CN108251670B - Preparation method of high-temperature-resistant intermetallic compound alloy - Google Patents
Preparation method of high-temperature-resistant intermetallic compound alloy Download PDFInfo
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Abstract
The invention relates toA preparation method of a high-temperature resistant intermetallic compound alloy belongs to the field of preparation of high-temperature resistant materials. Firstly, preparing raw materials of Mo-Si-B alloy according to weight percentage, wherein Mo: 70-89%, Si: 10-25%, B: 1-5%; and then, performing low-temperature pre-sintering on the raw materials by adopting a powder metallurgy method to form lump materials, and performing high-temperature synthesis by adopting an electron beam melting method to obtain the high-temperature resistant intermetallic compound alloy lump. The Mo-Si-B alloy obtained by casting has uniform chemical components and full compactness without holes, and the metallographic structure of the Mo-Si-B alloy obtained by casting is alpha-Mo and Mo3Si and Mo5SiB2。
Description
Technical Field
The invention relates to a preparation method of a high-temperature resistant intermetallic compound alloy, and main metals and compounds related to the compound alloy comprise alpha-Mo and Mo3Si and Mo5SiB2. The invention belongs to the field of preparation of high-temperature resistant materials.
Background
In modern industry, high temperature processes are becoming more common, which places higher demands on the use temperatures of some high temperature structural materials, such as turbines, aircraft engine blades, heat exchangers and heating elements. Structural materials used in high temperature environments should have sufficiently high service temperatures, oxidation resistance and fracture toughness, and in order to achieve these desirable properties, new materials must be developed. Intermetallic compounds that may be used at high temperatures have been extensively studied. Mo-Si-B alloy is used as a structural material and a high-temperature oxidation-resistant coating material for the latest generation of aeroengines, and a great deal of research is carried out abroad and breakthrough progress is obtained. Research results show that the Mo-Si-B series alloy added with boron has excellent high-temperature mechanical property and can be matched with MoSi2Compared with excellent high-temperature oxidation resistance.
High-temperature structural use with metal aluminides (mainly Ni-Al, Ti-Al and Fe-Al systems) as mainstream since the end of the 70 sIntermetallic compounds have been studied extensively and intensively. Currently, modified structure aluminides, in particular Ti-Al and Ni-Al based compound alloys (mainly Ni)3Al and Ti3A1) And composites thereof have entered the research phase of engineering applications. Ni3Al and Ti3Aluminides such as A1 have good room temperature plasticity and high specific strength, but have poor oxidation resistance at a temperature higher than 650 ℃, and need to be coated with a protective coating. Ti-Al alloys also exhibit poor oxidation resistance at temperatures above 800 ℃; al (Al)3Ti has the disadvantages of low melting point (1340 deg.C) and narrow composition range.
Starting from the end of the 80 s, metal silicides (in particular MoSi) for structures were used2) Have been studied intensively. MoSi2Has high melting point (2030 ℃) and excellent high-temperature oxidation resistance, the using temperature of the heating element used as a high-temperature industrial furnace reaches 1800 ℃, however, MoSi2The room temperature mechanical property and the high temperature creep resistance of the base alloy are poor, and PEST oxidation is easy to occur at about 500 ℃. Mo5Si3Is also a structural material which can be used in high temperature environment and has creep resistance superior to MoSi2But the high temperature oxidation resistance is very poor.
Mo-Si-B alloy is used as a structural material and a high-temperature oxidation-resistant coating material for the latest generation of aeroengines. The current research on Mo-Si-B alloys is mainly focused on two systems: alpha-Mo + Mo3Si+Mo5SiB2(T2)；Mo5Si3(T1)+Mo3Si+Mo5SiB2(T2)。
The current methods for preparing Mo-Si-B alloys can be divided into two categories: arc melting and powder metallurgy. The powder metallurgy method can be divided into a powder sintering/pressing method, a combustion synthesis method (self-propagating high-temperature synthesis), a reaction hot pressing method, a discharge plasma sintering method, a mechanical alloying method and the like.
The electric arc melting has the advantages of simple equipment, low energy requirement, instant synthesis and the like, but has the main defects that holes and cracks are generated in the prepared material, and the mechanical processing is not facilitated. In addition, for Mo-Si-B alloy, higher melting temperature is needed to overcome the obstruction of high melting point of silicide; during smelting, silicon loss caused by volatilization can generate some undesirable intermediate phases, reduce the mechanical properties of the material and cause non-uniform components.
