CN110229969B - Nano TiC particle reinforced aluminum-based composite material prepared by melt reaction method and method - Google Patents
Nano TiC particle reinforced aluminum-based composite material prepared by melt reaction method and method Download PDFInfo
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Abstract
The invention discloses a nano TiC particle reinforced aluminum-based composite material prepared by a melt reaction method and a method thereof, firstly, K is added2TiF6Mixing the powder and graphite powder according to the molar ratio of 1 (1-1.5), and then grinding to obtain mixed powder; then adding the mixed powder into an Al melt at the temperature of 800-900 ℃, performing ultrasonic dispersion and stirring treatment, and reacting to obtain a mixed melt; and finally, carrying out ultrasonic stirring treatment on the mixed melt, and then pouring to obtain the nano TiC ceramic particle reinforced aluminum matrix composite material. The invention can obtain the nano TiC particle reinforced aluminum matrix composite material through a simple preparation process.
Description
Technical Field
The invention belongs to the field of advanced aluminum matrix composite material preparation, and particularly relates to a method for preparing an in-situ nano TiC particle reinforced aluminum matrix composite material by an ultrasonic-assisted melt reaction method.
Background
The nano ceramic particles are introduced into a pure aluminum or aluminum alloy melt and then solidified to prepare the nano ceramic particle reinforced aluminum-based composite material, so that the specific strength, specific modulus and high-temperature creep resistance of aluminum (alloy) can be obviously improved, and the nano ceramic particle reinforced aluminum-based composite material has a very wide application prospect in the fields of aerospace, automobile manufacturing, electronic devices, sports equipment and the like. The in-situ endogenetic ceramic particles can be obtained in the aluminum melt by an in-situ reaction method, have good interface bonding property and chemical compatibility with a matrix, and can ensure that the aluminum matrix composite material has excellent comprehensive performance. In addition, the in-situ reaction method has the outstanding advantages of simple process, low cost, suitability for large-scale production and the like, and draws attention in the field of preparation of the particle reinforced aluminum matrix composite. However, the in situ generation of nano-scale ceramic particles within an aluminum melt is more difficult. At present, the particle size of in-situ endogenetic ceramic is mostly submicron and micron particle size. Taking in-situ generated TiC particles as an example, in the existing literature (CN102260814B), Ti powder, Al powder, and carbon nanotubes are used as raw materials, and the nano TiC particle reinforced aluminum matrix composite material is prepared by processes of mixing, compacting, combustion synthesis, and the like. In the literature (CN104532068B), Al powder, titanium powder, graphite powder, and NaCl are used as raw materials, and the pressed body is put into an aluminum melt to obtain in-situ TiC particles with a particle size of 0.1-1 μm. Therefore, obtaining nano-particle size in-situ generated TiC ceramic particles in an aluminum melt is difficult. Further exploring the synthesis of in-situ nano ceramic particles in the aluminum melt has very important significance for preparing high-performance nano particle reinforced aluminum matrix composite materials.
Disclosure of Invention
The invention aims to provide a nano TiC particle reinforced aluminum-based composite material prepared by a melt reaction method and a method thereof, so as to overcome the problems in the prior art. The invention can obtain the nano TiC particle reinforced aluminum matrix composite material through a simple preparation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a nano TiC particle reinforced aluminum matrix composite material by a melt reaction method comprises the following steps:
step 1: will K2TiF6Mixing the powder and graphite powder according to the molar ratio of 1 (1-1.5), and then grinding to obtain mixed powder;
step 2: adding the mixed powder into an Al melt at the temperature of 800-900 ℃, performing ultrasonic dispersion and stirring treatment, and reacting to obtain a mixed melt;
and step 3: and carrying out ultrasonic stirring treatment on the mixed melt, and then pouring to obtain the nano TiC ceramic particle reinforced aluminum matrix composite.
Further, K in step 12TiF6The purity of the powder and the graphite powder is more than 99 percent, and the granularity is less than 100 mu m.
