CN1958817A - 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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- 239000000956 alloy Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 10
- -1 niobium-titanium-aluminum Chemical compound 0.000 title abstract description 6
- 238000005054 agglomeration Methods 0.000 title 1
- 230000002776 aggregation Effects 0.000 title 1
- 238000007599 discharging Methods 0.000 title 1
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 229910010038 TiAl Inorganic materials 0.000 claims abstract description 17
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 3
- 239000010439 graphite Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000013590 bulk material Substances 0.000 claims abstract 2
- 238000004321 preservation Methods 0.000 claims abstract 2
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims 3
- 229910000838 Al alloy Inorganic materials 0.000 claims 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 15
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract 2
- 238000002360 preparation method Methods 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 12
- 238000011160 research Methods 0.000 description 7
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 239000004575 stone Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 229910021362 Ti-Al intermetallic compound Inorganic materials 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- 229910000952 Be alloy Inorganic materials 0.000 description 1
- 206010010214 Compression fracture Diseases 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002707 nanocrystalline material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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Abstract
一种利用放电等离子烧结制备高铌钛铝基合金材料的方法，属于高铌钛铝金属间化合物材料技术领域。采用由元素混合粉末与合金粉末组成的原料粉末，装入石墨模具中，再置入放电等离子烧结炉中，施加10～80MPa的轴向压力，采用真空度10－2～6Pa的真空条件或惰性气体保护下进行烧结，升温速度为50～800℃/min，烧结温度为900～1400℃，保温后随炉冷却至室温，即可得到高Nb－TiAl基合金块体材料。优点在于：可以在短时间内、较低的烧结温度下制备出致密度高、成分均匀、性能优异的高铌钛铝基合金块体材料；具有节能环保，操作简单，可重复性强。The invention discloses a method for preparing a high-niobium-titanium-aluminum-based alloy material by spark plasma sintering, which belongs to the technical field of high-niobium-titanium-aluminum intermetallic compound materials. Use the raw material powder composed of element mixed powder and alloy powder, put it into the graphite mold, and then put it into the discharge plasma sintering furnace, apply an axial pressure of 10-80MPa, and use a vacuum condition of 10-2-6Pa or inert Sintering is carried out under gas protection, the heating rate is 50-800°C/min, and the sintering temperature is 900-1400°C. After heat preservation, it is cooled to room temperature with the furnace to obtain a high Nb-TiAl-based alloy bulk material. The advantages are: high niobium-titanium-aluminum-based alloy bulk materials with high density, uniform composition and excellent performance can be prepared in a short period of time and at a relatively low sintering temperature; they are energy-saving, environmentally friendly, easy to operate and highly repeatable.
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): 1216) 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 properties of nanocrystallineTi-Al-X alloys.Materials Science And Engineering, 2002, A329-331:196-205; 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 art 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-8.5Nd-0.2B-0.2W-0.1Y powdered alloy (spherical powder art in advance, 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, add axle pressure and be 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
| Sintering temperature/℃ | Types of organization | Compression performance | ||
| σ bc/MPa | σ 0.2c/MPa | ε c/％ | ||
| 1050 1100 1150 1200 1250 | DP DP NL FL FL | 3200 3103 2967 2927 2888 | 1356 1157 1038 922 878 | 47.3 29 27.2 26.9 26.9 |
*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-8.5Nd-0.2B-0.2W-0.1Y alloy powder art 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%.
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| CN104625066A (en) * | 2015-01-30 | 2015-05-20 | 北京科技大学 | Method for manufacturing high-niobium titanium-aluminum alloy material by adopting two-step pressure infiltration |
| 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 |
| WO2016055013A1 (en) * | 2014-10-09 | 2016-04-14 | 南京理工大学 | Tial intermetallic compound single crystal material and preparation method therefor |
| CN107130139A (en) * | 2017-06-15 | 2017-09-05 | 北京科技大学 | A kind of method of the intensified-sintered Powder Metallurgy TiAl based Alloys of addition 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 |
| CN108034866A (en) * | 2018-01-22 | 2018-05-15 | 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 |
| CN113927031A (en) * | 2021-10-18 | 2022-01-14 | 四川大学 | A method of Ti-5Al-5Mo-5V-3Cr-Zr alloy doping with Y to improve the properties of titanium alloy |
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| JPH09287038A (en) * | 1996-04-23 | 1997-11-04 | Ishikawajima Harima Heavy Ind Co Ltd | Method for producing composite product of TiAl alloy and metal fiber |
| CN1142305C (en) * | 2001-11-08 | 2004-03-17 | 北京科技大学 | High temperature high performance high-niobium titanium-aluminium alloy |
| US7566415B2 (en) * | 2002-11-18 | 2009-07-28 | Adma Products, Inc. | Method for manufacturing fully dense metal sheets and layered composites from reactive alloy powders |
| CN1478757A (en) * | 2003-07-18 | 2004-03-03 | 清华大学 | A method for preparing high-purity bulk titanium-aluminum-carbon material by spark plasma sintering |
| CN100425722C (en) * | 2005-11-30 | 2008-10-15 | 济南大学 | Method for improving property of TiAI intermetallic compound based composite material |
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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 |
| CN104625066A (en) * | 2015-01-30 | 2015-05-20 | 北京科技大学 | Method for manufacturing high-niobium titanium-aluminum alloy material by adopting two-step pressure infiltration |
| 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 |
| CN107130139A (en) * | 2017-06-15 | 2017-09-05 | 北京科技大学 | A kind of method of the intensified-sintered Powder Metallurgy TiAl based Alloys of addition Sn |
| 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 |
| CN108034866A (en) * | 2018-01-22 | 2018-05-15 | 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 |
| CN113927031A (en) * | 2021-10-18 | 2022-01-14 | 四川大学 | A method of Ti-5Al-5Mo-5V-3Cr-Zr alloy doping with Y to improve the properties of titanium 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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