CN100465309C - Method for preparing alloy material of high niobium-titanium-aluminum by discharging plasma agglomeration - Google Patents
Method for preparing alloy material of high niobium-titanium-aluminum by discharging plasma agglomeration Download PDFInfo
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- CN100465309C CN100465309C CNB2006101133256A CN200610113325A CN100465309C CN 100465309 C CN100465309 C CN 100465309C CN B2006101133256 A CNB2006101133256 A CN B2006101133256A CN 200610113325 A CN200610113325 A CN 200610113325A CN 100465309 C CN100465309 C CN 100465309C
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Abstract
This invention discloses a method for preparing high-Nb Ti-Al alloy by discharge plasma sintering. The method comprises: loading element mixed powder alloy powder into a graphite mold, placing in a discharge plasma-sintering furnace, applying an axial pressure of 10-80 MPa, heating at a rate of 50-800 deg.C/min in 10-2-6 Pa vacuum or inert atmosphere, sintering at 900-1400 deg.C, keeping the temperature, and cooling to room temperature to obtain high-Nb Ti-Al alloy blocks. The method can prepare highly compact high-Nb Ti-Al alloy blocks with uniform composition and high performance in a short time and at a low sintering temperature. Besides, the method also has such advantages as low energy consumption, little pollution, easy operation and good repeatability.
Description
Technical field
The invention belongs to high-Nb Ti-Al inter-metallic compound material technical field, a kind of method of utilizing discharge plasma sintering to prepare alloy material of high niobium-titanium-aluminum particularly is provided.
Background technology
TiAl base alloy is because of it has that proportion is low, hot strength good, rigidity and Young's modulus is big and advantages such as good oxidization resistance energy, creep-resistant property and anti-fatigue performance, in fields such as Aeronautics and Astronautics and automobiles, be a kind of high-temperature structural material that has competitive power.But the biggest obstacle of TiAl base alloy practical application at present is that this alloy temperature-room type plasticity is low, formability difference and in the oxidisability deficiency more than 850 ℃.At above problem, research and development use temperature higher high temperature TiAl alloy, and to update and develop its effective technology of shaping be an important content of following work.
Experimental results show that the Nb element is one of the most effective alloying element that improves the alloy high-temp performance, the adding of high-melting-point constituent element Nb can improve the fusing point and the ordering temperature of TiAl alloy, thereby can improve the use temperature of alloy, meanwhile also can improve the hot strength and the antioxidant property of alloy greatly.Thereby in TiAl metallic compound research field, high Nb-TiAl alloy has caused increasing concern, China's research has in this regard also obtained remarkable progress, wherein two national patent CN1069775, CN1352318 have successfully been applied for by the high Nb-TiAl base alloy of Chen Guoliang academician independent development, alloy has excellent hot strength and high-temperature oxidation resistance, ultimate-use temperature can be improved 60～100 ℃.
But the adding of high Nb brings superior high-temperature behavior simultaneously, also increases substantially because of alloy melting point, hot strength, causes the smelting temperature of alloy and hot processing temperature to improve, thereby has increased the preparation difficulty of alloy.As everyone knows, prepare high-quality high Nb-TiAl alloy, it is the guarantee of accurately carrying out smoothly of other research work, also be alloy moves towards the practical stage from conceptual phase prerequisite simultaneously, and good preparation technology is the prerequisite that obtains the high quality alloy, therefore the preparation technology of high Nb-TiAl alloy is carried out exploratory development and has realistic meanings.
At present, focus mostly in the content of the aspects such as strengthening mechanism, thermal treatment process, alloy structure and property relationship of antioxidant property, Nb for the research of high Nb-TiAl alloy, and rare at the preparation technology's of high Nb-TiAl alloy research specially.(aeronautical material journal, 2004,24 (1): 12-16) prepared the alloy of Ti-45Al-8.5Nb, Ti-45Al-8.5Nb-0.1C, Ti-45Al-8.5Nb-0.1C-0.2W three kinds of compositions with the ingot metallurgy method such as Li Shujiang.But the alloy preparation process is comparatively complicated, and occurs casting flaw, component segregation and grain size non-uniform phenomenon easily, also is difficult to the small-sized component preparation that realizes that shape is comparatively complicated simultaneously.
Based on above deficiency, we have adopted the discharge plasma sintering legal system to be equipped with high Nb-TiAl alloy.
