CN110747361A - Preparation method of titanium boride reinforced aluminum-based composite material based on ultrasonic and mechanical stirring - Google Patents
Preparation method of titanium boride reinforced aluminum-based composite material based on ultrasonic and mechanical stirring 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
Abstract
The invention relates to the field of metal alloy material preparation, and discloses a method for preparing titanium boride reinforced aluminum-based composite material based on ultrasonic and mechanical stirring, which comprises the steps of fully mixing potassium fluotitanate, potassium fluoborate reaction salt powder and sodium fluoroaluminate powder through mechanical stirring and drying for later use; placing an aluminum alloy ingot into a graphite crucible, heating until the temperature of an aluminum melt is stabilized at 800-850 ℃, adding the dried mixed powder into the aluminum melt, mechanically stirring, skimming scum when the temperature of the composite material is cooled to 720 ℃, pouring the composite material into a graphite mold, and cooling; putting the cooled sample into a graphite crucible again, heating the sample by using a resistance furnace until the sample is melted, and adding a high-energy ultrasonic radiation rod into the mixed meltCarrying out ultrasonic treatment on the mixed melt, pouring the mixed melt into a graphite mold after the ultrasonic treatment time is over, immediately cooling a sample by using liquid nitrogen, and thus obtaining the nano TiB in the nano titanium boride reinforced aluminum-based composite material2The particles are uniformly distributed and have no agglomeration phenomenon.
Description
Technical Field
The invention relates to the field of metal alloy material preparation, in particular to a preparation method of a titanium boride reinforced aluminum matrix composite material based on ultrasonic and mechanical stirring.
Background
The ceramic particle reinforced aluminum matrix composite has the advantages of high specific modulus, high hardness, high wear resistance and the like, and is widely applied to the fields of aerospace, automobile manufacturing and the like. Titanium boride (TiB)2) The composite material has the characteristics of high hardness, high thermal stability, corrosion resistance, no interface reaction with aluminum melt, good chemical stability and the like, and becomes a hotspot in the research of particle reinforced aluminum matrix composite materials. TiB2The nano particles are tightly combined with the alloy matrix, so that the properties of the matrix such as elastic modulus, yield strength, wear resistance and the like can be obviously improved.
However, a number of studies have shown that TiB is prepared by conventional addition methods2The wettability of the nano particles and the aluminum melt is poor, so that the nano particles are difficult to enter the aluminum melt; TiB prepared by in situ method2The nano particles have the problems of particle agglomeration, low particle yield and the like in the aluminum melt, which has adverse effect on the performance improvement of the aluminum matrix composite.
Disclosure of Invention
Based on the problems, the invention provides a preparation method of a titanium boride reinforced aluminum matrix composite material based on ultrasonic and mechanical stirring, which comprises the steps of uniformly mixing reaction salt and cosolvent powder, adding the reaction salt and the cosolvent powder into an aluminum melt, increasing the contact area of the reaction salt in a molten state and the aluminum melt in a mechanical stirring manner by using a stirrer, accelerating the reaction rate, promoting the reaction, improving the yield of reactants, skimming scum, pouring into a mold and cooling; remelting the cooled sample, and performing ultrasonic treatment on the remelted mixed melt by using a high-energy ultrasonic radiation rodTreating, pouring into a mold, cooling with liquid nitrogen, and finally obtaining the nano TiB in the nano titanium boride reinforced aluminum-based composite material2The particles are uniformly distributed and have no agglomeration phenomenon.
