CN115341115B - Aluminum-titanium-carbon intermediate alloy refiner and preparation method thereof - Google Patents
Aluminum-titanium-carbon intermediate alloy refiner and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/08—Amorphous alloys with aluminium as the major constituent
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Abstract
The invention relates to an aluminum-titanium-carbon intermediate alloy refiner and a preparation method thereof. According to the preparation method disclosed by the invention, MAX ceramic powder (ternary compound containing Ti element and C element) with a TiC structure is adopted as a Ti source and a C source, and TiC particles are formed through the high-temperature reaction of the ternary compound and Al and the 'top-down' in-situ decomposition, so that the problems of reactant residues, uneven diffusion of the Ti element and the C element and the like in the traditional 'bottom-up' preparation method are avoided, and the preparation method has the advantages of simple process, environment friendliness, lower cost, convenience in material component design and the like, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of aluminum and aluminum alloy grain refinement, in particular to an aluminum-titanium-carbon intermediate alloy refiner and a preparation method thereof.
Background
The aluminum alloy is used as a typical representative of light alloy materials, is widely applied to the fields of industry, national defense, traffic, consumer electronics products and the like by virtue of excellent mechanical and physical properties, and becomes a second largest metal material next to steel materials by virtue of obvious advantages in technical properties, economy and the like, thereby occupying important roles in the whole national economic development. As a structural material, grain refinement of aluminum and aluminum alloys is not only a main means of strengthening and toughening thereof, but also a necessary premise for application thereof. From the process of nucleation and growth of crystal grains, the realization of grain refinement solves the problems of the nucleation rate of the initial crystal grains and the growth rate after the formation of the initial crystal grains. At present, the non-uniform nucleation rate is improved by adding a grain refiner, and the method is the simplest and efficient method for realizing grain refinement.
In the prior art, commonly used aluminum alloy grain refiners are Al-Ti-B grain refiners. However, al-Ti-B refiners also expose problems during long-term application, such as TiB 2 Particles are easy to gather in the melt, so that the refining effect is reduced, and meanwhile, the subsequent processing of the material is adversely affected. From the analysis of the basic principle of non-uniform nucleation, the wettability of the crystal nucleus and the nucleation core directly influences the nucleation work (namely the nucleation difficulty), the wettability depends on the contact structure between the crystal nucleus and the nucleation core, and if the atomic arrangement is well matched and the lattice parameters are close, the interface energy between the crystal nucleus and the nucleation core is small, and the wettability is good. TiC and Al belong to a face-centered cubic structure, the lattice constants are similar, and the lattice matching principle is met, so that the Al-Ti-C refiner is considered to be an ideal substitute material for the Al-Ti-B refiner. However, it has long been difficult to prepare grain refiners containing TiC particles due to the extremely low solubility of carbon in aluminum melts. Al-Ti-C grain refiner was prepared until A.Banerji et Al in 1985 solved the problem of absorption of C element in aluminum melt and showed excellent refining performance, and Al-Ti-C refiner was not attracting attention and research again by scholars. Because of the wettability problem of carbon in aluminum melts, researchers have also conducted extensive research on the preparation methods of Al-Ti-C refiners, and formed various preparation methods of Al-Ti-C master alloys, such as melt reaction methods, self-propagating high-temperature synthesis methods, thermal explosion synthesis methods, and the like.
For example, CN98119377.3 discloses a method for preparing an aluminum-based intermediate alloy containing titanium and carbon, which comprises the steps of firstly melting industrial pure aluminum to 750-850 ℃, then adding an activating agent, later adding fluotitanate and graphite powder, adding a covering agent, keeping the reaction for 10-30 minutes, removing slag, and casting into ingots to obtain the intermediate alloy. The disadvantage of this method is that a large amount of AlF is formed during the production process 3 And toxic gases, such as the magnesium alloy, pollute the environment, and meanwhile, the intermediate alloy often contains salt inclusions so as to influence the performance of the intermediate alloy.
