CN102534279B - In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys - Google Patents
In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys Download PDFInfo
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- CN102534279B CN102534279B CN201210019532.0A CN201210019532A CN102534279B CN 102534279 B CN102534279 B CN 102534279B CN 201210019532 A CN201210019532 A CN 201210019532A CN 102534279 B CN102534279 B CN 102534279B
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Abstract
An in situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys belongs to technical field of ally material manufacturing. The in situ reaction hot-pressing method is characterized by adopting a spark plasma sintering (SPS) furnace to eliminate low temperature solid-solid reaction among three elements of Mo, Si and B mainly through control of technological parameters, utilizing solid-liquid reaction among the three elements to in situ synthesize a T2 phase, fully using heat released by in-situ reaction, simultaneously hot-pressing compactly by one step, reducing hot-pressing temperature, improving material density, refining tissues, simplifying processes, and utilizing advantages that an in situ synthesis interface is clean, free of Mo3Si, Mo5Si3, Mo2B, MoB and other leading phases and high in purity to manufacture the T2 phase alloys with small crystal particle and high compactness and purity. Therefore good high temperature oxidation resistance, excellent mechanical properties and particularly high temperature mechanical properties of the T2 phase are exerted to the maximum limit, properties of the T2 phase alloys are improved to the maximum limit, and the in situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys is simple and convenient in process, easy to control and simplified in working procedure.
Description
Technical field
The invention belongs to alloy material preparing technical field, particularly the preparation of the intermetallic compound silicon molybdenum compound of high-melting-point, infusibility.
Background technology
T2 has high fusing point (~ 2200 ℃), relatively low density (8.864g/cm mutually
3), excellent hot strength, good high temperature creep drag and oxidation drag, good thermal conductivity and electroconductibility, be considered to have in aerospace and gas turbine engine field ultrahigh-temperature of new generation (1200-1600 ℃) structured material of broad prospect of application.But, due to its cubic D8
1(tI32, I4/mcm) crystalline structure, less between Composition Region, the little atom of solid solution limited in one's ability, therefore, has proposed very high requirement to preparing high-purity and fine and close T2 phase alloy technique.
At present, the preparation method of T2 phase alloy mainly contains arc melting+annealing process, mechanical alloying etc.Wherein, adopt arc melting+annealing process (Nunes C A, et al. Intermetallics, 2000,8:327-337; Rawn C J, et al. Intermetallics, 2001,9:209-216) the T2 phase alloy prepared organize thick, the uneven segregation of composition is serious, inevitably occurs Mo
3si, Mo
5si
3, Mo
2the leading phase such as B, MoB, and contain tiny crack in tissue; Mechanical alloying (Yamauchi A, et al. J. Alloy. Compd., 2007,434-435:420-423; Abbasi A R, et al. Mater. Sci. Eng. A, 2011, A528:3295-3301) be that powder is realized viscous deformation, cold welding, fragmentation under high energy ball mill, thereby reach the physical and chemical process of atomic level alloying between element, be therefore difficult to accurately control reaction process, react incomplete and lack moulding process, in order to obtain fine and close T2 phase alloy, need to add follow-up densification operation.Mo in T2 phase alloy prepared by above-mentioned these techniques
3si, Mo
5si
3, Mo
2the appearance of the leading phase such as B, MoB can reduce high temperature oxidation resistance and the especially mechanical behavior under high temperature of mechanical property of material; And organize thick, inhomogeneous and tiny crack to be also unfavorable for the improvement of T2 phase alloy mechanical property; Mechanical alloy metallization processes also needs the follow-up fine and close operations such as hot pressing, and preparation section is many, controls complicated.
Summary of the invention
The object of the invention is to utilize reaction in－situ heat pressing process, by controlling its processing parameter, prepare tiny, the high densification of crystal grain, high-purity T2 phase alloy, thereby bring into play to greatest extent good high temperature oxidation resistance and the especially mechanical behavior under high temperature of excellent mechanical property of T2 phase, improve to greatest extent T2 phase alloy performance, and simple process, be easy to control, operation simplify.