In order to solve the technical problems, the invention adopts the technical scheme that:
the preparation method of the titanium boride reinforced aluminum-based composite material based on ultrasonic and mechanical stirring comprises the following steps:
s1: weighing a certain mass of aluminum alloy ingot for later use;
s2: by pre-forming 3 vol% of TiB in a reinforced aluminum matrix composite2Weighing potassium fluotitanate and potassium fluoborate reaction salt powder by using particles, wherein the mass of cosolvent sodium fluoaluminate powder is 10 percent of the total mass of two reaction salts of potassium fluotitanate and potassium fluoborate, fully mixing by mechanical stirring, and drying in a drying furnace at the temperature of 200-300 ℃ for 1-2 hours for later use;
s3: putting the weighed aluminum alloy ingot into a graphite crucible, heating the aluminum alloy ingot by using a resistance furnace, adding the dried mixed powder into an aluminum melt when the temperature of the aluminum melt is stabilized at 800-850 ℃, mechanically stirring the aluminum melt, skimming scum when the temperature of the composite material is cooled to 720 ℃, pouring the aluminum alloy ingot into a graphite mold preheated at 300 ℃ and cooling the aluminum alloy ingot;
s4: putting the cooled sample into a graphite crucible again, heating the sample to 720 ℃ by using a resistance furnace to melt the sample to form a mixed melt, adding a high-energy ultrasonic radiation rod into the mixed melt, controlling the ultrasonic frequency to be 18-20 KHz, the power to be 1-2 KW and the amplitude to be 10-15 mu m, controlling the immersion depth of the ultrasonic radiation rod to be 15-25 mm, and controlling the ultrasonic treatment time to be 30-240 s;
s5: and after the ultrasonic treatment time is finished, pouring the mixed melt into a graphite mold preheated at 300 ℃, and cooling by using liquid nitrogen to obtain the final nano titanium boride reinforced aluminum matrix composite.
Furthermore, one end of the ultrasonic radiation rod is connected into the ultrasonic transducer, and the other end of the ultrasonic radiation rod is immersed into the mixed melt in the graphite crucible; the transducer is electrically connected with the ultrasonic power supply.
Further, the aluminum alloy ingot was a 2Al4 aluminum alloy.
Further, in the step S3, the adding time of the reaction salt and the cosolvent is controlled to be 15-25S, and a stirrer is used for mechanical stirring when the reaction salt and the cosolvent are added, wherein the stirring speed is 150rpm, and the stirring time is 30 min.
Furthermore, a thermocouple for measuring the temperature of the mixed melt is arranged in the graphite crucible, the signal output end of the thermocouple is electrically connected with a data collector, and the data collector is in communication connection with a computer terminal.
Compared with the prior art, the invention has the beneficial effects that:
1) firstly, uniformly mixing reaction salt and cosolvent powder, then adding the reaction salt and the cosolvent powder into an aluminum melt, simultaneously adopting a stirrer to increase the contact area of the reaction salt in a molten state and the aluminum melt in a mechanical stirring manner, accelerating the reaction rate, promoting the reaction to proceed, improving the yield of reactants, and then skimming scum and pouring the scum into a mold for cooling; remelting the cooled sample, performing ultrasonic treatment on the remelted mixed melt by using a high-energy ultrasonic radiation rod, pouring the mixture into a mold, cooling the mixture by using liquid nitrogen, and finally obtaining the nano TiB in the nano titanium boride reinforced aluminum-based composite material2The particles are uniformly distributed and have no agglomeration phenomenon.
2) The fine mesh Cu in the microstructure of the aluminum-based composite material obtained by the invention2Al phase distributed in Al base, nano TiB2The particles are uniformly distributed and have no agglomeration phenomenon; the process is safe, reliable, economical, efficient and simple to operate.
3) The composite material is subjected to mechanical property detection, and compared with the composite material prepared by a common method, the composite material prepared by the technical scheme of the patent has the advantages that the performance is greatly improved, the yield strength, the tensile strength and the hardness are respectively improved by 54%, 21% and 27%, meanwhile, the abrasion quality is reduced by 37%, and the abrasion resistance is improved.