CN00123953.8 discloses a process for preparing aluminium-titanium-carbon intermediate alloy, which comprises melting industrial pure aluminium to 1100-1350 deg.c, adding pure titanium and graphite powder, preserving heat for 0.5-30 min, cooling, casting into ingot directly or making into wire intermediate alloy by continuous casting and rolling equipment. Although the method does not involve the use of fluorotitanate, the method has high heating temperature and high energy consumption, and incomplete reaction of graphite and Ti often occurs in the method, and free carbon remains in the master alloy, so that the performance of the master alloy is affected.
CN02156761.1 discloses an aluminum-titanium-carbon intermediate alloy grain refiner, which relates to an Al-Ti-C grain refiner containing TiC particles for refining aluminum and aluminum alloy and a preparation method of the grain refiner. The method comprises the steps of firstly melting industrial pure aluminum to 800-900 ℃, then adding titanium sponge to prepare an Al-Ti intermediate alloy melt, introducing a carbon source (one of industrial graphite, natural graphite, amorphous graphite, activated carbon or carbon black) by nitrogen or argon, and stirring by adopting a graphite rotor at a rotating speed of 100-400 rpm until no monomer carbon exists. Although this method recognizes the problem of carbon residue, it is difficult to control the complete reaction of carbon by stirring alone, and it is difficult to judge that no monomer carbon is present in practical operation.
CN200410103904.3 discloses the composition, structure characteristics, preparation method and application method for grain refinement of aluminum and aluminum alloy under the action of ultrasonic field. Firstly melting an aluminum ingot to 800-900 ℃, then adding potassium fluotitanate and graphite carbon, adding a covering agent (5% NaCl+5% KCl), mechanically stirring for 2-5 minutes, adding ultrasonic waves into a melt which starts to react through an ultrasonic generator and an amplitude transformer for 10-15 minutes, starting an ultrasonic vibration head after the reaction is finished, transferring the melt to a heat preservation furnace after heating, heat preservation, standing and deslagging, and then casting into an ingot or continuously casting and rolling into wires with the diameter of 9.5mm, thereby obtaining the required intermediate alloy refiner. The method has complex process and also involves the use of fluotitanate, and the prepared intermediate alloy has the possibility of fluoride inclusion and can generate a large amount of KF and AlF 3 Etc. are toxicThe gas causes a certain harm to the environment.
CN200710016306.6 discloses a method for preparing aluminum-titanium-carbon intermediate alloy, which comprises the steps of firstly melting pure aluminum and aluminum-titanium intermediate alloy, heating to 900-1300 ℃, then adding aluminum-carbon binary intermediate alloy, preserving heat, mechanically stirring for 2-30 minutes, then adding reserved aluminum-titanium intermediate alloy cold charge, and directly casting into ingots or preparing wires. The method has the advantages of higher smelting temperature, high energy consumption, and complex process because different intermediate alloys are required to be added for multiple times. In addition, the method does not control the reaction of Ti element and C element, so the problem of carbon residue in the initial master alloy cannot be effectively solved.
CN201510166380.0 discloses an aluminum-titanium-carbon intermediate alloy refiner and a preparation process thereof, CN201510042442.7 discloses an aluminum-titanium-carbon intermediate alloy refiner, both potassium fluotitanate and potassium fluoborate are simultaneously used for preparing the intermediate alloy refiner, and the prepared intermediate alloy also has the problems of salt inclusion, generation of toxic and harmful gases and the like.
In summary, the preparation method of the aluminum-titanium-carbon intermediate alloy refiner disclosed in the patent document is easy to see that the existing preparation method adopts simple substances or compounds containing Ti element and C element to synthesize TiC particles in situ in a 'bottom-up' mode. The 'bottom-up' in-situ synthesis method involves the decomposition of Ti-containing compounds and the diffusion and reaction of Ti element and C element, and the method often causes the problems of residual initial reactants (such as free carbon), uneven diffusion reaction of Ti element and C element, and the like, which have direct influence on the preparation quality of Al-Ti-C refiner.