Pressing/sintering is a traditional powder metallurgy process in which the pressing stage employs both Cold Isostatic Pressing (CIP) and Hot Isostatic Pressing (HIP). The cold isostatic pressing can ensure that the density distribution of the sample is uniform; the hot isostatic pressing can eliminate the inner pores and defects of the product and improve the density. The traditional powder metallurgy method has simple and mature process, but the obtained Mo-Si-B alloy has lower density and certain pores.
Self-propagating high-temperature synthesis (SHS) is to ignite powder compact in a certain atmosphere, the temperature of the adjacent materials is suddenly raised by the generated heat released from chemical reaction to keep the reaction continuously, and reactants are converted into products when the combustion wave advances forward. The product prepared by the technology has high purity, low energy consumption and quick and simple process. But the main problems are that the product has more pores, the density is lower and the synthesis process is difficult to control.
Reactive hot pressing is a technique in which a powder mixture is put in a die while being heated and pressurized, a combustion reaction is ignited, and molding, synthesis and sintering are performed in the same process by utilizing the reaction and heat release between powders. The reaction hot pressing can make the product obtain the density which can not be achieved by cold pressing and reaction sintering under the condition of lower pressure, and can complete densification in a shorter time at a lower temperature than that of the common hot pressing, and fine grain structures can be easily obtained.
Spark Plasma Sintering (SPS) can prepare a material with uniform tissue, fine grains and high density at an extremely short sintering time and a relatively low sintering temperature. The unique plasma activation and rapid sintering effects of the material inhibit the growth of crystal grains. The microstructure of the original particles is well maintained, thereby essentially improving the material performance.
Mechanical Alloying (MA) is a complex physicochemical process in which the powder is subjected to repeated deformation, cold welding and crushing by high-energy ball milling, thereby achieving the level alloying of atoms between elements. The mechanical alloying realizes alloying in a solid state, can avoid a complex solidification process, and has simple and economic process conditions; uniform and fine microstructures and dispersed strengthening phases can be obtained, so that the toughness of intermetallic compounds is improved, and the processing performance is improved; can not be melted completely, and is particularly suitable for the alloying of refractory metals. However, the mechanical alloying method has some problems, such as contamination of powder material caused by abrasion doping of milling pot and milling ball during high energy ball milling.
Disclosure of Invention
The invention aims to provide a synthesis preparation method of a high-temperature resistant intermetallic compound, wherein main metals and compounds related to the compound comprise alpha-Mo and Mo3Si and Mo5And SiB. A new method is used for preparing the fully-compact Mo-Si-B alloy with uniform components.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-temperature resistant intermetallic compound alloy comprises the following steps:
(1) preparing raw materials of the Mo-Si-B alloy according to the weight percentage, wherein the weight percentage of Mo: 70-89%, Si: 10-25%, B: 1-5%;
(2) performing low-temperature pre-sintering on the raw materials in the step (1) by adopting a powder metallurgy method to form lump materials, and performing high-temperature synthesis by adopting an electron beam melting method to obtain high-temperature-resistant intermetallic compound alloy lumps;
(3) and mechanically crushing the synthesized alloy block to obtain heat-resistant alloy powder with different particle size distributions, pressing and molding the powder and sintering at high temperature to obtain an alloy part blank with uniform components and low impurity content.
In the method, in the step (1), silicon can be added in the form of molybdenum silicide in the raw materials so as to reduce excessive volatilization of silicon in the fusion casting process.
In the step (2), the preparation method of the high-temperature resistant intermetallic compound alloy block specifically comprises the following steps:
(a) the raw material powder is proportioned and mixed according to the above component proportion, the uniformly mixed raw material powder is subjected to cold isostatic pressing on a cold isostatic pressing machine, and a blank is obtained; the pressure of the cold isostatic pressing is 150-250 MPa, and the pressure maintaining time is 5-20 minutes;
(b) pre-sintering the obtained blank, wherein the pre-sintering process comprises the following steps: heating at a heating rate of 5-10 ℃/min, wherein the pre-sintering temperature is 1000-1200 ℃, the pre-sintering time is 1-2 hours, then cooling to room temperature along with the furnace, and the pre-sintering atmosphere is hydrogen to obtain a pre-sintered bar;
(c) and (3) melting the pre-sintered bar by using electron beams to synthesize an intermetallic compound at a high temperature of 2500-3000 ℃, wherein the melting time is 1-10 minutes, and cooling the ingot along with the furnace after the synthesis reaction.