Further, the ultrasonic agitation treatment in the step 2 specifically comprises: and immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the Al melt, wherein the ultrasonic power is 0.5-1.5kW, and the ultrasonic amplitude rod lasts for 5-10 min.
Further, after the ultrasonic dispersion stirring treatment is carried out in the step 2, the reaction is continued for 20-50min to obtain a mixed melt.
Further, the ultrasonic agitation treatment in the step 3 specifically comprises: and immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the mixed melt, wherein the ultrasonic power is 0.5-1.5kW, and the ultrasonic amplitude rod lasts for 5 min.
Further, the mass fraction of TiC in the nano TiC ceramic particle reinforced aluminum matrix composite material obtained in the step 3 is less than or equal to 10%.
A nanometer TiC particle reinforced aluminum-based composite material prepared by a melt reaction method is prepared by the method for preparing the nanometer TiC particle reinforced aluminum-based composite material by the melt reaction method.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention utilizes K2TiF6The powder and graphite powder are reactants, the processing is very simple, and the powder and the graphite powder can be added into the aluminum melt by simple mixing. After the mixed powder is added into the aluminum melt, high-strength ultrasound is introduced at the initial stage of the reaction, and the cavitation and acoustic flow effects of the ultrasound are utilized, so that the wettability of the graphite powder can be obviously improved, the graphite powder can easily enter the aluminum melt, participate in the reaction and effectively reduce burning loss; on the other hand, the ultrasonic acoustic flow effect can ensure that reactants are fully dispersed in the aluminum melt, thereby improving the synthesis efficiency of the nano TiC particles. The ultrasonic wave is applied before the casting, so that the synthesized nano TiC particles can be fully dispersed in the aluminum melt, and the nano TiC particle reinforced aluminum matrix composite material with uniform tissue can be obtained after the casting. The TiC synthesized by the process has the particle size less than 100nm and the average particle size of about 80 nm.
Drawings
FIG. 1 is an XRD diffraction pattern of the nano TiC particle reinforced aluminum matrix composite material prepared in example 1;
FIG. 2 is a microstructure photograph of the nano TiC particle reinforced aluminum matrix composite prepared in example 1;
fig. 3 is an enlarged photograph of TiC particles in the nano TiC particle reinforced aluminum matrix composite prepared in example 1.
Detailed Description
The invention is described in further detail below:
a method for preparing an in-situ nano TiC particle reinforced aluminum matrix composite material comprises the following steps:
step 1: k with the purity of more than 99 percent and the granularity of less than 100 mu m2TiF6The powder and graphite powder are prepared according to the following weight ratio of 1: (1-1.5) and then uniformly mixing to obtain mixed powder;
step 2: adding the mixed powder into an Al melt with the temperature of 800-900 ℃, immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, applying high-intensity ultrasound with the ultrasonic power of 0.5-1.5kW and the ultrasonic treatment time of 5-10min, and then continuing the reaction for 20-50min to obtain a mixed melt;
and step 3: before casting, an ultrasonic amplitude rod made of Nb-Zr alloy is immersed into the mixed melt and high-intensity ultrasonic is applied, the ultrasonic power is 0.5-1.5kW, the ultrasonic treatment time is 5min, liquid molten salt impurities on the surface of the melt are removed, and then the nano TiC ceramic particle reinforced aluminum-based composite material is obtained through casting, wherein the mass fraction of the nano TiC particles is less than or equal to 10%, and the adding amount of the mixed powder can be adjusted.
It should be noted that the base material may be selected from aluminum alloys other than pure aluminum.