Therefore, there is a need to develop a novel aluminum-titanium-carbon intermediate alloy refiner and a preparation method thereof, wherein MAX ceramic powder (ternary compound containing Ti element and C element) containing TiC structure is adopted as Ti source and C source, and TiC particles are formed by the high-temperature reaction of the ternary compound and Al and 'top-down' in-situ decomposition, so that the problems of reactant residue, uneven diffusion of Ti element and C element and the like in the traditional 'bottom-up' preparation method are avoided. In addition, the preparation method of 'top-down' in-situ decomposition has the advantages of simple process, environmental protection, lower cost, convenient material component design and the like, and is suitable for large-scale production.
Disclosure of Invention
In order to solve the technical problems, the invention provides an aluminum-titanium-carbon intermediate alloy refiner and a preparation method thereof, wherein MAX ceramic powder and aluminum powder containing TiC structures are weighed according to mass proportion, and the aluminum-titanium-carbon intermediate alloy refiner is obtained through mixing, compression molding and high-temperature treatment in sequence and cooling. According to the preparation method disclosed by the invention, MAX ceramic powder (ternary compound containing Ti element and C element) with a TiC structure is adopted as a Ti source and a C source, and TiC particles are formed through the high-temperature reaction of the ternary compound and Al and the 'top-down' in-situ decomposition, so that the problems of reactant residues, uneven diffusion of the Ti element and the C element and the like in the traditional 'bottom-up' preparation method are avoided, and the preparation method has the advantages of simple process, environment friendliness, lower cost, convenience in material component design and the like, and is suitable for large-scale production.
The invention aims to provide a preparation method of an aluminum-titanium-carbon intermediate alloy refiner, which comprises the following steps:
(1) Mixing: weighing MAX ceramic powder containing TiC structure and aluminum powder according to mass proportion, and uniformly mixing to obtain mixed powder;
(2) And (5) press forming: pressing the mixed powder in the step (1) to form a mixed blank;
(3) High temperature treatment: and (3) carrying out high-temperature treatment on the mixed blank in the step (2), and cooling to obtain the aluminum-titanium-carbon intermediate alloy refiner.
According to the preparation method disclosed by the invention, MAX ceramic powder (ternary compound containing Ti element and C element) containing a TiC structure is adopted as an initial reactant, and TiC particles are formed by virtue of in-situ decomposition of the MAX ceramic powder and Al from top to bottom at high temperature, so that the problem of intermediate alloy inclusion caused by incomplete reactant reaction in the traditional bottom-to-top preparation method is avoided, and the preparation method has the advantages of simple process, environment friendliness, lower cost, convenience in material component design and the like, and is suitable for large-scale production.
As a preferable technical scheme of the invention, the mass percentage of MAX ceramic powder containing TiC structure in the mass proportion in the step (1) is 1-30 wt.%, and the balance is aluminum powder and unavoidable impurities.
The mass percentage of MAX ceramic powder containing TiC structure in the present invention is 1-30 wt.%, for example, 1wt.%, 3wt.%, 5wt.%, 8wt.%, 10wt.%, 15wt.%, 18wt.%, 20wt.%, 23wt.%, 25wt.%, 27wt.%, or 30wt.%, etc., but not limited to the recited values, other non-recited values in the range of values are equally applicable.
As a preferable technical scheme of the invention, the MAX ceramic powder containing TiC structure in the step (1) comprises Ti 2 AlC powder, ti 3 AlC 2 Powder or Ti 3 SiC 2 Any one or the combination of at least two of the powder, preferably Ti 2 AlC powder.
As a preferable technical scheme of the invention, the uniform mixing in the step (1) is carried out by ball milling.
As a preferable technical scheme of the invention, the grinding balls adopted by the ball milling are agate balls.
Preferably, the grinding balls are removed by sieving.
