CN101397613A - Method for preparing molybdenum-silicium-boron alloy - Google Patents

Method for preparing molybdenum-silicium-boron alloy Download PDF

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CN101397613A
CN101397613A CNA200810231975XA CN200810231975A CN101397613A CN 101397613 A CN101397613 A CN 101397613A CN A200810231975X A CNA200810231975X A CN A200810231975XA CN 200810231975 A CN200810231975 A CN 200810231975A CN 101397613 A CN101397613 A CN 101397613A
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sintering
powder
molybdenum
alloy
melting
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CN101397613B (en
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孙军
张国君
杨双平
孙院军
江峰
刘刚
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Shandong Ming metal Mstar Technology Ltd
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Xian Jiaotong University
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Abstract

The invention discloses a method for preparing molybdenum-silicon-boron alloy, which comprises the steps that: molybdenum powder, silicon powder and boron powder are taken as raw materials; after even mixed treatment, the alloy powder is subjected to smelting in an arc-melting furnace, a smelting operating current is 700A to 800A; a lump after smelting is subjected to crushing and annealing treatment, the annealing temperature is 1200 DEG C to 1300 DEG C, the time is 0.5 hour to 1.5 hours; and then the alloy powder after the annealing treatment is put in an electricity-discharging plasma sintering furnace for sintering, the sintering temperature is 1400 DEG C to 1600 DEG C, the sintering time is 2min to 5min and the sintering pressure is 10MPa to 30MPa. The molybdenum-silicon-boron alloy prepared by the method has the advantages of simple method and fast speed, and has high organization compaction, strength and extensibility.