The present invention is described in detail below with reference to examples:
example 1
Step 1: will K2TiF6Powder (purity greater than 99%, average particle size 20 μm), graphite powder (purity greater than 99%, average particle size 40 μm), according to 1: 1.2, and then uniformly mixing to obtain mixed powder;
step 2: adding the mixed powder into an Al melt with the temperature of 850 ℃, immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, applying high-intensity ultrasound with the ultrasonic power of 1.5kW for 5min, and then reacting for 30min to obtain a mixed melt;
and step 3: before casting, an ultrasonic amplitude rod made of Nb-Zr alloy is immersed into the mixed melt and high-intensity ultrasonic is applied, the ultrasonic power is 1.5kW, the ultrasonic treatment time is 5min, liquid molten salt impurities on the surface of the melt are removed, and then the nano TiC ceramic particle reinforced aluminum-based composite material is obtained through casting, wherein the mass fraction of the nano TiC particles is 7%.
Fig. 1 is an XRD diffraction pattern of the nano TiC particle reinforced aluminum matrix composite prepared by using an ultrasonic-assisted melt reaction process. As can be seen from the figure, the in-situ endogenetic enhancement particles are TiC phase, and no other phases are generated basically. FIG. 2 is a photograph of the microstructure of the composite material. As can be seen from the figure, under the action of high-intensity ultrasound, the obtained composite material has uniform microstructure and no obvious defects. FIG. 3 shows the in-situ TiC particle morphology in the composite material. As can be seen, the in-situ generated TiC particles have a particle size substantially less than 100nm and an average particle size of about 80 nm.
Example 2
Step 1: will K2TiF6Powder (purity greater than 99%, average particle size 20 μm), graphite powder (purity greater than 99%, average particle size 40 μm), according to 1: 1.1, and then uniformly mixing to obtain mixed powder;
step 2: adding the mixed powder into an Al melt with the temperature of 850 ℃, immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, applying high-intensity ultrasound with the ultrasonic power of 1.2kW for 5min, and then reacting for 50min to obtain a mixed melt;
and step 3: before casting, an ultrasonic amplitude rod made of Nb-Zr alloy is immersed into the mixed melt and high-intensity ultrasonic is applied, the ultrasonic power is 1.0kW, the ultrasonic treatment time is 5min, liquid molten salt impurities on the surface of the melt are removed, and then the nano TiC ceramic particle reinforced aluminum-based composite material is obtained through casting, wherein the mass fraction of the nano TiC particles is 10%.
Example 3
Step 1: will K2TiF6Powder (purity greater than 99%, average particle size 20 μm), graphite powder (purity greater than 99%, average particle size 40 μm), according to 1: 1.5, and then uniformly mixing to obtain mixed powder;
step 2: adding the mixed powder into an Al melt with the temperature of 800 ℃, immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, applying high-intensity ultrasound with the ultrasonic power of 1.5kW for 10min, and then reacting for 50min to obtain a mixed melt;
and step 3: before casting, an ultrasonic amplitude rod made of Nb-Zr alloy is immersed into the mixed melt and high-intensity ultrasonic is applied, the ultrasonic power is 1.5kW, the ultrasonic treatment time is 5min, liquid molten salt impurities on the surface of the melt are removed, and then the nano TiC ceramic particle reinforced aluminum-based composite material is obtained through casting, wherein the mass fraction of the nano TiC particles is 5%.
Example 4
Step 1: will K2TiF6Powder (purity greater than 99%, average particle size 20 μm), graphite powder (purity greater than 99%, average particle size 40 μm), according to 1: 1.3, and then uniformly mixing to obtain mixed powder;
step 2: adding the mixed powder into an Al melt with the temperature of 900 ℃, immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, applying high-intensity ultrasound with the ultrasonic power of 0.5kW for 5min, and then reacting for 20min to obtain a mixed melt;
and step 3: before casting, an ultrasonic amplitude rod made of Nb-Zr alloy is immersed into the mixed melt and high-intensity ultrasonic is applied, the ultrasonic power is 1.2kW, the ultrasonic treatment time is 5min, liquid molten salt impurities on the surface of the melt are removed, and then the nano TiC ceramic particle reinforced aluminum-based composite material is obtained through casting, wherein the mass fraction of the nano TiC particles is 5%.