The present invention adopts SPS sintering oven, main by controlling processing parameter, eliminate the low temperature solid-solid reaction between Mo, Si and B element, and utilize the synthetic T2 phase of solid-liquid reaction original position between them, and make full use of the step hot pressing densification simultaneously of reaction in－situ liberated heat, reduce hot pressing temperature, improve material density, thinning microstructure, simplifies working process, and brings into play the synthetic interface cleaning of original position simultaneously, does not contain Mo
3si, Mo
5si
3, Mo
2the leading phase such as B, MoB, the advantage that purity is high, prepare tiny, the high densification of crystal grain, high-purity T2 phase alloy.Raw material involved in the present invention is from Mo powder (5.96 μ m, 99.99 wt%), Si powder (6.23 μ m, 99.999wt%) and B powder (3.63 μ m, 99.99wt%) mixture, and its one-tenth is grouped into by Mo
5siB
2the interval preparation of stoichiometric composition, by comprehensive ball mill ball milling 15-30h (take dehydrated alcohol as medium), afterwards at 50 ℃ of vacuum-drying 8-12h.
The concrete preparation process of T2 phase alloy is as follows:
(1) with Mo powder (5.96 μ m, 99.99 wt%), Si powder (6.23 μ m, 99.999wt%) and B powder (3.63 μ m, 99.99wt%), be raw material, by Mo
5siB
2stoichiometric composition interval make required mixed powder, its atomic percent is: 61.5-63.0%Mo, 12.0-14.0%Si and 23.5-25.5%B, by comprehensive ball mill with 300 revs/min of ball milling 15-30h (take dehydrated alcohol as medium), then at 50 ℃ of vacuum-drying 8-12h.
(2) on SPS sintering oven, carry out reaction in－situ hot pressing, temperature rise rate is 100-300 ℃/min, sintering temperature is 1450-1600 ℃, soaking time is 5-30min, exert pressure as 40-60MPa, after sintering completes, with the speed of 10-20 ℃/min, be cooled to 400-500 ℃, last stove is chilled to room temperature.Release gradually after pressurize is arrived 1100-1200 ℃ in process of cooling.Whole sintering process is carried out under vacuum condition.
The invention has the advantages that and utilize reaction in－situ heat pressing process, on SPS sintering oven, main by controlling processing parameter, the low temperature solid-solid reaction between elimination Mo, Si and B element, and utilize the synthetic T2 phase of solid-liquid reaction original position between them, and make full use of the simultaneously step hot pressing densification of reaction in－situ liberated heat, reduce hot pressing temperature, improve material density, thinning microstructure, simplify working process, bring into play the synthetic interface cleaning of original position simultaneously, do not contain Mo
3si, Mo
5si
3, Mo
2the leading phase such as B, MoB, the advantage that purity is high, prepare tiny, the high densification of crystal grain, high-purity T2 phase alloy, therefore, this T2 phase alloy can be brought into play good high temperature oxidation resistance and the especially mechanical behavior under high temperature of excellent mechanical property of T2 phase to greatest extent, improves to greatest extent its performance.Because the present invention only need control reaction in－situ hot pressing parameters, reaction in－situ synthetic with hot-pressing densification simultaneously a step completes, without follow-up secondary densification technique, therefore simple process, be easy to control, operation simplifies.
Accompanying drawing explanation
Fig. 1 is Mo-13Si-25B, 200 ℃/min temperature rise rate, 1500 ℃ of sintering temperature T2 phase alloy XRD spectral lines;
Fig. 2 is Mo-13Si-25B, 200 ℃/min temperature rise rate, 1500 ℃ of sintering temperature T2 phase alloy crystal grain distribution plans;
Fig. 3 is Mo-13Si-25B, 200 ℃/min temperature rise rate, 1500 ℃ of sintering temperature T2 phase alloy differing temps three-point bending fracture toughness;
Fig. 4 is Mo-13Si-25B, 200 ℃/min temperature rise rate, 1500 ℃ of sintering temperature T2 phase alloy differing temps compression true stress-true strain curves;
Fig. 5 is Mo-14Si-23.5B, 100 ℃/min temperature rise rate, 1500 ℃ of sintering temperature T2 phase alloy XRD spectral lines;
Fig. 6 is Mo-12Si-25.5B, 200 ℃/min temperature rise rate, 1450 ℃ of sintering temperature T2 phase alloy XRD spectral lines.