Drawings
FIG. 1 is a process for preparing TiB according to the present invention2A mechanical stirring schematic diagram of the/2A 14 aluminum matrix composite material;
FIG. 2 is a schematic diagram of the preparation of TiB according to the present invention2Ultrasonic treatment of/2A 14 aluminum matrix compositesA schematic diagram;
FIG. 3 is a process for preparing TiB according to the present invention2The microstructure of the/2A 14 aluminum matrix composite;
wherein, 1, a stirrer; 2. a graphite crucible; 3. a reaction salt; 4. an aluminum melt; 5. mixing the melt; 6. a resistance furnace; 7. an ultrasonic power supply; 8. a transducer; 9. an ultrasonic radiation rod; 10. a thermocouple; 11. a data acquisition unit; 12. and (4) a computer terminal.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1:
referring to fig. 1 and 2, the preparation method of the titanium boride reinforced aluminum matrix composite material based on ultrasonic and mechanical stirring comprises the following steps:
s1: weighing a certain mass of aluminum alloy ingot for later use;
s2: by pre-forming 3 vol% of TiB in a reinforced aluminum matrix composite2Weighing potassium fluotitanate and potassium fluoborate reaction salt 3 powder by using particles, wherein the mass of cosolvent sodium fluoaluminate powder is 10 percent of the total mass of potassium fluotitanate and potassium fluoborate reaction salt 3, fully mixing by mechanical stirring, and drying in a drying furnace at 200-300 ℃ for 1-2 hours for later use;
s3: putting the weighed aluminum alloy ingot into a graphite crucible 2, heating by using a resistance furnace 6, adding the dried mixed powder into an aluminum melt 4 when the temperature of the aluminum melt 4 is stabilized at 800-850 ℃, mechanically stirring, skimming scum when the temperature of the composite material is cooled to 720 ℃, pouring into a graphite mold preheated at 300 ℃ and cooling;
s4: putting the cooled sample into the graphite crucible 2 again, heating the sample to 720 ℃ by using a resistance furnace 6 to melt the sample to form a mixed melt 5, adding a high-energy ultrasonic radiation rod 9 into the mixed melt 5, controlling the ultrasonic frequency to be 18-20 KHz, the power to be 1-2 KW and the amplitude to be 10-15 mu m, controlling the immersion depth of the ultrasonic radiation rod 9 to be 15-25 mm, and controlling the ultrasonic treatment time to be 30-240 s;
s5: and after the ultrasonic treatment time is finished, pouring the mixed melt 5 into a graphite mold preheated at 300 ℃, and cooling by using liquid nitrogen to obtain the final nano titanium boride reinforced aluminum matrix composite.
In this example, potassium fluorotitanate (K)2TiF6) Potassium fluoroborate (KBF)4) Cosolvent sodium fluoroaluminate (Na)3AlF6) The quality of the powder is chemically pure, and the following in-situ chemical reactions occur in the aluminum melt 4:
3K2TiF6+6KBF4+10Al→3TiB2+9KAlF4+K3AlF6
the reaction can generate nano-scale TiB with no pollution on the surface2The particles greatly improve the wettability of the nano particles and the aluminum melt 4, and facilitate the interface combination of the particles and the matrix. The cavitation effect and acoustic flow effect generated by the high-energy ultrasound in the aluminum melt 4 can promote wetting of particles, break up agglomeration of the particles and greatly help uniform distribution of the particles. The aluminum-based composite material with uniformly distributed particles under the ultrasonic action can be obtained by using liquid nitrogen for cooling, so that the phenomenon of re-agglomeration of particles caused by sedimentation of the particles by gravity in the traditional cooling mode is avoided. The aluminum matrix composite material obtained in the embodiment has fine mesh Cu in microstructure2Al phase distributed in Al base, nano TiB2The particles are uniformly distributed and have no agglomeration phenomenon. The process is safe, reliable, economical, efficient and simple to operate.
In this embodiment, in step S3, the adding time of the reaction salt 3 and the cosolvent is controlled to be 15-25S, and the stirrer 1 is used for mechanical stirring when the reaction salt 3 and the cosolvent are added, the stirring speed is 150rpm, and the stirring time is 30 min.
One end of an ultrasonic radiation rod 9 is connected into an ultrasonic transducer 8, and the other end is immersed into the mixed melt 5 in the graphite crucible 2; the transducer 8 is electrically connected with the ultrasonic power supply 7. The ultrasonic power supply 7 provides working current for the transducer 8, the transducer 8 converts electric energy into mechanical energy of ultrasonic vibration, and the nano TiB in the composite melt is obtained after the ultrasonic radiation rod 9 is immersed in the composite melt2The particles are uniformly dispersed in the aluminum melt 4 under the ultrasonic treatment, and no agglomeration phenomenon is generated.
In the embodiment, a thermocouple 10 for measuring the temperature of the mixed melt 5 is arranged in the graphite crucible 2, the signal output end of the thermocouple 10 is electrically connected with a data acquisition unit 11, and the data acquisition unit 11 is in communication connection with a computer terminal 12. The temperature of the melt in the heating, stirring and ultrasonic processing processes is collected by the thermocouple 10, processed by the data collector 11 and converted into a temperature value, and the temperature value is transmitted to the computer terminal 12 for display, so that an operator can know the temperature in the preparation process conveniently to perform corresponding recording and control.
