed agglomerates in the matrix. In the case of FIG. 14, tiH 2 The particles had an average particle size of 50 μm and, due to the excessive particle size, were deposited on the bottom of the material. In the case of FIG. 15, tiH 2 The mass ratio of particles to melt is 1. In the case of FIG. 16, tiH 2 The mass ratio of the particles to the melt is 1. In FIG. 17, the argon pressure was 0.005MPa, and the pressure was too low, so that the dehydrogenation effect was poor, and a large number of pores were present in the composite material.
Test example 2
The porosities of the titanium particle-reinforced magnesium-based composites obtained in examples 1 to 8 and comparative examples 1 to 8 were measured with reference to ASTM E2109 TSA porosity test Standard, and the results are shown in Table 1:
table 1 porosity results
| Porosity (%) | Porosity (%) | ||
| Example 1 | 0.65 | Comparative example 1 | 2.63 |
| Example 2 | 0.81 | Comparative example 2 | 1.52 |
| Example 3 | 0.76 | Comparative example 3 | 2.35 |
| Example 4 | 0.77 | Comparative example 4 | 1.63 |
| Example 5 | 0.87 | Comparative example 5 | 1.38 |
| Example 6 | 0.68 | Comparative example 6 | 1.12 |
| Example 7 | 0.91 | Comparative example 7 | 0.88 |
| Example 8 | 0.86 | Comparative example 8 | 3.11 |
As can be seen from table 1: the porosity of the titanium particle reinforced magnesium matrix composite material obtained in the embodiment is less than 1 percent. The comparative example affected the density due to the formation of pores and particle agglomeration.
In summary, the preparation method of the titanium particle reinforced magnesium matrix composite material provided by the application has at least the following advantages:
①TiH 2 the density of the granules was 3.75g/cm 3 Less than the density of the titanium particles (density of the titanium particles is 4.5 g/cm) 3 ) The sedimentation tendency is small when the material is added, and gravity segregation is not easy to form;
(2) the agglomeration of particles is reduced due to the action of the air film, and the stirring time can be greatly shortened;
(3) the melt is subjected to dehydrogenation treatment, and the prepared composite material is compact and has no air holes.
The present invention has been described in terms of the preferred embodiment, and it is not intended to be limited to the embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. The preparation method of the titanium particle reinforced magnesium matrix composite is characterized by comprising the following steps:
melting the magnesium alloy matrix at 650-750 ℃, and then cooling to 550-650 ℃ to obtain a magnesium alloy matrix melt; mixing the magnesium alloy matrix melt with TiH under the condition of stirring 2 Mixing the particles;
wherein, the TiH 2 The mass ratio of the particles to the magnesium alloy matrix is 1 (50-250); the TiH 2 The average particle size of the particles is 0.5-10 μm;
before mixing with the magnesium alloy matrix melt, firstly processing the TiH 2 Preheating the particles; preheating for 30-120min; preheating comprises vacuum preheating or preheating in a non-vacuum environment, wherein the temperature of the vacuum preheating is 80-350 ℃, and the temperature of the preheating in the non-vacuum environment is 80-300 ℃;
further comprises melting the magnesium alloy matrix and the TiH 2 Removing hydrogen from the mixed melt of the particles; the dehydrogenation comprises the following steps: to mix TiH 2 Introducing inert gas into the magnesium alloy melt of the particles;
the dehydrogenation is carried out under the stirring condition; the pressure of the inert gas is 0.01-0.06MPa.
2. The method of claim 1, wherein the TiH is 2 The mass ratio of the particles to the magnesium alloy matrix is 1 (50-100);
the TiH 2 The purity of the particles is more than or equal to 99.9 percent.
3. The method of claim 1, wherein the magnesium alloy matrix melt is mixed with the TiH 2 The mixing of the particles comprises: adding the TiH into the magnesium alloy matrix melt under the condition that the rotating speed is 300-500rpm 2 Particles of said TiH 2 After the particles are added, the magnesium alloy matrix melt and the TiH are mixed 2 The mixed melt of the granules is mixed for 3-30min under the condition that the rotating speed is 600-1000rpm.
4. The method of claim 3, wherein the magnesium alloy matrix melt and the TiH are mixed together to form the TiH alloy 2 The mixed melt of the granules is mixed for 3-5min under the condition that the rotating speed is 600-1000rpm.
5. The method of claim 3, wherein the mixing temperature is 550 to 650 ℃.
6. The production method according to any one of claims 1 to 5, wherein the temperature of the vacuum preheating is 80 to 200 ℃.
7. The production method according to any one of claims 1 to 5, wherein the melting of the magnesium alloy substrate is performed under a vacuum degree of 10Pa or less.
8. The method of claim 1, wherein the inert gas is argon.
9. The production method according to claim 1, wherein the stirring speed during the dehydrogenation is 600 to 1000rpm.
10. The preparation method of claim 9, wherein the stirring mechanism for stirring is made of graphite, ceramic, stainless steel or titanium alloy;
the middle of the stirring mechanism is provided with a pore;
the inert gas is introduced into the magnesium alloy matrix melt and the TiH through the pores of the stirring mechanism 2 A mixed melt of the particles.
11. The method of claim 1, further comprising casting after removing hydrogen;
the casting temperature is 650-750 ℃;
after the hydrogen removal is finished, the process of raising the temperature to the preset casting temperature is carried out under the condition that the stirring rotating speed is 800-1200 rpm.
12. The method as claimed in claim 1, wherein the titanium particle reinforced Mg-based composite material has a porosity of 1% or less.
13. The method as claimed in claim 1, wherein the reinforcing phase in the titanium particle reinforced Mg-based composite material is elemental titanium.
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