It is worth to say that the screening of the invention not only can remove grinding balls, but also can make the mixed powder after ball milling more fluffy, has higher fluidity and is more beneficial to the subsequent compression molding.
Preferably, the ball-milling ball mass ratio is (2-4): 1, such as 2:1, 2.3:1, 2.5:1, 2.8:1, 3:1, 3.3:1, 3.5:1, 3.6:1, 3.8:1 or 4:1, etc., but not limited to the recited values, other non-recited values within the range of values are equally applicable.
Preferably, the ball milling time is 5 to 10 hours, for example, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours, 8 hours, 8.5 hours, 9 hours, 9.5 hours or 10 hours, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In a preferred embodiment of the present invention, the pressure of the press molding in the step (2) is 50 to 200MPa, for example, 50MPa, 80MPa, 100MPa, 120MPa, 150MPa, 160MPa, 180MPa or 200MPa, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
As a preferable technical scheme of the invention, the high-temperature treatment in the step (3) comprises the steps of placing the mixed blank in the step (2) into an alumina crucible, and then placing the alumina crucible into a high-temperature furnace.
Preferably, the cooling of step (3) is furnace-wise cooling.
As a preferable embodiment of the present invention, the high temperature treatment in the step (3) is performed under an argon atmosphere or under a vacuum state.
Preferably, the target temperature of the high temperature treatment in the step (3) is 700 to 1100 ℃, for example, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃ or the like, but the target temperature is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
Preferably, the temperature rising rate of the high temperature treatment in the step (3) is 5 to 30 ℃/min, for example, 5 ℃/min, 8 ℃/min, 10 ℃/min, 13 ℃/min, 15 ℃/min, 17 ℃/min, 20 ℃/min, 23 ℃/min, 25 ℃/min, 27 ℃/min or 30 ℃/min, etc., but the temperature rising rate is not limited to the recited value, and other non-recited values within the range of the value are equally applicable.
Preferably, the heat-preserving time of the high temperature treatment in the step (3) is 5 to 120min, for example, 5min, 10min, 20min, 40min, 50min, 60min, 80min, 100min, 110min or 120min, etc., but not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Mixing: weighing MAX ceramic powder containing TiC structure and aluminum powder according to mass ratio, adopting ball milling and mixing uniformly, wherein grinding balls adopted by the ball milling are agate balls, controlling the mass ratio of ball materials to be (2-4): 1, the time to be 5-10 h, and adopting screening to remove the grinding balls to obtain mixed powder;
wherein the mass percentage of the MAX ceramic powder containing the TiC structure is 1-30 wt.%, and the balance is aluminum powder and unavoidable impurities; the MAX ceramic powder containing TiC structure comprises Ti 2 AlC powder, ti 3 AlC 2 Powder or Ti 3 SiC 2 Any one or the combination of at least two of the powder;
(2) And (5) press forming: pressing the mixed powder in the step (1) at 50-200 MPa to form a mixed blank;
(3) High temperature treatment: and (3) placing the mixed blank in the step (2) into an alumina crucible, placing the alumina crucible into a high-temperature furnace for high-temperature treatment, wherein the high-temperature treatment is performed under argon atmosphere or vacuum state, the temperature is increased to the target temperature of 700-1100 ℃ at the heating rate of 5-30 ℃/min, the heat preservation time is 5-120 min, and then cooling to room temperature along with the furnace to obtain the aluminum-titanium-carbon intermediate alloy refiner.
The second purpose of the invention is to provide an aluminum titanium carbon intermediate alloy refiner which is prepared by the preparation method of one purpose.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) According to the preparation method, MAX ceramic powder (ternary compound containing Ti element and C element) containing TiC structure is adopted as a Ti source and a C source, and TiC particles are formed through the high-temperature reaction of the ternary compound and Al and 'top-down' in-situ decomposition, so that an Al-Ti-C intermediate alloy refiner material containing TiC particles is obtained;
(2) According to the preparation method disclosed by the invention, MAX ceramic powder containing a TiC structure is adopted as an initial reactant, and TiC particles are formed by virtue of in-situ decomposition of the MAX ceramic powder and Al from top to bottom at high temperature, so that the problem of intermediate alloy inclusion caused by incomplete reactant reaction in the traditional bottom-to-top preparation method is avoided, and the preparation method has the advantages of simple process, environment friendliness, lower cost, convenience in material component design and the like, and is suitable for large-scale production.