Example 5
Step 1: will K2TiF6Powder (purity greater than 99%, average particle size 40 μm), graphite powder (purity greater than 99%, average particle size 20 μm), according to 1: 1, and then uniformly mixing to obtain mixed powder;
step 2: adding the mixed powder into an Al melt with the temperature of 900 ℃, immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the melt, applying high-intensity ultrasound with the ultrasonic power of 0.8kW for 8min, and then reacting for 20min to obtain a mixed melt;
and step 3: before casting, an ultrasonic amplitude rod made of Nb-Zr alloy is immersed into the mixed melt and high-intensity ultrasonic is applied, the ultrasonic power is 0.5kW, the ultrasonic treatment time is 5min, liquid molten salt impurities on the surface of the melt are removed, and then the nano TiC ceramic particle reinforced aluminum-based composite material is obtained through casting, wherein the mass fraction of the nano TiC particles is 5%.
Claims (2)
1. A method for preparing a nano TiC particle reinforced aluminum matrix composite material by a melt reaction method is characterized by comprising the following steps:
step 1: will K2TiF6Mixing the powder and graphite powder according to the molar ratio of 1 (1-1.5), and grinding to obtain mixed powder, wherein K2TiF6The purity of the powder and the graphite powder is more than 99 percent, and the granularity is less than 100 mu m;
step 2: adding the mixed powder into an Al melt with the temperature of 800-900 ℃, and performing ultrasonic dispersion stirring treatment, wherein the ultrasonic stirring treatment specifically comprises the following steps: immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the Al melt, wherein the ultrasonic power is 0.5-1.5kW, the ultrasonic time is 5-10min, and then continuously reacting for 20-50min to obtain a mixed melt;
and step 3: carrying out ultrasonic stirring treatment on the mixed melt, wherein the ultrasonic stirring treatment specifically comprises the following steps: and immersing an ultrasonic amplitude rod made of Nb-Zr alloy into the mixed melt, wherein the ultrasonic power is 0.5-1.5kW, the time is 5min, and then pouring to obtain the nano TiC particle reinforced aluminum-based composite material with the mass fraction of less than or equal to 10%, wherein the size of the nano TiC particles is less than 100 nm.
2. A nano TiC particle reinforced aluminum matrix composite material prepared by a melt reaction method is characterized by being prepared by the method for preparing the nano TiC particle reinforced aluminum matrix composite material by the melt reaction method in claim 1.
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| CN111378861B (en) * | 2020-03-24 | 2021-01-01 | 北京科技大学 | Preparation method of in-situ synthesized dual-phase particle reinforced aluminum matrix composite |
| CN112501468B (en) * | 2020-05-22 | 2022-04-22 | 武汉南瑞电力工程技术装备有限公司 | Smelting process of carbon nano tube reinforced aluminum-based composite material |
| TR202018737A2 (en) * | 2020-11-21 | 2021-06-21 | Cms Jant Ve Makina Sanayi Anonim Sirketi | Hybrid mixing system and method for using in aluminum matrix composite casting process |
| CN114934297B (en) * | 2022-05-23 | 2023-10-31 | 安徽工业大学 | Method for preparing aluminum-based composite material by composite electrodeposition in aluminum electrolyte containing nano particles |
| CN115505779A (en) * | 2022-10-08 | 2022-12-23 | 秦皇岛峰越科技有限公司 | Preparation method for in-situ generation of aluminum-based titanium carbide composite material |
| CN116377297B (en) * | 2023-04-13 | 2023-11-14 | 肇庆市大正铝业有限公司 | Hard aluminum alloy and preparation method thereof |
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Effective date of registration: 20221213 Address after: 712046 Floor 2, Building 7, Incubation Park, Gaoke Second Road, Xianyang Hi tech Industrial Development Zone, Shaanxi Province Patentee after: Xianyang Gazelle Valley New Material Technology Co.,Ltd. Address before: 710049 No. 28 West Xianning Road, Shaanxi, Xi'an Patentee before: XI'AN JIAOTONG University |