In the step (3), silicon, boron and/or compounds thereof are added again to the heat-resistant alloy powder obtained by mechanical crushing, and the addition amount of silicon and/or boron elements is increased appropriately to obtain the desired chemical composition. Preferably, 5 to 20 wt.% of excess silicon is added, and 5 to 20 wt.% of excess boron is added, that is, the weight of the added silicon is 5 to 20% of the weight of the added silicon in the step (1), and the weight of the added boron is 5 to 20% of the weight of the added boron in the step (1).
In the step (3), the synthesized alloy block is mechanically crushed to obtain heat-resistant alloy powder with different particle sizes meeting the requirements, and then the powder is pressed, formed and sintered at high temperature to finally obtain an alloy part blank with uniform components and low impurity content, and the method comprises the following steps:
(i) ball-milling an intermetallic compound alloy block synthesized by electron beam melting by using a ball mill to obtain alloy powder with different particle sizes, wherein the rotating speed of the ball mill is 100-;
(ii) uniformly stirring the ball-milled powder or the ball-milled powder and other alloy powder (excessive silicon, boron and/or compounds thereof) and then performing compression molding to obtain a blank; the pressing pressure is 150-250 MPa, and the pressure maintaining time is 5-20 minutes;
(iii) and sintering the obtained blank at a high temperature, wherein the pre-sintering process comprises the following steps: heating at a heating rate of 5-10 ℃/min, wherein the pre-sintering temperature is 1500-1800 ℃, the pre-sintering time is 1-2 hours, and then cooling to room temperature along with the furnace, wherein the pre-sintering atmosphere is hydrogen, so as to obtain a sintered bar.
The invention has the advantages that:
1. the intermetallic compound powder synthesized by the electron beam melting at high temperature has high purity, low impurity content and uniform chemical composition.
2. The main phases of the intermetallic compound alloy obtained after the electron beam high-temperature synthesis are respectively alpha-Mo and Mo3Si and Mo5SiB2。
3. The component proportion of the intermetallic compound alloy can be adjusted according to different requirements, so that the alloy meeting different requirements can be obtained.
4. The synthesis of the intermetallic compound is a chemical reaction process finished by the water-cooled copper crucible through electron beam processing, and the problem of secondary pollution cannot be caused in the synthesis process.
5. The preparation process of the sintered blank adopts a powder metallurgy method, so that the final sintered blank has fine microstructure, uniform components and full compactness without holes.
6. The alloy of the invention has good performance at the temperature of over 1200 ℃.
Drawings
FIG. 1 is a metallographic structure diagram of a high temperature resistant Mo-Si-B alloy prepared in example 1.
Detailed Description
Example 1
The present example was prepared according to the following alloy composition (weight percentage): mo: 87.52%, Si 11.32%, B: 1.16 percent. The silicon is added in the form of molybdenum silicide to reduce excessive volatilization of silicon during the casting process. And (3) mixing the raw material powder according to the component proportion, wherein the rotating speed of a mixer is 60 revolutions per minute, and the mixing is carried out for 12 hours.
And (3) carrying out cold isostatic pressing on the uniformly mixed raw material powder on a 220MPa cold isostatic press for 8 minutes to obtain a phi 25-30 mm rod with certain compactness.
Pre-sintering the obtained blank, wherein the pre-sintering process comprises the following steps: heating at the heating rate of 10 ℃/min, wherein the pre-sintering temperature is 1000 ℃, the pre-sintering time is 2 hours, and then cooling to room temperature along with the furnace, wherein the pre-sintering atmosphere is hydrogen, so as to obtain the pre-sintered bar stock.
And (3) melting the pre-sintered bar by utilizing an electron beam to synthesize an intermetallic compound at a high temperature of 2800 ℃ for 3 minutes, and cooling the ingot along with the furnace after the synthesis reaction.
And (3) carrying out ball milling on the intermetallic compound alloy block synthesized by electron beam melting by using a ball mill to obtain alloy powder with different particle sizes, wherein the rotating speed of the ball mill is 200 r/min, the ball-to-material ratio of the ball mill is 10:1, and the average particle size of the obtained powder is 3 microns.
And uniformly stirring the ball-milled powder, 5 wt.% of excessive silicon and 5 wt.% of excessive boron powder, and then performing compression molding to obtain a blank. The pressing pressure is 200MPa, and the dwell time is 10 minutes.
Sintering the obtained blank at high temperature, wherein the sintering process comprises the following steps: heating at a heating rate of 10 ℃/min, wherein the sintering temperature is 1700 ℃, the sintering time is 2 hours, and then cooling to room temperature along with the furnace, and the sintering atmosphere is hydrogen, so as to obtain a sintered bar.