Detailed Description
To facilitate understanding of the present invention, examples are set forth below. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a preparation method of an aluminum-titanium-carbon intermediate alloy refiner, which comprises the following steps:
(1) Mixing: weighing Ti according to mass proportion 2 Uniformly mixing AlC powder and aluminum powder by adopting ball milling, wherein grinding balls adopted by the ball milling are agate balls, the mass ratio of ball materials is controlled to be 3:1, the time is 8 hours, and screening is adopted to remove the grinding balls, so as to obtain mixed powder;
wherein, in the mass ratio, ti 2 21wt.% of AlC powder, and the balance of aluminum powder and unavoidable impurities;
(2) And (5) press forming: pressing and molding the mixed powder in the step (1) under 150MPa to obtain a mixed blank;
(3) High temperature treatment: and (3) placing the mixed blank in the step (2) into an alumina crucible, placing the alumina crucible into a high-temperature furnace for high-temperature treatment, wherein the high-temperature treatment is performed under argon atmosphere or vacuum state, the temperature is increased to the target temperature of 900 ℃ at the heating rate of 10 ℃/min, the heat preservation time is 60min, and then cooling to room temperature along with the furnace to obtain the aluminum-titanium-carbon intermediate alloy refiner.
Example 2
This example provides a method for preparing an aluminum titanium carbon master alloy refiner except for adding Ti in the mass ratio of step (1) 2 The mass percentage of AlC powder is changed from 21wt.% to 1wt.%, and the other conditions are exactly the same as in example 1.
Example 3
This example provides a method for preparing an aluminum titanium carbon master alloy refiner except for adding Ti in the mass ratio of step (1) 2 The mass percentage of AlC powder is changed from 21wt.% to 30wt.%, and the other conditions are exactly the same as in example 1.
Example 4
The embodiment provides a preparation method of an aluminum-titanium-carbon intermediate alloy refiner, which comprises the following steps:
(1) Mixing: weighing Ti according to mass proportion 3 AlC 2 The powder and aluminum powder are uniformly mixed by adopting ball milling, wherein grinding balls adopted by the ball milling are agate balls, the mass ratio of ball materials is controlled to be 4:1, the time is 5 hours, and the grinding balls are removed by sieving to obtain mixed powder;
wherein, in the mass ratio, ti 3 AlC 2 15wt.% of powder, and the balance of aluminum powder and unavoidable impurities;
(2) And (5) press forming: pressing and molding the mixed powder in the step (1) under 150MPa to obtain a mixed blank;
(3) High temperature treatment: and (3) placing the mixed blank in the step (2) into an alumina crucible, placing the alumina crucible into a high-temperature furnace for high-temperature treatment, wherein the high-temperature treatment is performed under argon atmosphere or vacuum state, the temperature is increased to the target temperature of 900 ℃ at the heating rate of 15 ℃/min, the heat preservation time is 60min, and then cooling to room temperature along with the furnace to obtain the aluminum-titanium-carbon intermediate alloy refiner.