Embodiment
embodiment 1:the nominal composition of mixed powder is Mo-13Si-25B (atomic percent, %), and through comprehensive ball mill, with 300 revs/min of ball milling 24h (take dehydrated alcohol as medium), 50 ℃ of vacuum-drying 9h, weigh 62.66g.Adopt SPS-1500 agglomerating plant, load weighted powder is inserted in the graphite jig that internal diameter is 30mm, temperature rise rate is 200 ℃/min, and sintering temperature is 1500 ℃, and soaking time is 7min, exerts pressure as 60MPa.After sintering completes, with the speed of 20 ℃/min, be cooled to 500 ℃, last stove is chilled to room temperature.Release gradually after pressurize to 1200 ℃ in process of cooling.Whole sintering process is carried out under vacuum condition, finally obtains Φ 30mm × 10mm sample blanks.Fig. 1 is the XRD spectral line of T2 phase alloy, does not find Mo
3si, Mo
5si
3, Mo
2b, MoB etc. are leading to be existed mutually, and purity is high, is obviously better than arc melting+annealing process (Nunes C A, et al. Intermetallics, 2000,8:327-337; Rawn C J, et al. Intermetallics, 2001,9:209-216) and mechanical alloying (Yamauchi A, et al. J. Alloy. Compd., 2007,434-435:420-423; Abbasi A R, et al. Mater. Sci. Eng. A, 2011, A528:3295-3301).The relative density of this T2 phase alloy is ~ 99.5%, and average grain size is 1.44 μ m (Fig. 2), is significantly less than arc melting+annealing process (Nunes C A, et al. Intermetallics, 2000,8:327-337; Rawn C J, et al. Intermetallics, 2001,9:209-216).T2 phase alloy has good mechanical property (Fig. 3-4), room temperature, 1200 ℃ of three-point bending fracture toughness
k iCbe respectively 3.41MPam
1/2with 9.66 MPam
1/2(Fig. 3), room temperature, 1200 ℃, 1400 ℃ compressive strengths are respectively 2905MPa, 965MPa and 483MPa (Fig. 4).
embodiment 2:the nominal composition of mixed powder is Mo-14Si-23.5B (atomic percent, %), and through comprehensive ball mill, with 300 revs/min of ball milling 24h (take dehydrated alcohol as medium), 50 ℃ of vacuum-drying 9h, weigh 62.66g.Adopt SPS-1500 agglomerating plant, load weighted powder is inserted in the graphite jig that internal diameter is 30mm, temperature rise rate is 100 ℃/min, and sintering temperature is 1500 ℃, and soaking time is 7min, exerts pressure as 60MPa.After sintering completes, with the speed of 20 ℃/min, be cooled to 500 ℃, last stove is chilled to room temperature.Release gradually after pressurize to 1200 ℃ in process of cooling.Whole sintering process is carried out under vacuum condition, finally obtains Φ 30mm × 10mm sample blanks.Fig. 5 is the XRD spectral line of this technique T2 phase alloy sample, can find out in alloy and only contain T2 phase, does not find Mo
3si, Mo
5si
3, Mo
2b, MoB etc. are leading to be existed mutually, and purity is high, is obviously better than arc melting+annealing process (Nunes C A, et al. Intermetallics, 2000,8:327-337; Rawn C J, et al. Intermetallics, 2001,9:209-216) and mechanical alloying (Yamauchi A, et al. J. Alloy. Compd., 2007,434-435:420-423; Abbasi A R, et al. Mater. Sci. Eng. A, 2011, A528:3295-3301).