Example 2:
referring to fig. 1 and 2, 500g of 2a14 aluminum alloy ingot is weighed, the weighed 2a14 aluminum alloy ingot is placed in a graphite crucible 2, the graphite crucible is heated by a resistance furnace 6 to be melted, and 3 vol% of TiB is pre-generated according to an in-situ reaction equation2Weighing potassium fluotitanate (K) by using particles2TiF6) Potassium fluoroborate (KBF)4) 88.33g and 92.75g of reaction salt 3 powder respectively, and then cosolvent sodium fluoroaluminate (Na)3AlF6) Has a mass of 18.11 g. Fully mixing by mechanical stirring, drying in a drying furnace at 200 ℃ for 2h, adding the dried mixed powder into the aluminum melt 4 when the temperature of the aluminum melt 4 is stabilized at 820 ℃, wherein the adding time is 15s, mechanical stirring is introduced in the adding process, the stirring speed is 150rpm, and the stirring time is 30 min; when the temperature of the composite material is cooled to 720 ℃, skimming scum, and pouring the composite material into a graphite mold which is preheated at 300 ℃ for cooling. And putting the cooled sample into the graphite crucible 2 again, heating the sample to 720 ℃ by using a resistance furnace 6 to melt the sample to form a mixed melt 5, adding high-energy ultrasound into the mixed melt 5, wherein the ultrasonic frequency is 20KHz, the power is 1KW, the amplitude is 12 mu m, the immersion depth of an ultrasonic radiation rod 9 is 20mm, the ultrasonic treatment time is 90s, and after the ultrasonic treatment time is over, pouring the mixed melt 5 into a graphite mold preheated at 300 ℃ and cooling the graphite mold by using liquid nitrogen to obtain the final nano titanium boride reinforced aluminum-based composite material.
Example 3:
referring to FIGS. 1-3, first weigh 550g of 2A14 aluminum alloy ingot, putting the weighed 2A14 aluminum alloy ingot into a graphite crucible 2, heating the ingot by a resistance furnace 6 until the ingot is melted, and pre-generating 3 vol% of TiB according to an in-situ reaction equation2Weighing potassium fluotitanate (K) by using particles2TiF6) Potassium fluoroborate (KBF)4) 97.17g and 102.03g of reaction salt 3 powder respectively, and then sodium fluoroaluminate (Na) as cosolvent3AlF6) Has a mass of 19.92 g. Fully mixing by mechanical stirring, drying in a drying furnace at 300 ℃ for 1h, adding the dried mixed powder into the aluminum melt 4 when the temperature of the aluminum melt 4 is stabilized at 830 ℃, wherein the adding time is 20s, and mechanical stirring is introduced during the adding process, the stirring speed is 150rpm, and the stirring time is 30 min; when the temperature of the composite material is cooled to 720 ℃, skimming scum, and pouring the composite material into a graphite mold which is preheated at 300 ℃ for cooling. And putting the cooled sample into the graphite crucible 2 again, heating the sample to 720 ℃ by using the resistance furnace 6 to melt the sample to form a mixed melt 5, adding high-energy ultrasound into the mixed melt 5, wherein the ultrasonic frequency is 19KHz, the power is 2KW, the amplitude is 15 mu m, the immersion depth of the ultrasonic radiation rod 9 is 25mm, the ultrasonic treatment time is 120s, and after the ultrasonic treatment time is over, pouring the mixed melt 5 into a graphite mold preheated at 300 ℃ and cooling the mixed melt by using liquid nitrogen to obtain the final nano titanium boride reinforced aluminum-based composite material.
As-cast TiB2As shown in FIG. 3, the microstructure of the aluminum-based composite material/2A 14 showed that coarse dendritic primary crystals were not present in the microstructure of the aluminum-based composite material, and that the primary α -Al phase was in the TiB phase2Under the effect of particle and ultrasonic cavitation, the grain is obviously refined. Under the synergistic action of ultrasonic cavitation and ultrasonic acoustic flow, no obvious particle agglomeration and TiB (titanium boron) in the composite material occur2The particles are uniformly distributed in the tissue.
By detecting the mechanical property of the composite material obtained by the embodiment, compared with the composite material prepared by a common method, the performance of the composite material prepared by the technical scheme is greatly improved, the yield strength, the tensile strength and the hardness are respectively improved by 54 percent, 21 percent and 27 percent, meanwhile, the abrasion quality is reduced by 37 percent, and the abrasion resistance is improved.
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the process of verifying the invention and are not intended to limit the scope of the invention, which is defined by the claims, and all the equivalent structural changes made by applying the content of the specification of the invention should be covered by the scope of the invention.