Example 5
The embodiment provides a preparation method of an aluminum-titanium-carbon intermediate alloy refiner, which comprises the following steps:
(1) Mixing: weighing Ti according to mass proportion 2 Uniformly mixing AlC powder and aluminum powder by adopting ball milling, wherein grinding balls adopted by the ball milling are agate balls, the mass ratio of ball materials is controlled to be 2:1, the time is 10 hours, and screening is adopted to remove the grinding balls, so as to obtain mixed powder;
wherein, in the mass ratio, ti 2 21wt.% of AlC powder, and the balance of aluminum powder and unavoidable impurities;
(2) And (5) press forming: pressing and molding the mixed powder in the step (1) under 50MPa to obtain a mixed blank;
(3) High temperature treatment: and (3) placing the mixed blank in the step (2) into an alumina crucible, placing the alumina crucible into a high-temperature furnace for high-temperature treatment, wherein the high-temperature treatment is performed under argon atmosphere or vacuum state, the temperature is increased to the target temperature of 700 ℃ at the heating rate of 5 ℃/min, the heat preservation time is 120min, and then cooling to room temperature along with the furnace to obtain the aluminum-titanium-carbon intermediate alloy refiner.
Example 6
The embodiment provides a preparation method of an aluminum-titanium-carbon intermediate alloy refiner, which comprises the following steps:
(1) Mixing: weighing Ti according to mass proportion 2 Uniformly mixing AlC powder and aluminum powder by adopting ball milling, wherein grinding balls adopted by the ball milling are agate balls, the mass ratio of ball materials is controlled to be 4:1, the time is 5 hours, and screening is adopted to remove the grinding balls, so as to obtain mixed powder;
wherein, in the mass ratio, ti 2 21wt.% of AlC powder, and the balance of aluminum powder and unavoidable impurities;
(2) And (5) press forming: pressing and molding the mixed powder in the step (1) under 200MPa to obtain a mixed blank;
(3) High temperature treatment: and (3) placing the mixed blank in the step (2) into an alumina crucible, placing the alumina crucible into a high-temperature furnace for high-temperature treatment, wherein the high-temperature treatment is performed under argon atmosphere or vacuum state, the temperature is increased to the target temperature of 1100 ℃ at the heating rate of 30 ℃/min, the heat preservation time is 5min, and then cooling to room temperature along with the furnace to obtain the aluminum-titanium-carbon intermediate alloy refiner.
And (3) testing the refining effect:
pure aluminum was heated to melt and various amounts of the aluminum titanium carbon master alloy refiner described in example 1 were added, specifically in amounts corresponding to the Ti in the initial master alloy 2 The AlC content is calculated, the temperature is raised to 760 ℃ and kept for 30 to 60 minutes, and then the temperature is lowered to 720 ℃ for casting. Firstly, cutting, grinding, polishing and corroding a cast aluminum alloy sample according to national standard GB/T13298-2015 'method for testing a metal microstructure'; then, according to national standard GB/T6394-2017 'method for measuring average grain size of metals', the corroded sample is subjected to grain size analysis, and specific test analysis results are shown in Table 1:
TABLE 1
As can be seen from Table 1, when 0.1wt.% of the refiner was added, the grains of the aluminum matrix were refined from 1 to 2cm to about 700. Mu.m; when 0.6wt.% of the master alloy is added, the grains of the aluminum matrix are further refined to about 200 μm, which indicates that the Al-Ti-C grain refiner of the invention has good grain refining effect. As the amount of the refiner added increases, the aluminum matrix grain refining effect also gradually increases, mainly because the number of TiC particles in the refiner that exert the refining effect increases.
In summary, the preparation method disclosed by the invention adopts MAX ceramic powder (ternary compound containing Ti element and C element) containing TiC structure as a Ti source and a C source, and the TiC particles are formed by the high-temperature reaction of the ternary compound and Al and the 'top-down' in-situ decomposition, so that the problems of reactant residues, uneven diffusion of Ti element and C element and the like in the traditional 'bottom-up' preparation method are avoided, and the preparation method has the advantages of simple process, environment friendliness, lower cost, convenience in material component design and the like, and is suitable for large-scale production.
