CN101089209A - Method for preparing high Nb-Ti-Lu porous material - Google Patents
Method for preparing high Nb-Ti-Lu porous material Download PDFInfo
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- CN101089209A CN101089209A CN 200710118710 CN200710118710A CN101089209A CN 101089209 A CN101089209 A CN 101089209A CN 200710118710 CN200710118710 CN 200710118710 CN 200710118710 A CN200710118710 A CN 200710118710A CN 101089209 A CN101089209 A CN 101089209A
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- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000011148 porous material Substances 0.000 title claims description 43
- 239000000843 powder Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910004349 Ti-Al Inorganic materials 0.000 claims description 4
- 229910004692 Ti—Al Inorganic materials 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004411 aluminium Substances 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001275 Niobium-titanium Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000010955 niobium Substances 0.000 description 18
- 238000009826 distribution Methods 0.000 description 16
- 239000010936 titanium Substances 0.000 description 14
- 230000003078 antioxidant effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910021362 Ti-Al intermetallic compound Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000011800 void material Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011236 particulate material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910006281 γ-TiAl Inorganic materials 0.000 description 1
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Abstract
This invention relates to the production of intermetallic compounds. The raw materials of titanium powder, aluminium powder and niobium powder mixture is pressed to form billets by using die forming method. The lower temperature pre-reaction at temperature of 500-800 deg.C for 50-150 min is proceeded upon the billets; and then higher temperature sintering synthesis of up-said billets is proceeded at temperature of 1300-1400 deg.C for 60-180 min. vacuum low pressure sintering method is used for said reaction with its vacuum degree of 0.1-0.001 Pa, and its pressure of 0.5-10 KPa to produce high niobium titanium aluminium porous intermetallic compound.
Description
Technical field
The invention belongs to the intermetallic compound technical field, a kind of method for preparing high Nb-Ti-Lu porous material particularly is provided.Specifically be the preparation method of titanium, aluminium and the synthetic high-Nb Ti-Al porous intermetallic compound of niobium element powders reaction.
Background technology
Porous material has become the performance function-structured material with huge applications potentiality owing to have excellent physics, mechanical property concurrently.The high porosity of porous material makes it have less density and low heat-conduction coefficient, has caused huge thermal resistance and smaller volume thermal capacitance, becomes traditional lagging material.Porous material is widely used at numerous industrial circles such as aerospace, the energy, chemical industry and metallurgy.The greatest drawback of common porous metal material is corrosion resistance difference and high-temperature behavior deficiency.Common porous ceramics matter crisp and not anti-thermal shock, intensity is relatively poor and be difficult to weld assemblyization.Therefore, the porous material that has excellent adiabatic capacity and hot strength, easily processing assembling concurrently becomes new research focus.
The high-Nb Ti-Al intermetallic compound is as potential lightweight high-temperature structural material, concentrated the advantage of pottery and plain metal, show excellent physicals, mechanical property and good high temperature oxidation resistance and anti-various by force/weak acid alkali salt mist corrosive nature.With the high-Nb Ti-Al intermetallic compound as porous material, can solve the high-temperature oxidation resistant of plain metal and antiacid caustic corrosion poor performance and ceramic porous material preferably and be difficult to technological difficulties such as weld assemblyization and intensity is relatively poor, carry high-Nb Ti-Al belong between the use properties of compound porous material and expansion Service Environment etc.Compare with common porous material, the high Nb-Ti-Lu porous material preparation process is simple, and is with low cost, and preparation process does not have any environmental pollution.Simultaneously, the high Nb-Ti-Lu porous material hole forms the solution of problem in science such as mechanism, also is the basic theory and the favourable of assessment of performance of porous material are replenished, and has important significance for theories.According to the new patent searching result, adopt Ti, Al, the synthetic preparation of Nb element powders reaction high-Nb Ti-Al intermetallic compound porous material, still there is not other any relevant report both at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing high Nb-Ti-Lu porous material.This alloy has low density, mechanical behavior under high temperature is good, antioxidant property is high and characteristics, especially hot environment such as heat-proof quality excellence under, play and stop or reduce the effect that heat transmits.This will expand the range of application of high-Nb Ti-Al intermetallic compound.
The technical solution used in the present invention is:
At first composition proportion is that 35～55at.%Ti powder, 35-55at.%Al powder and 5～30at.%Nb powder mix uniformly.The particle diameter of Ti powder is 10～150 μ m, and the particle diameter of Al powder is that the particle diameter of 5～150 μ m and Nb powder is 2～25 μ m.