Discharge plasma sintering (Spark Plasma Sintering is called for short SPS) is that the nineties is from the full-fledged a kind of sintering technology of Japan.Advantages such as the SPS technology is fast because of its heat-up rate, sintering time is short, weave construction is controlled show wide application prospect in field of material preparation.This technology has been successfully applied to the preparation of multiple novel materials such as function-graded material, nano material, porous material, metal-base composites, fibre reinforced composites at present.Wherein, aspect the preparation intermetallic compound, because intermetallic compound room temperature fragility and dystectic feature, in preparation process, often need high-energy and high vacuum system, and utilize the SPS technology to prepare intermetallic compound, because effectively utilized intergranular spontaneous heating effect and surface activation, can realize low temperature, Fast Sintering, so the SPS technology is a kind of effective ways of preparation inter-metallic compound material.Up to the present, have only several investigators of minority to carry out the research (B.C.Mei that the SPS technology prepares general T iAl base alloy both at home and abroad, Y.Miyamoto.Preparation of Ti-Al intermetallic compounds by spark plasmasintering.Metallurgical and Materials Transactions, 2001,32A (3A): 843-847; K.Matsugi, N.Ishibashi, T.Hatayama et al.Microstructure of spark sinteredtitanium-aluminide compacts.Intermetallics, 1996,4:457-467; H.A.Calderon, V.Garibay-Febles, M.Umemoto et al.Mechanical propertics of nanocrystallineTi-Al-Xalloys.Materials Science And Engineering, 2002, A329-33; 96-205; S.J.Hwang, M.S.Kim, S.Y.Jung et al.Consolidation of mechanically milled TiAlalloys by spark plasma sintering.Journal of Metastable and NanocrystallineMaterials, 2003,15-16:361-366), but the research for the SPS technology prepares high Nb-TiAl base alloy material does not also have relevant report.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing discharge plasma sintering to prepare alloy material of high niobium-titanium-aluminum, realize that low temperature, Fast Sintering prepare the high-performance alloy material of high niobium-titanium-aluminum.
The present invention realizes by following manner:
The raw material powder that employing is made up of element mixed powder and powdered alloy, wherein, the shared weight percent of powdered alloy is 50～100%, all the other are the element mixed powder; Behind the raw material powder mixing, in the graphite jig of packing into, insert again in the discharge plasma sintering stove, apply the axle pressure of 10～80MPa, adopt vacuum tightness 10
-2Carry out sintering under the vacuum condition of～6Pa or the protection of inert gas, heat-up rate is 50～800 ℃/min, and sintering temperature is 900～1400 ℃, cools to room temperature after the insulation with the furnace, can obtain high Nb-TiAl base alloy block material.
The composition of powdered alloy of the present invention is: Al content is 45～46%, and Nb content is 8～10%, and C content is 0～0.2%, and W content is 0～0.2%, Y content is 0～0.1%, more than is atomic percent, and surplus is Ti; The formulated component of element mixed powder is: Al content is 45～46%, and Nb content is 8～10%, and C content is 0～0.2%, and W content is 0～0.2%, Y content is 0～0.1%, more than is atomic percent, and surplus is Ti.
Advantage of the present invention is:
1) can reduce the sintering temperature of material, generally than low 100-200 ℃ of ordinary sinter temperature;
2) warming and cooling rate is fast, shortens generated time greatly;
3) prepared high Nb-TiAl base alloy material density height, composition homogeneous microstructure, the excellent performance that goes out, its mechanical property can surpass the cast alloy materials of identical component proportioning;
4) by changing sintering process, can realize control to alloy microscopic structure;
5) can realize the comparatively preparation of complex part of partial shape, especially on the preparation miniature workpiece, have more advantage;
6) these method energy-conserving and environment-protective are simple to operate, can realize numerical control operating, and experiment is repeatable strong.
Embodiment
Embodiment 1
To synthetic Ti-45Al-8.5 in advance
Nb-0.2B-0.2W-0.1Y powdered alloy (spherical powder, mean particle size is 30 μ m, oxygen level is 0.12w.%, carbon content is 0.03w.%) put into the stone mill mould of Φ 20, then the stone mill mould is put into the discharge plasma sintering stove, system is evacuated to 2Pa, adds axle pressure and is 40MPa, speed with 100 ℃/min is warming up to required sintering temperature (1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃), then furnace cooling behind insulation 5min under this temperature.After testing, more than the density of preparation sample is 4.29g/m
3, near the theoretical density of material; Under different sintering temperatures, can obtain dissimilar microstructures.