As shown in FIG. 1, the metallographic structure of the high temperature resistant Mo-Si-B alloy prepared in this example shows that the alloy has uniform chemical composition, no porosity and full compactness, and the metallographic structure of the Mo-Si-B alloy obtained after casting is α -Mo and Mo3Si and Mo5SiB2。
Claims (4)
1. A preparation method of a high-temperature resistant intermetallic compound alloy comprises the following steps:
(1) preparing raw materials of the Mo-Si-B alloy according to the weight percentage, wherein the weight percentage of Mo: 70-89%, Si: 10-25%, B: 1-5%, adding silicon in the form of molybdenum silicide;
(2) performing low-temperature pre-sintering on the raw materials in the step (1) by adopting a powder metallurgy method to form lump materials, and performing high-temperature synthesis by adopting an electron beam melting method to obtain high-temperature-resistant intermetallic compound alloy lumps; the method comprises the following steps:
(a) the raw material powder is proportioned and mixed according to the component proportion, the uniformly mixed raw material powder is subjected to cold isostatic pressing on a cold isostatic pressing machine, and a blank is obtained; the pressure of the cold isostatic pressing is 150-250 MPa, and the pressure maintaining time is 5-20 minutes;
(b) pre-sintering the obtained blank, wherein the pre-sintering process comprises the following steps: heating at a heating rate of 5-10 ℃/min, wherein the pre-sintering temperature is 1000-1200 ℃, the pre-sintering time is 1-2 hours, then cooling to room temperature along with the furnace, and the pre-sintering atmosphere is hydrogen to obtain a pre-sintered bar;
(c) carrying out high-temperature synthesis on the pre-sintered bar by using electron beam melting to obtain an intermetallic compound, wherein the synthesis temperature is 2500-3000 ℃, the melting time is 1-10 minutes, and the ingot is cooled along with the furnace after the synthesis reaction;
(3) and mechanically crushing the synthesized alloy block to obtain heat-resistant alloy powder with different particle sizes meeting the requirements, adding silicon, boron and/or compounds thereof into the heat-resistant alloy powder obtained by mechanical crushing, then performing compression molding and high-temperature sintering on the powder, and finally obtaining an alloy part blank with uniform components and low impurity content.
2. The method for producing a high-temperature-resistant intermetallic compound alloy according to claim 1, characterized in that: the weight of the added silicon is 5-20% of the weight of the added silicon, and the weight of the added boron is 5-20% of the weight of the added boron.
3. The method for producing a high-temperature-resistant intermetallic compound alloy according to claim 1 or 2, characterized in that: the method comprises the following steps of mechanically crushing the synthesized alloy block to obtain heat-resistant alloy powder with different particle sizes meeting requirements, and then performing compression molding and high-temperature sintering on the powder, wherein the method comprises the following specific steps:
(i) ball-milling an intermetallic compound alloy block synthesized by electron beam melting by using a ball mill to obtain alloy powder with different particle sizes, wherein the rotating speed of the ball mill is 100-;
(ii) uniformly stirring the ball-milled powder or the mixed powder of the ball-milled powder and silicon, boron and/or compounds thereof, and then performing compression molding to obtain a blank; the pressing pressure is 150-250 MPa, and the pressure maintaining time is 5-20 minutes;
(iii) and sintering the obtained blank at a high temperature, wherein the pre-sintering process comprises the following steps: heating at a heating rate of 5-10 ℃/min, wherein the pre-sintering temperature is 1500-1800 ℃, the pre-sintering time is 1-2 hours, and then cooling to room temperature along with the furnace, wherein the pre-sintering atmosphere is hydrogen, so as to obtain a sintered bar.
4. The method for producing a high-temperature-resistant intermetallic compound alloy according to claim 3, characterized in that: the grain size of the alloy powder is 1-15 microns.
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| CN114182150B (en) * | 2021-11-01 | 2022-11-01 | 台州学院 | Novel nonequilibrium Mo + Mo5SiB2+Mo5Si3Base alloy and method for producing same |
| CN114672712B (en) * | 2022-04-13 | 2022-12-06 | 西安理工大学 | Lamellar Mo2TiAlC2 toughened molybdenum-silicon-boron alloy and preparation method thereof |
| CN114799616B (en) * | 2022-04-28 | 2023-10-20 | 桂林电子科技大学 | High-entropy intermetallic compound material, preparation method thereof and electronic solder |
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