Adopt the mode of compression molding, be pressed into laminar blank, pressing pressure is 50～500MPa.Subsequently, adopt two elementary reaction synthesis technique sintering, i.e. low temperature pre-reaction and pyroreaction.The temperature in low temperature pre-reaction stage is 500～800 ℃, and soaking time is 50～150 minutes; The temperature in pyroreaction stage is 1300～1400 ℃, and soaking time is 60～180 minutes.Sintering processing adopts vacuum minute-pressure sintering, and vacuum tightness is 1 * 10
-1～1 * 10
-3Pa, pressure is 0.5～10KPa.After reaction was finished, controlled chilling speed by 10～40 ℃/min cooling, thereby obtained the high-Nb Ti-Al porous intermetallic compound.
The invention effect
(1) because high niobium containing titanium aluminium alloy has that density is little, use temperature is high (800～900 ℃, can reach 1200 ℃ in short-term), mechanical behavior under high temperature and antioxidant property excellence, acidproof/caustic corrosion is strong, adopt high niobium containing titanium aluminium alloy to prepare porous material, can increase substantially the work-ing life and the Service Environment of porous material, and enlarge the use range of porous material.
(2) adopt the high-Nb Ti-Al intermetallic compound to prepare porous material, help the pore size distribution of control material, adapt to different application requiring.The pore-creating mechanism that adopts the synthetic high Nb-Ti-Lu porous material of element powder reaction is that Al element and the inclined to one side diffusion of Ti generation cause the Kirkendall effect.This effect can cause the percentage of open area of high Nb-Ti-Lu porous material 20～55%, and powder metallurgical technique itself produces a certain amount of mesopore in addition.By the control certain process conditions,, can obtain the accurately porous insert of control of aperture as granularity and composition proportion, pressing pressure, sintering temperature and the soaking time etc. of Ti and Al powder.
(3) pore-creating owing to utilize inclined to one side diffusion between Ti and the Al need not added pore-forming material can obtain 30～65% porosity, thereby has avoided removing the pore-forming material link in the traditional preparation process technology, has saved the energy, and pollution-free, and simple to operate.
Description of drawings
Fig. 1 is the hole shape looks of Ti-48Al-6Nb (1350 ℃/180min high temperature sintering) porous material.
Fig. 2 is the pore size distribution curve of Ti-48Al-6Nb (1350 ℃/180min high temperature sintering) porous material.
Fig. 3 is the hole shape looks of Ti-48Al-6Nb (1300 ℃/60min high temperature sintering) porous material.
Fig. 4 is a particulate material pattern in Ti-48AI-6Nb (1300 ℃/60min high temperature sintering) porous material.
Fig. 5 is the pore size distribution curve of Ti-48Al-6Nb (1300 ℃/60min high temperature sintering) porous material.
Embodiment
Embodiment 1: adopt granularity to be Ti powder and the Al powder of 40～75 μ m, granularity is the Nb powder of 5～25 μ m, carries out proportioning by Ti-48AI-6Nb (at.%) composition, after mixing, carry out die forming under 200MPa pressure, suppressing diameter is 33mm, the sheet of the thick 2～3mm base of colding pressing.Sintering adopts two elementary reaction synthesis techniques, vacuum atmosphere, and vacuum degree control is 1 * 10
-2～1 * 10
-3Pa.The low temperature reaction sintering temperature is 600 ℃, and soaking time is 120min, and high temperature sintering is 1350 ℃, and soaking time is 180min, and pressurization pressure is 1.2KPa.After reaction finished, rate of cooling was controlled at 30 ℃/min.The high Nb-Ti-Lu porous material of this acquisition is arranged, have even pore distribution, not of uniform size and be mazy pore structure, as shown in Figure 1.The sintered compact skeleton is by γ-TiAl/ α
2-Ti
3The Al lamella is formed, and void distribution therebetween.Porosity 48～53%; The aperture is normal distribution, and narrow distribution range is seen Fig. 2.Thermal conductivity is 2.4W2m
-1K
-1, have excellent antioxidant property simultaneously.
Embodiment 2: adopt granularity to be Ti powder and the Al powder of 75～150 μ m, granularity is the Nb powder of 5～25 μ m, carries out proportioning by Ti-48Al-8Nb (at.%) composition, after mixing, carry out die forming under 50MPa pressure, suppressing diameter is 33mm, the sheet of the thick 2～3mm base of colding pressing.Sintering adopts two elementary reaction synthesis techniques, vacuum atmosphere, and vacuum degree control is 1 * 10
-2～1 * 10
-3Pa.The low temperature reaction sintering temperature is 550 ℃, and soaking time is 150min, and high temperature sintering is 1350 ℃, and soaking time is 180min.Pressurization pressure is 2.1KPa.After reaction finished, rate of cooling was controlled at 40 ℃/min.The high Nb-Ti-Lu porous material of this acquisition is arranged, have even pore distribution, not of uniform size and be mazy pore structure.The sintered compact skeleton is by γ/α
2Lamella is formed, and void distribution therebetween.Porosity 50～55%; The aperture is normal distribution, and thermal conductivity is 2.0Wm
-1K
-1, have excellent antioxidant property simultaneously.