The applicant states that the detailed process equipment and process flows of the present invention are described by the above examples, but the present invention is not limited to, i.e., does not mean that the present invention must be practiced in dependence upon, the above detailed process equipment and process flows. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (18)
1. The preparation method of the aluminum-titanium-carbon intermediate alloy refiner is characterized by comprising the following steps of:
(1) Mixing: weighing MAX ceramic powder containing TiC structure and aluminum powder according to mass proportion, and uniformly mixing to obtain mixed powder; the MAX ceramic powder is a ternary compound containing Ti element and C element;
(2) And (5) press forming: pressing the mixed powder in the step (1) to form a mixed blank;
(3) High temperature treatment: and (3) carrying out high-temperature treatment on the mixed blank in the step (2), and cooling to obtain the aluminum-titanium-carbon intermediate alloy refiner.
2. The method according to claim 1, wherein the mass percentage of MAX ceramic powder containing TiC structure in the mass ratio in the step (1) is 1-30 wt.%, and the balance is aluminum powder and unavoidable impurities.
3. The method according to claim 1, wherein the MAX ceramic powder containing TiC structure in step (1) comprises Ti 2 AlC powder, ti 3 AlC 2 Powder or Ti 3 SiC 2 Any one or the combination of at least two of the powder.
4. The method according to claim 3, wherein the MAX ceramic powder containing TiC structure in step (1) is Ti 2 AlC powder.
5. The method of claim 1, wherein the step (1) of uniformly mixing is performed by ball milling.
6. The method according to claim 5, wherein the milling balls used for the ball milling are agate balls.
7. The method of claim 6, wherein the grinding balls are removed by sieving.
8. The method according to claim 5, wherein the ball mill has a ball mass ratio of (2-4): 1.
9. The method according to claim 5, wherein the ball milling time is 5 to 10 hours.
10. The method according to claim 1, wherein the pressure of the press molding in the step (2) is 50 to 200MPa.
11. The method of claim 1, wherein the high temperature treatment of step (3) comprises placing the mixed blank of step (2) into an alumina crucible, and then placing the alumina crucible into a high temperature furnace.
12. The method of claim 1, wherein the cooling in step (3) is furnace-wise cooling.
13. The method according to claim 1, wherein the high-temperature treatment in step (3) is performed under an argon atmosphere or under a vacuum state.
14. The method according to claim 1, wherein the target temperature of the high-temperature treatment in the step (3) is 700 to 1100 ℃.
15. The method according to claim 1, wherein the rate of temperature rise in the high temperature treatment in step (3) is 5 to 30 ℃/min.
16. The method according to claim 1, wherein the high temperature treatment in step (3) is carried out for a period of 5 to 120 minutes.
17. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
(1) Mixing: weighing MAX ceramic powder containing TiC structure and aluminum powder according to mass ratio, adopting ball milling and mixing uniformly, wherein grinding balls adopted by the ball milling are agate balls, controlling the mass ratio of ball materials to be (2-4): 1, the time to be 5-10 h, and adopting screening to remove the grinding balls to obtain mixed powder;
wherein the mass percentage of the MAX ceramic powder containing the TiC structure is 1-30 wt.%, and the balance is aluminum powder and unavoidable impurities; the MAX ceramic powder containing TiC structure comprises Ti 2 AlC powder, ti 3 AlC 2 Powder or Ti 3 SiC 2 Any one or the combination of at least two of the powder;
(2) And (5) press forming: pressing the mixed powder in the step (1) at 50-200 MPa to form a mixed blank;
(3) High temperature treatment: and (3) placing the mixed blank in the step (2) into an alumina crucible, placing the alumina crucible into a high-temperature furnace for high-temperature treatment, wherein the high-temperature treatment is performed under argon atmosphere or vacuum state, the temperature is increased to the target temperature of 700-1100 ℃ at the heating rate of 5-30 ℃/min, the heat preservation time is 5-120 min, and then cooling to room temperature along with the furnace to obtain the aluminum-titanium-carbon intermediate alloy refiner.
18. An aluminum-titanium-carbon intermediate alloy refiner, which is characterized by being prepared by the preparation method of any one of claims 1-17.
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