Claims (5)
1. The preparation method of the titanium boride reinforced aluminum matrix composite material based on ultrasonic and mechanical stirring is characterized by comprising the following steps:
s1: weighing a certain mass of aluminum alloy ingot for later use;
s2: by pre-forming 3 vol% of TiB in a reinforced aluminum matrix composite2Weighing potassium fluotitanate and potassium fluoborate reaction salt powder by using particles, wherein the mass of cosolvent sodium fluoaluminate powder is 10 percent of the total mass of two reaction salts of potassium fluotitanate and potassium fluoborate, fully mixing by mechanical stirring, and drying in a drying furnace at the temperature of 200-300 ℃ for 1-2 hours for later use;
s3: putting the weighed aluminum alloy ingot into a graphite crucible, heating the aluminum alloy ingot by using a resistance furnace, adding the dried mixed powder into an aluminum melt when the temperature of the aluminum melt is stabilized at 800-850 ℃, mechanically stirring the aluminum melt, skimming scum when the temperature of the composite material is cooled to 720 ℃, pouring the aluminum alloy ingot into a graphite mold preheated at 300 ℃ and cooling the aluminum alloy ingot;
s4: putting the cooled sample into a graphite crucible again, heating the sample to 720 ℃ by using a resistance furnace to melt the sample to form a mixed melt, adding a high-energy ultrasonic radiation rod into the mixed melt, controlling the ultrasonic frequency to be 18-20 KHz, the power to be 1-2 KW and the amplitude to be 10-15 mu m, controlling the immersion depth of the ultrasonic radiation rod to be 15-25 mm, and controlling the ultrasonic treatment time to be 30-240 s;
s5: and after the ultrasonic treatment time is finished, pouring the mixed melt into a graphite mold preheated at 300 ℃, and cooling by using liquid nitrogen to obtain the final nano titanium boride reinforced aluminum matrix composite.
2. The method for preparing titanium boride reinforced aluminum matrix composite based on ultrasonic and mechanical stirring as claimed in claim 1, wherein: one end of the ultrasonic radiation rod is connected into the ultrasonic transducer, and the other end of the ultrasonic radiation rod is immersed into the mixed melt in the graphite crucible; the transducer is electrically connected with the ultrasonic power supply.
3. The method for preparing titanium boride reinforced aluminum matrix composite based on ultrasonic and mechanical stirring as claimed in claim 2, wherein: the aluminum alloy ingot is 2Al4 aluminum alloy.
4. The method for preparing titanium boride reinforced aluminum matrix composite based on ultrasonic and mechanical stirring as claimed in claim 2 or 3, wherein: and S3, controlling the adding time of the reaction salt and the cosolvent to be 15-25S, and mechanically stirring by using a stirrer when the reaction salt and the cosolvent are added, wherein the stirring speed is 150rpm, and the stirring time is 30 min.
5. The method for preparing titanium boride reinforced aluminum matrix composite based on ultrasonic and mechanical stirring as claimed in claim 4, wherein: a thermocouple for measuring the temperature of the mixed melt is arranged in the graphite crucible, the signal output end of the thermocouple is electrically connected with a data acquisition unit, and the data acquisition unit is in communication connection with a computer terminal.
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| CN112195358A (en) * | 2020-10-14 | 2021-01-08 | 广东省科学院材料与加工研究所 | Aluminum-based alloy, aluminum-based composite material, and preparation method and application thereof |
| CN112301298A (en) * | 2020-09-22 | 2021-02-02 | 哈尔滨工业大学（威海） | Light heat-resistant high-rigidity multi-element reinforced aluminum-based composite material and preparation method thereof |
| CN112708804A (en) * | 2020-12-18 | 2021-04-27 | 江苏大学 | Graphene and in-situ nanoparticle reinforced aluminum-based composite material and preparation method thereof |
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| CN112301298A (en) * | 2020-09-22 | 2021-02-02 | 哈尔滨工业大学（威海） | Light heat-resistant high-rigidity multi-element reinforced aluminum-based composite material and preparation method thereof |
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| CN112708804A (en) * | 2020-12-18 | 2021-04-27 | 江苏大学 | Graphene and in-situ nanoparticle reinforced aluminum-based composite material and preparation method thereof |
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| CN113504155A (en) * | 2021-05-27 | 2021-10-15 | 郑州大学 | Device and method for detecting particle wettability in water by ultrasonic waves |
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