CN101250635A - Method for manufacturing high performance sinter Mo-Ti-Zr molybdenum alloy - Google Patents
Method for manufacturing high performance sinter Mo-Ti-Zr molybdenum alloy Download PDFInfo
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- CN101250635A CN101250635A CNA2008100310445A CN200810031044A CN101250635A CN 101250635 A CN101250635 A CN 101250635A CN A2008100310445 A CNA2008100310445 A CN A2008100310445A CN 200810031044 A CN200810031044 A CN 200810031044A CN 101250635 A CN101250635 A CN 101250635A
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Abstract
The invention relates to a method for preparing high-performance Mo-Ti-Zr(TZM) through utilizing powder metallurgy, which comprises the following steps: mechanically milling metal Mo powder, Ti(TiH2), Zr(ZrH2) powder and organic binder in a high energy ball mill, preparing pre-alloyed powder which is evenly mixed, pressing and forming mixed powder, presintering pressed compact in protective atmosphere, dehydrogenating, deoxidizing, wherein deoxidizing, controlling carbon and sintering in high temperature in high-temperature protective atmosphere, and finally, doing sintering later process for sintered compact. The mechanical property of TZM molybdenum alloy which is prepared by the method of the invention is better than that of alloy which is manufactured by a normal powder metallurgy process, wherein the highest tensile strength can reach570-600Mpa, and percentage of elongation reaches 19-25%.
Description
Technical field:
The present invention relates to field of powder metallurgy, particularly adopt powder metallurgy process to prepare the method for high-performance TZM (Mo-Ti-Zr) molybdenum alloy.
Background technology:
The TZM alloy is comparatively use always in the molybdenum base alloy a kind of, because of it has the fusing point height, intensity is big, electrical and thermal conductivity performance good, etch resistant properties reaches advantages such as mechanical behavior under high temperature is good by force, be used to process high-temperature structural material in a large number, obtained in high temperature fields such as Aeronautics and Astronautics and atomic energy industry very to use widely.At present, alloying element Ti, Zr and C add among the Mo preparation TZM alloy to can adopt arc melting method and powder metallurgic method, wherein comparatively general with arc melting.Yet this method technology is very complicated, especially fusion process, because various element fusing points differ greatly, the poly-partially phenomenon of element is serious in the alloy, and minimizing the poly-partially method of alloying element is to repeat that the alloy ingot bar is worn into powder repeatedly to repeat melting, like this, just, make operation more complicated.Simultaneously, the coarse microstructure of arc melting method institute alloyage, yield rate is lower, and amount of finish is big, causes its production cost very high.The powder metallurgy process operation is simple relatively, can save main equipments such as vacuum arc fumace, large-size extruder and forging hammer and corresponding high-temperature heater, operation is simplified, production cycle shortens, consume and reduce, throughput and yield rate are improved, the component of preparing are complex-shaped, finished product is near net shape, amount of finish is few or do not have processing, material use efficiency height, and the gained alloy microscopic structure is even simultaneously, and crystal grain is more tiny, quality product is higher, has lower Financial cost and very large technical superiority.At present, more existing researchers have studied the powder metallurgy technology of preparing of TZM alloy both at home and abroad, prepared TZM alloy strength scope is between 490～540MPa, its intensity still has much room for improvement, and the lower defective of toughness that the TZM alloy of ordinary powder metallurgical method preparation simultaneously exists is still the bottleneck of this kind of restriction alloy on using.
Summary of the invention:
The present invention has overcome the deficiency of arc melting and ordinary powder metallurgical technology, adopts high-energy ball milling+compression molding+presintering+high temperature sintering+sintering postorder treatment technology to prepare high-performance TZM molybdenum alloy.With metal M o powder, with Ti or TiH
2With Zr or ZrH
2Powder and organic binder bond carry out mechanical ball milling in high energy ball mill, prepare the powdered alloy that mixes; Adopt compression moulding to prepare the alloy pressed compact; pressed compact is carrying out low temperature presintering and high temperature sintering respectively under protective atmosphere; last sintered blank is carried out the sintering postorder and is handled under protective atmosphere; the alloy excellence that the prepared TZM molybdenum alloy mechanical property that goes out is made than arc melting method and ordinary powder metallurgy method; the high energy of tensile strength reaches 570～600Mpa, and unit elongation reaches 19～25%.