Embodiment 3: adopt granularity to be Ti powder and the Al powder of 10～25 μ m, granularity is the Nb powder of 5～25 μ m, carries out proportioning by Ti-48Al-6Nb (at.%) composition, after mixing, carry out die forming under 375MPa pressure, suppressing diameter is 33mm, the sheet of the thick 2～3mm base of colding pressing.Sintering adopts two elementary reaction synthesis techniques, vacuum atmosphere, and vacuum degree control is 1 * 10
-2～1 * 10
-3Pa.The low temperature reaction sintering temperature is 600 ℃, and soaking time is 120min, and high temperature sintering is 1335 ℃, and soaking time is 180min.Pressurization pressure is 1.6KPa.After reaction finished, rate of cooling was controlled at 30 ℃/min.The high Nb-Ti-Lu porous material of this acquisition is arranged, have even pore distribution, not of uniform size and be mazy pore structure.The sintered compact skeleton is by γ/α
2Lamella is formed, and void distribution therebetween.Porosity 24～29%; The aperture is normal distribution, and thermal conductivity is 6.1Wm
-1K
-1, have excellent antioxidant property simultaneously.
Embodiment 4: adopt granularity to be Ti powder and the Al powder of 25～40 μ m, granularity is the Nb powder of 5～25 μ m, carries out proportioning by Ti-48Al-6Nb (at.%) composition, after mixing, carry out die forming under 200MPa pressure, suppressing diameter is 33mm, the sheet of the thick 2～3mm base of colding pressing.Sintering adopts two elementary reaction synthesis techniques, vacuum atmosphere, and vacuum degree control is 1 * 10
-2～1 * 10
-3Pa.The low temperature reaction sintering temperature is 600 ℃, and soaking time is 120min, and high temperature sintering is 1300 ℃, and soaking time is 60min.Pressurization pressure is 0.5KPa.After reaction finished, rate of cooling was controlled at 30 ℃/min.The high Nb-Ti-Lu porous material of this acquisition is arranged, have even pore distribution, not of uniform size and be mazy pore structure.The sintered compact skeleton is mainly by γ/α
2Lamella is formed, and has a spot of AlNb in addition
2Phase, void distribution are seen Fig. 3 therebetween.Some granular materials on skeleton, occur, determine that through composition analysis particulate material is γ or the α of solid solution Nb
2Fig. 4 is the granular material pattern on the skeleton.Wherein, A particulate component (atomic ratio) is: Ti-59.47, Al-32.21, Nb-8.32; The B particulate component is: Ti-55.14, Al-33.39, Nb-11.46; The C particulate component is: Ti-49.49, Al-48.18, Nb-2.33; The D particulate component is: Ti-50.06, Al-45.41, Nb-4.53.Porosity 28～33%; The aperture is skewed distribution, two most probable apertures occur, sees Fig. 5.Thermal conductivity is 6.1Wm
-1K
-1, have excellent antioxidant property simultaneously.
Claims (2)
1, a kind of method for preparing high Nb-Ti-Lu porous material is characterized in that: at first composition proportion is that 35～55at.%Ti powder, 35～55at.%Al powder and 5～30at.%Nb powder mix uniformly; Adopt the mode of compression molding, be pressed into laminar blank, pressing pressure is 50～500MPa; Subsequently, adopt low temperature pre-reaction and pyroreaction synthesis technique sintering, the temperature in low temperature pre-reaction stage is 500～800 ℃, and soaking time is 50～150 minutes; The temperature in pyroreaction stage is 1300～1400 ℃, and soaking time is 60～180 minutes; Sintering processing adopts vacuum minute-pressure sintering, and vacuum tightness is 1 * 10
-1～1 * 10
-3Pa, pressure is 0.5～10KPa; After reaction was finished, controlled chilling speed by 10～40 ℃/min cooling, obtained the high-Nb Ti-Al porous intermetallic compound.
2, in accordance with the method for claim 1, it is characterized in that: the particle diameter of Ti powder is 10～150 μ m, and the particle diameter of Al powder is that the particle diameter of 5～150 μ m and Nb powder is 2～25 μ m.