Description

The preparation method of a kind of molybdenum-silicon-boron alloy
Technical field
The invention belongs to powder metallurgical technology, the preparation method of particularly a kind of molybdenum-silicon-boron alloy.
Background technology
In recent years, fast development along with space flight and aviation and national defense industry, high-temperature mechanics and antioxidant property to high-temperature structural material have proposed higher, harsher requirement, and superalloys such as present widely used nickel based super alloy have become the bottleneck of restriction related industries field development because of himself limitation (the highest service temperature can not above 1100 ℃).Therefore the various countries scientist has accelerated the research progress to high-temperature structural material of future generation, and present result of study shows, molybdenum-silicon-boron alloy is the most potentially can replace nickel based super alloy, becomes the optimal candidate material of high-temperature structural material of future generation.
Molybdenum-silicon-boron alloy is meant by Mo 5Si 3, Mo 5SiB 2(T2 phase) and Mo3Si three-phase, α-Mo and Mo 5SiB 2Two-phase or α-Mo, Mo 3Si and Mo 5The alloy of SiB2 three phase composites.Wherein the former has extremely excellent resistance of oxidation, but its room temperature fracture toughness property is lower; And all contain α-Mo phase among the latter, cause its oxidation-resistance not by Mo 5Si 3, Mo 5SiB 2And Mo 3The oxidation-resistance of the alloy of Si three phase composites is strong, but because α-Mo is that the ductility phase is (with respect to Mo 3Si and Mo 5SiB 2), this alloy at room temperature and high temperature fracture toughness are improved significantly.
The main method of preparation molybdenum-silicon-boron alloy material is arc melting+hot pressing sintering method at present.Although this method has process stabilizing, composition advantage of uniform, but this method lifetime is long, complicated operation, shortcomings such as cost height, this preparation method generally needs long time homogenizing to obtain required molybdenum-silicon-boron alloy material product, and in addition, the silicon series intermetallic compound powder that this method obtains often has higher oxygen level and other impurity, the engineering that has influenced material is used, and these problems have all become one of restriction molybdenum-silicon-boron alloy development and key in application problem.
Discharge plasma sintering technique is the new technology of material preparation.It is to utilize pulse high current directly to put on conductive die and the sample, produces the body heating, makes to be sintered sample and to be rapidly heated; Simultaneously, pulsed current causes intergranular discharge effect, can purify particle surface, realizes Fast Sintering, suppresses particle effectively and grows up.Traditional hot pressed sintering mainly is by the energising joule heating that produces and these two carrying out that factor is impelled sintering process of viscous deformation of pressurizeing and causing.And the discharge plasma sintering process is except above-mentioned effect, on the compacted granules sample, applied the dc pulse current that produces by particular power source, and effectively utilize the self-heating effect of between powder granule, discharging and being produced, have the advantages that to be different from the conventional sintering method: sintering temperature is low, sintering time is short, tiny, the uniform tissue of crystal grain can be obtained, and the state of nature of starting materials can be kept; Can obtain high compactedness material.
Therefore, the sintering time that utilizes discharge plasma sintering technique to have is short, can obtain tiny, the clean particle surface of crystal grain, uniform tissue, and can obtain characteristics such as high compactedness material and prepare molybdenum-silicon-boron alloy material, and be applied in the actual production, be expected to solve the preparation difficulty that present high-quality molybdenum-silicon-boron alloy material faces.
Summary of the invention
The object of the present invention is to provide a kind of simply, high-quality molybdenum-silicon-boron alloy preparation method fast, and prepare the microtexture even compact of molybdenum-silicon-boron alloy with method of the present invention, have high-density and intensity.
Molybdenum-silicon provided by the present invention-boron alloy preparation method, preparation process is as follows:
With molybdenum powder, silica flour, boron powder is raw material, and wherein the mass percent of silica flour and boron powder is respectively 10.0-14.5% and 1.0-4.5%, and all the other are molybdenum powder.Powdered alloy carries out melting after handling through uniform mixing in arc-melting furnace, the melting working current is 700-800A, the block after the melting is pulverized and anneal again, and annealing temperature is: 1200-1300 ℃, the time is: 0.5-1.5 hour;
Alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering, heat-up rate is 50-500 ℃/min, sintering temperature is: 1400-1600 ℃, the axial pressure of sintering is: 10-30MPa, sintered heat insulating time: 2-5min;
Furnace cooling takes out mould behind the sintering after 400-500 ℃, is cooled to room temperature in air, after the demoulding top layer 0.3-0.5mm is removed in the sintered compact processing that obtains, and promptly obtains molybdenum-silicon-boron alloy material.
The key problem in technology that the present invention solves is to select suitable sintering method and technology, makes the weave construction densification of prepared molybdenum-silicon-boron alloy, and grain-size is tiny evenly, thereby has guaranteed that resulting material has high-density and high strength.
Embodiment
Embodiment one: take by weighing the 85.2g molybdenum powder respectively; 12.6g silica flour and 2.2g boron powder; adopting mixer to carry out uniform mixing handles; in arc-melting furnace, carry out melting; the melting working current is 700A; block after the melting is pulverized and anneal; annealing temperature is: 1200 ℃; time is: 1.0 hours; subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering; heat-up rate is 300 ℃/min; sintering temperature is: 1450 ℃, the axial pressure of sintering is: 25MPa, sintered heat insulating time: 3min; take out mould behind the furnace cooling to 450 ℃ behind the sintering; in air, be cooled to room temperature, after the demoulding top layer 0.3mm removed in the sintered compact processing that obtains, promptly obtain molybdenum-silicon-boron alloy material.
Embodiment two: take by weighing the 86.1g molybdenum powder respectively; 11.5g silica flour and 2.4g boron powder; adopting mixer to carry out uniform mixing handles; in arc-melting furnace, carry out melting; the melting working current is 750A; block after the melting is pulverized and anneal; annealing temperature is: 1250 ℃; time is: 1.0 hours; subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering; heat-up rate is 400 ℃/min; sintering temperature is: 1400 ℃, the axial pressure of sintering is: 28MPa, sintered heat insulating time: 5min; take out mould behind the furnace cooling to 400 ℃ behind the sintering; in air, be cooled to room temperature, after the demoulding top layer 0.3mm removed in the sintered compact processing that obtains, promptly obtain molybdenum-silicon-boron alloy material.
Embodiment three: take by weighing the 87.5g molybdenum powder respectively; 11.2g silica flour and 1.3g boron powder; adopting mixer to carry out uniform mixing handles; in arc-melting furnace, carry out melting; the melting working current is 800A; block after the melting is pulverized and anneal; annealing temperature is: 1300 ℃; time is: 1.0 hours; subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering; heat-up rate is 350 ℃/min; sintering temperature is: 1550 ℃, the axial pressure of sintering is: 28MPa, sintered heat insulating time: 3min; take out mould behind the furnace cooling to 400 ℃ behind the sintering; in air, be cooled to room temperature, after the demoulding top layer 0.4mm removed in the sintered compact processing that obtains, promptly obtain molybdenum-silicon-boron alloy material.
Embodiment four: take by weighing the 83.7g molybdenum powder respectively; 13.1g silica flour and 3.2g boron powder; adopting mixer to carry out uniform mixing handles; in arc-melting furnace, carry out melting; the melting working current is 750A; block after the melting is pulverized and anneal; annealing temperature is: 1200 ℃; time is: 1.5 hours; subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering; heat-up rate is 200 ℃/min; sintering temperature is: 1600 ℃, the axial pressure of sintering is: 23MPa, sintered heat insulating time: 2min; take out mould behind the furnace cooling to 500 ℃ behind the sintering; in air, be cooled to room temperature, after the demoulding top layer 0.5 mm removed in the sintered compact processing that obtains, promptly obtain molybdenum-silicon-boron alloy material.
Embodiment five: take by weighing the 87.4g molybdenum powder respectively; 10.7g silica flour and 1.9g boron powder; adopting mixer to carry out uniform mixing handles; in arc-melting furnace, carry out melting; the melting working current is 700A; block after the melting is pulverized and anneal; annealing temperature is: 1300 ℃; time is: 0.5 hour; subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering; heat-up rate is 500 ℃/min; sintering temperature is: 1500 ℃, the axial pressure of sintering is: 26MPa, sintered heat insulating time: 4min; take out mould behind the furnace cooling to 450 ℃ behind the sintering; in air, be cooled to room temperature, after the demoulding top layer 0.4 mm removed in the sintered compact processing that obtains, promptly obtain molybdenum-silicon-boron alloy material.
Embodiment six: take by weighing the 81.7g molybdenum powder respectively; 14.2g silica flour and 4.1g boron powder; adopting mixer to carry out uniform mixing handles; in arc-melting furnace, carry out melting; the melting working current is 800A; block after the melting is pulverized and anneal; annealing temperature is: 1300 ℃; time is: 1.0 hours; subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering; heat-up rate is 150 ℃/min; sintering temperature is: 1600 ℃, the axial pressure of sintering is: 24MPa, sintered heat insulating time: 3min; take out mould behind the furnace cooling to 400 ℃ behind the sintering; in air, be cooled to room temperature, after the demoulding top layer 0.5mm removed in the sintered compact processing that obtains, promptly obtain molybdenum-silicon-boron alloy material.