For achieving the above object, scheme of the present invention is:
The preparation method of a kind of powder metallurgy high-performance Mo-Ti-Zr (TZM) molybdenum alloy is characterized in that:
(1) alloying element and composition thereof be Ti (0.4～1.0wt%), Zr (0.06～0.12wt%) and C (0.01～0.04wt%), surplus is Mo;
(2) powdered alloy adds 0.5～1.5wt% organic binder bond, adopts high-energy ball milling to prepare pre-alloyed powder, and organic binder bond is one or more organic binder bonds among paraffin, polyoxyethylene glycol, stearic acid or the PVB;
(3) with the compression moulding on press of prepared pre-alloyed powder;
(4) prepared pressed compact is carried out presintering, dehydrogenation and deoxidation under protective atmosphere, its technology is: be raised to 250～600 ℃ of insulation 30～150min from room temperature, be raised to 700～1200 ℃ of insulation 30～180min again.The protective atmosphere that adopts can be vacuum, N
2, Ar, H
2In one or both;
(5) presintered compact is carried out high temperature sintering under protective atmosphere, deoxidation and control carbon, its technology is: be raised to 1200～1700 ℃ of insulation 30～150min from room temperature, be raised to 1800～2050 ℃ of insulation 60～210min at last.The protective atmosphere that adopts can be vacuum, N
2, Ar, H
2In one or both;
(6) sintered blank of preparation is further handled under protective atmosphere, at 1100～1500 ℃ of insulation 30～180min, protective atmosphere is a vacuum, N
2, Ar, H
2In one or both;
(7) alloy sample after the thermal treatment is carried out Performance Detection, the high energy of its tensile strength reaches 580～600Mpa, and unit elongation reaches 19～25%, the alloy excellence that alloy mechanical property is made than the ordinary powder metallurgy method.
Advantage of the present invention and positively effect are embodied in:
1. employing powder metallurgy process, with respect to the arc melting method, its operation is simple, and the gained alloy property is higher simultaneously.
2. adopt the mixed powder high-energy ball milling to prepare pre-alloyed powder, pre-alloyed powder adopts presintering, dehydrogenation deoxidation+high temperature sintering, high temperature deoxidation control carbon+sintering postorder treatment technology to prepare the TZM alloy after moulding, with respect to ordinary powder metallurgical technology institute alloyage, its tensile strength improves greatly, overcome the general low problem of powder metallurgy TZM alloy unit elongation simultaneously, unit elongation reaches 19～25%.
3. adopt high-energy ball milling to prepare powdered alloy, it is pre-alloyed that machinery takes place mixed powder, improved the solid solution capacity of alloying element in Mo.
Embodiment:
Example 1:
(1) be example with preparation 300g powdered alloy, by mass percentage, take by weighing the quality of each component of powdered alloy:
Stearic acid heating for dissolving in alcohol is put into ball grinding cylinder with powder, charges into N in ball grinding cylinder
2Gas, setting the ball milling time is 5h, the preparation pre-alloyed powder.Take out powder, drying, standby with the bag encapsulation then.
(2) with made pre-alloyed powder compression moulding.
(3) with pressed compact presintering under vacuum atmosphere of preparation, its technology is: be raised to 380 ℃ of insulation 45min from room temperature, be raised to 1100 ℃ of insulation 150min again;
(4) presintered compact that obtains is led to the hydrogen high temperature sintering, its technology is: be raised to 1450 ℃ of insulation 100min from room temperature, be raised to 1950 ℃ of insulation 200min at last;
(5) sintered blank that obtains is incubated 30min under 1200 ℃ of Ar gas atmosphere, then furnace cooling;
(6) alloy sample after will handling carries out Performance Detection, and its tensile strength can reach more than the 575Mpa, and unit elongation reaches more than 20%.
Example 2:
(1) be example with preparation 300g powdered alloy, by mass percentage, take by weighing the quality of each component of powdered alloy:
Stearic acid heating for dissolving in alcohol is put into ball grinding cylinder with powder, charges into N in ball grinding cylinder
2Gas, setting the ball milling time is 15h, the preparation pre-alloyed powder.Take out powder, drying, standby with the bag encapsulation then.
(2) with the pre-alloyed powder compression moulding for preparing.
(3) pressed compact that is shaped is carried out hydrogen presintering, its technology is: be raised to 450 ℃ of insulation 30min from room temperature, be raised to 1050 ℃ of insulation 120min again
(4) with presintered compact high temperature sintering in cracked ammonium atmosphere, its technology is: be raised to 1400 ℃ of insulation 100min from room temperature, be raised to 1920 ℃ of insulation 200min at last.
(5) sintered blank is incubated 60min under 1350 ℃ of vacuum atmospheres.
(6) with the alloy sample Performance Detection after handling in (5), its tensile strength can reach more than the 590Mpa, and unit elongation reaches more than 23%.