Concrete experimental result is as follows:
Table 1
*DP: bifurcation tissue; NL: nearly holostrome sheet tissue; FL: holostrome sheet tissue; σ
Bc: ultimate compression strength; σ
0.2c: compression yield strength; ε
c: rate of compression;
Embodiment 2
With the element mixed powder of synthetic 70w.%Ti-45Al-8.5Nb-0.2B-0.2W-0.1Y powdered alloy and 30w.% and powdered alloy identical component proportioning in advance, put into the stone mill mould of Φ 20 after mixing, then the stone mill mould is put into the discharge plasma sintering stove, system is evacuated to 2Pa, add axle pressure and be 40MPa, speed with 100 ℃/min is warming up to 1050 ℃, then furnace cooling behind insulation 5min under this temperature.After testing, the density of sample is 4.29g/m
3, near the theoretical density of material.The mechanical property of sample is: ultimate compression strength is 3010MPa, and compression yield strength is 1006MPa, and the compression fracture strain is 42.0%.
Claims (1)
1. method of utilizing discharge plasma sintering to prepare alloy material of high niobium-titanium-aluminum, it is characterized in that: adopt with powdered alloy or element mixed powder and mix the raw material powder of forming with powdered alloy, wherein, the shared weight percent of powdered alloy is 50～100%, and all the other are the element mixed powder; Behind the raw material powder mixing, in the graphite jig of packing into, insert again in the discharge plasma sintering stove, apply the axle pressure of 10～80MPa, adopt vacuum tightness 10
-2Carry out sintering under the vacuum condition of～6Pa or the protection of inert gas, heat-up rate is 50～800 ℃/min, and sintering temperature is 900～1400 ℃, cools to room temperature after the insulation with the furnace, can obtain high Nb-TiAl base alloy block material; The composition of described powdered alloy is: Al content is 45～46%, and Nb content is 8～10%, and C content is 0～0.2%, and W content is 0～0.2%, Y content is 0～0.1%, more than is atomic percent, and surplus is Ti; The formulated component of element mixed powder is: Al content is 45～46%, and Nb content is 8～10%, and C content is 0～0.2%, and W content is 0～0.2%, Y content is 0～0.1%, more than is atomic percent, and surplus is Ti.
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| WO2016055013A1 (en) * | 2014-10-09 | 2016-04-14 | 南京理工大学 | Tial intermetallic compound single crystal material and preparation method therefor |
| CN104625066B (en) * | 2015-01-30 | 2017-09-29 | 北京科技大学 | A kind of method for preparing alloy material of high niobium-titanium-aluminum using two step pressure infiltrations |
| CN104942282A (en) * | 2015-07-14 | 2015-09-30 | 长春工业大学 | Pre-processing method for spark plasma sintering interface of amorphous alloy powder |
| CN107130139B (en) * | 2017-06-15 | 2018-09-18 | 北京科技大学 | A method of the addition intensified-sintered Powder Metallurgy TiAl based Alloys of Sn |
| CN107699738A (en) * | 2017-09-29 | 2018-02-16 | 成都露思特新材料科技有限公司 | A kind of fine-grained TiAl alloy and preparation method thereof, aero-engine, automobile |
| CN107952966A (en) * | 2017-11-24 | 2018-04-24 | 攀钢集团攀枝花钢铁研究院有限公司 | The preparation method at spherical titanium aluminium-based alloyed powder end |
| CN108034866B (en) * | 2018-01-22 | 2019-08-23 | 哈尔滨工业大学 | A kind of high-performance aluminium silicon nitride based composites and preparation method thereof |
| CN111961900A (en) * | 2020-09-07 | 2020-11-20 | 济南大学 | Novel titanium-aluminum-based composite material and preparation method thereof |
| CN113927031B (en) * | 2021-10-18 | 2023-04-21 | 四川大学 | Method for improving performance of titanium alloy by doping Y with Ti-5Al-5Mo-5V-3Cr-Zr alloy |
| CN115976367A (en) * | 2023-02-17 | 2023-04-18 | 浙江工业大学 | Rhenium alloying titanium-aluminum alloy and preparation method thereof |
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