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| CN101089209A true CN101089209A (en) | 2007-12-19 |
| CN100465311C CN100465311C (en) | 2009-03-04 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967578A (en) * | 2010-11-02 | 2011-02-09 | 北京科技大学 | Preparation method of gradient pore porous high-niobium titanium-aluminum alloy |
| CN101994043A (en) * | 2010-12-08 | 2011-03-30 | 北京科技大学 | High Nb containing TiAl porous intermetallic compound gradient material and preparation method thereof |
| CN102717086A (en) * | 2012-07-04 | 2012-10-10 | 北京科技大学 | Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process |
| CN102888530A (en) * | 2012-05-17 | 2013-01-23 | 吉林省必晟科技开发有限公司 | Method for preparing TiAl-based alloy |
| CN104109778A (en) * | 2014-08-12 | 2014-10-22 | 天津银龙高科新材料研究院有限公司 | High-damping Ti-Nb-Fe-O alloy and preparation method thereof |
| CN104404288A (en) * | 2014-11-23 | 2015-03-11 | 北京科技大学 | Method for preparing light Nb-Ti-Al based porous material |
| CN104903031A (en) * | 2013-03-01 | 2015-09-09 | 三菱综合材料株式会社 | Porous aluminum sintered compact |
| CN105386026A (en) * | 2015-11-05 | 2016-03-09 | 北京科技大学 | Method for preparing gamma aluminum oxide nano-porous layer on surface of porous alloy framework |
| CN105499576A (en) * | 2016-01-11 | 2016-04-20 | 北京科技大学 | Method for preparing porous titanium-aluminium alloy through powder metallurgy |
| CN107245594A (en) * | 2017-06-23 | 2017-10-13 | 歌尔股份有限公司 | The preparation method of powdered metallurgical material |
| CN109890932A (en) * | 2016-10-12 | 2019-06-14 | 香港科技大学 | The aluminium composite material with ceramic substrate of lightweight and high tenacity |
| CN115961169A (en) * | 2021-10-08 | 2023-04-14 | 哈尔滨工业大学 | Nb-phase toughened high-strength high-plasticity gamma-TiAl-based alloy and preparation method thereof |
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|---|---|---|---|---|
| DE10058155A1 (en) * | 2000-11-22 | 2002-05-23 | Geesthacht Gkss Forschung | Alloy based on titanium aluminides produced using a smelting and powder metallurgical process and containing an alloy composition made from titanium, aluminum and niobium has specified an aluminum content |
| US6852273B2 (en) * | 2003-01-29 | 2005-02-08 | Adma Products, Inc. | High-strength metal aluminide-containing matrix composites and methods of manufacture the same |
| JP2004238670A (en) * | 2003-02-05 | 2004-08-26 | Showa Denko Kk | Electrode material for capacitor, its manufacturing method, and electrolytic capacitor |
-
2007
- 2007-07-12 CN CNB2007101187104A patent/CN100465311C/en not_active Expired - Fee Related
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| CN101967578B (en) * | 2010-11-02 | 2012-05-09 | 北京科技大学 | Preparation method of gradient pore porous high-niobium titanium-aluminum alloy |
| CN101967578A (en) * | 2010-11-02 | 2011-02-09 | 北京科技大学 | Preparation method of gradient pore porous high-niobium titanium-aluminum alloy |
| CN101994043A (en) * | 2010-12-08 | 2011-03-30 | 北京科技大学 | High Nb containing TiAl porous intermetallic compound gradient material and preparation method thereof |
| CN102888530B (en) * | 2012-05-17 | 2015-12-09 | 吉林省必晟科技开发有限公司 | A kind of preparation method of TiAl-base alloy |
| CN102888530A (en) * | 2012-05-17 | 2013-01-23 | 吉林省必晟科技开发有限公司 | Method for preparing TiAl-based alloy |
| CN102717086A (en) * | 2012-07-04 | 2012-10-10 | 北京科技大学 | Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process |
| CN102717086B (en) * | 2012-07-04 | 2014-09-17 | 北京科技大学 | Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process |
| US9669462B2 (en) | 2013-03-01 | 2017-06-06 | Mitsubishi Materials Corporation | Porous aluminum sintered compact |
| CN104903031A (en) * | 2013-03-01 | 2015-09-09 | 三菱综合材料株式会社 | Porous aluminum sintered compact |
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| CN104404288A (en) * | 2014-11-23 | 2015-03-11 | 北京科技大学 | Method for preparing light Nb-Ti-Al based porous material |
| CN104404288B (en) * | 2014-11-23 | 2016-08-24 | 北京科技大学 | A kind of method preparing lightweight Nb-Ti-Al based porous materials |
| CN105386026A (en) * | 2015-11-05 | 2016-03-09 | 北京科技大学 | Method for preparing gamma aluminum oxide nano-porous layer on surface of porous alloy framework |
| CN105386026B (en) * | 2015-11-05 | 2018-06-12 | 北京科技大学 | The method that porous alloy skeleton surface prepares gamma alundum (Al2O3) nano porous layer |
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| CN107245594B (en) * | 2017-06-23 | 2019-02-26 | 歌尔股份有限公司 | The preparation method of powdered metallurgical material |
| CN115961169A (en) * | 2021-10-08 | 2023-04-14 | 哈尔滨工业大学 | Nb-phase toughened high-strength high-plasticity gamma-TiAl-based alloy and preparation method thereof |
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| CN100465311C (en) | 2009-03-04 |
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