Claims (4)
1. the preparation method of a powder metallurgy high-performance Mo-Ti-Zr molybdenum alloy is characterized in that:
(1) with composition is the Zr of Ti, 0.06～0.12wt% of 0.4～1.0wt% and the C of 0.01～0.04wt%; surplus is the powdered alloy of Mo; with one or more organic binder bonds among paraffin, polyoxyethylene glycol, stearic acid or the PVB of 0.5～1.5wt%; adopt mechanical ball milling to prepare pre-alloyed powder, the protective atmosphere in the mechanical milling process is vacuum, Ar gas or N
2Gas;
(2) with prepared pre-alloyed powder compression moulding;
(3) prepared pressed compact is carried out presintering, dehydrogenation and deoxidation under protective atmosphere, its technology is: be raised to 250～600 ℃ of insulation 30～150min from room temperature, be raised to 700～1200 ℃ of insulation 30～180min again, the protective atmosphere of employing is a vacuum, N
2, Ar or H
2In one or both;
(4) presintered compact with preparation carries out high temperature sintering under protective atmosphere, deoxidation and control carbon, and its technology is: be raised to 1200～1700 ℃ of insulation 30～150min from room temperature, be raised to 1800～2050 ℃ of insulation 60～210min at last, the protective atmosphere of employing is a vacuum, N
2, Ar or H
2In one or both;
(5) sintered blank of preparation is further handled under protective atmosphere, at 1100～1500 ℃ of insulation 30～180min, obtained tensile strength and be up to 570～600Mpa, unit elongation reaches 19～25% molybdenum alloy.
2. the preparation method of Mo-Ti-Zr molybdenum alloy according to claim 1 is characterized in that: alloying element Ti is pure metal powder or its hydride powder TiH
2, alloy element Zr is pure metal powder or its hydride powder ZrH
2
3. the preparation method of sinter Mo-Ti-Zr molybdenum alloy according to claim 1; it is characterized in that: the described described high-energy ball milling of step (1) adopts dry grinding or adds the wet-milling of ball-milling medium, and the ball-milling medium that wet milling process adopted is that dehydrated alcohol, industrial naptha and acetone liquid protective atmosphere can be vacuum, Ar gas or N
2Gas, the ball milling time is 3h～20h.
4. the preparation method of sinter Mo-Ti-Zr molybdenum alloy according to claim 1, it is characterized in that: the protective atmosphere described in the step (5) is a vacuum, N
2, Ar, H
2In one or both.
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|---|---|---|---|---|
| CN101934372A (en) * | 2010-07-30 | 2011-01-05 | 西北有色金属研究院 | Method for preparing large powder metallurgy TZM blank with uniform carbon and oxygen distribution |
| CN102717061A (en) * | 2011-03-29 | 2012-10-10 | 厦门钨业股份有限公司 | A paraffin base compound forming agent for a water base cemented carbide mixture |
| CN103276266A (en) * | 2013-06-08 | 2013-09-04 | 金堆城钼业股份有限公司 | Method for preparing TZM alloy material through spray drying |
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| CN103627940A (en) * | 2013-11-27 | 2014-03-12 | 江西理工大学 | Powder metallurgical molybdenum base material applied to hot extrusion die and method for forming die |
| CN105451916A (en) * | 2014-05-13 | 2016-03-30 | 犹他大学研究基金会 | Production of substantially spherical metal powers |
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| CN110273149A (en) * | 2019-07-31 | 2019-09-24 | 安徽工业大学 | A kind of molybdenum-base alloy coating and the matrix with the alloy coat |
| CN110856870A (en) * | 2018-08-24 | 2020-03-03 | 可成科技股份有限公司 | Titanium-based workpiece and manufacturing method thereof |
| CN111203531A (en) * | 2020-03-02 | 2020-05-29 | 北京理工大学 | Powder metallurgy normal-pressure multi-step sintering method of high-density Ti-Nb-Mo alloy |
| CN112496326A (en) * | 2020-11-10 | 2021-03-16 | 中南大学 | Oxygen removing process for injection molding titanium alloy and application thereof |
| CN113637884A (en) * | 2021-07-20 | 2021-11-12 | 深圳大学 | Novel high-performance molybdenum alloy and preparation method thereof |
| CN117684033A (en) * | 2024-02-04 | 2024-03-12 | 有研工程技术研究院有限公司 | High-performance TZM alloy foil and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3995587A (en) * | 1973-06-28 | 1976-12-07 | General Electric Company | Continuous casting apparatus including Mo-Ti-Zr alloy bushing |
| US4945750A (en) * | 1987-02-02 | 1990-08-07 | Gte Products Corporation | Press forging of molybdenum or molybdenum alloy parts |
-
2008
- 2008-04-11 CN CNB2008100310445A patent/CN100567530C/en not_active Expired - Fee Related
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