embodiment 3:the nominal composition of mixed powder is Mo-12Si-25.5B (atomic percent, %), and through comprehensive ball mill, with 300 revs/min of ball milling 24h (take dehydrated alcohol as medium), 50 ℃ of vacuum-drying 9h, weigh 62.66g.Adopt SPS-1500 agglomerating plant, load weighted powder is inserted in the graphite jig that internal diameter is 30mm, temperature rise rate is 200 ℃/min, and sintering temperature is 1450 ℃, and soaking time is 7min, exerts pressure as 60MPa.After sintering completes, with the speed of 20 ℃/min, be cooled to 500 ℃, last stove is chilled to room temperature.Release gradually after pressurize to 1200 ℃ in process of cooling.Whole sintering process is carried out under vacuum condition, finally obtains Φ 30mm × 10mm sample blanks.Fig. 6 is the XRD spectral line of this technique T2 phase alloy sample, can find out in alloy and only contain T2 phase, does not find Mo
3si, Mo
5si
3, Mo
2b, MoB etc. are leading to be existed mutually, and purity is high, is obviously better than arc melting+annealing process (Nunes C A, et al. Intermetallics, 2000,8:327-337; Rawn C J, et al. Intermetallics, 2001,9:209-216) and mechanical alloying (Yamauchi A, et al. J. Alloy. Compd., 2007,434-435:420-423; Abbasi A R, et al. Mater. Sci. Eng. A, 2011, A528:3295-3301).
Claims (2)
1. prepare a reaction in－situ hot-press method for intermetallic compound T2 phase alloy, it is characterized in that utilizing tiny, the high densification of SPS sintering oven reaction in－situ hot pressing crystal grain, high-purity T2 phase alloy; Press Mo
5siB
2the required mixed powder of the interval preparation of stoichiometric composition, its atomic percent is: 61.5-63.0%Mo, 12.0-14.0%Si and 23.5-25.5%B; The technique of reaction in－situ hot pressing is: temperature rise rate 100-300 ℃/min, and sintering temperature 1450-1600 ℃, soaking time 5-30min, 40-60MPa exerts pressure, after sintering completes, with the speed of 10-20 ℃/min, be cooled to 400-500 ℃, last stove is chilled to room temperature; Release gradually after pressurize is arrived 1100-1200 ℃ in process of cooling.
2. the reaction in－situ hot-press method of preparing intermetallic compound T2 phase alloy as claimed in claim 1, the preparation that it is characterized in that mixed powder is by Mo
5siB
2the interval preparation of stoichiometric composition, and take dehydrated alcohol as medium, by comprehensive ball mill with 300 revs/min of ball milling 15-30h, afterwards at 50 ℃ of vacuum-drying 8-12h.
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| CN103938010B (en) * | 2014-04-23 | 2015-10-28 | 北京科技大学 | A kind of method preparing porous molybdenum silicon boron triple-phase alloys |
| CN103952581B (en) * | 2014-04-23 | 2016-01-20 | 北京科技大学 | A kind of method of adding pore-forming material and preparing high porosity molybdenum silicon boron porous material |
| CN104550904B (en) * | 2014-12-17 | 2016-09-14 | 武汉理工大学 | A kind of with Mo-B-O platelike crystal be the lubrication novel TiAl based self-lubricating material of phase and preparation method |
| CN111020259B (en) * | 2019-11-18 | 2021-11-23 | 海南大学 | Flaky intermetallic compound reinforced fine-grain tungsten alloy and preparation method thereof |
| CN114653950B (en) * | 2022-02-28 | 2024-06-18 | 金堆城钼业光明（山东）股份有限公司 | Molybdenum-silicon-boron solid solution reinforced molybdenum cutting wire and preparation method thereof |
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Non-Patent Citations (2)
| Title |
|---|
| 原位合成Mo5SiB2 的热力学分析;张来启等;《北京科技大学学报》;20080331;第30卷(第3期);281-284 * |
| 张来启等.原位合成Mo5SiB2 的热力学分析.《北京科技大学学报》.2008,第30卷(第3期),281-284. |
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