Claims (1)

1, the preparation method of a kind of molybdenum-silicon-boron alloy is characterized in that, step is as follows:
With molybdenum powder, silica flour, boron powder is raw material, and wherein the mass percent of silica flour and boron powder is respectively 10.0-14.5% and 1.0-4.5%, and all the other are molybdenum powder;
Powdered alloy carries out melting after handling through uniform mixing in arc-melting furnace, the melting working current is 700-800A, the block after the melting is pulverized and anneal again, and annealing temperature is: 1200-1300 ℃, the time is: 0.5-1.5 hour;
Subsequently the alloy powder after the anneal is packed in the graphite jig, mould is carried out sintering in the discharge plasma sintering stove, adopt the argon gas atmosphere protection during sintering, heat-up rate is 50-500 ℃/min, sintering temperature is: 1400-1600 ℃, the axial pressure of sintering is: 10-30MPa, sintered heat insulating time: 2-5min;
Furnace cooling takes out mould behind the sintering after 400-500 ℃, is cooled to room temperature in air, after the demoulding top layer 0.3-0.5mm is removed in the sintered compact processing that obtains, and promptly obtains molybdenum-silicon-boron alloy material.
CN200810231975XA 2008-10-28 2008-10-28 Method for preparing molybdenum-silicium-boron alloy Expired - Fee Related CN101397613B (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103160701A (en) * 2011-12-09 2013-06-19 北京有色金属研究总院 Preparation method for high-temperature-resistant Mo-Si-B alloy
CN103952581A (en) * 2014-04-23 2014-07-30 北京科技大学 Method for preparing high-porosity molybdenum-silicon-boron porous material by adding pore-forming agent
CN104451259A (en) * 2014-11-13 2015-03-25 内蒙古工业大学 Method for preparing zirconium alloy by sintering discharge plasma
CN105506331A (en) * 2016-01-19 2016-04-20 西安航天新宇机电设备厂 Mo-Si-B-Ti-Zr-Al-Nb composite material and preparation method thereof
CN108251670A (en) * 2016-12-28 2018-07-06 北京有色金属研究总院 The preparation method of compound alloy between refractory metal
CN109306421A (en) * 2018-09-18 2019-02-05 厦门虹鹭钨钼工业有限公司 A kind of anti-erosion molybdenum alloy electrode and its manufacturing method
CN112779448A (en) * 2020-12-27 2021-05-11 西北工业大学 High-temperature-resistant molybdenum oxide alloy and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103160701A (en) * 2011-12-09 2013-06-19 北京有色金属研究总院 Preparation method for high-temperature-resistant Mo-Si-B alloy
CN103952581A (en) * 2014-04-23 2014-07-30 北京科技大学 Method for preparing high-porosity molybdenum-silicon-boron porous material by adding pore-forming agent
CN104451259A (en) * 2014-11-13 2015-03-25 内蒙古工业大学 Method for preparing zirconium alloy by sintering discharge plasma
CN105506331A (en) * 2016-01-19 2016-04-20 西安航天新宇机电设备厂 Mo-Si-B-Ti-Zr-Al-Nb composite material and preparation method thereof
CN108251670A (en) * 2016-12-28 2018-07-06 北京有色金属研究总院 The preparation method of compound alloy between refractory metal
CN108251670B (en) * 2016-12-28 2020-01-10 有研工程技术研究院有限公司 Preparation method of high-temperature-resistant intermetallic compound alloy
CN109306421A (en) * 2018-09-18 2019-02-05 厦门虹鹭钨钼工业有限公司 A kind of anti-erosion molybdenum alloy electrode and its manufacturing method
CN112779448A (en) * 2020-12-27 2021-05-11 西北工业大学 High-temperature-resistant molybdenum oxide alloy and preparation method thereof

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