CN1962911A - Process for preparing molybdenum alloy TZM by powder metallurgy - Google Patents
Process for preparing molybdenum alloy TZM by powder metallurgy Download PDFInfo
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Abstract
The invention discloses a preparing method of difficult dissolving alloy through powder metallurgical technique, which is characterized by the following: selecting titanium hydride and zirconium hydride particle of Fisher grain at 5-10um with maximum particle not more than 10um; preparing TZM modybdenum alloy; dispersing evenly in the sintering course due to little second phase grain size; improving high-temperature property and normal-temperature fragility.
Description
Technical field
A kind of method of preparing molybdenum alloy TZM by powder metallurgy relates to a kind of employing powder metallurgical technique and prepares the refractory metal alloy method.
Background technology
The TZM molybdenum alloy is a kind of molybdenum alloy commonly used, because it has excellent high-temperature intensity, good electrical conductivity and hot expansibility, thereby it has purposes very widely at thermal structure spare, aerospace industry, electronic industry and glass work.Powder metallurgy process is a kind of less expensive method of preparation TZM molybdenum alloy, thereby has obtained using widely.General, the titanium hydride that conventional powder metallurgy TZM molybdenum alloy is selected for use and the Fisher particle size of zircoium hydride powder are greater than 20 μ m, the problem of bringing thus mainly shows: because the second phase particle size is bigger, sintering process subsequently is difficult to make its diffusion evenly (1); (2) because the inhomogeneous homogeneity of material structure that causes of sintering diffusion reduces, this has not only influenced the high-temperature behavior of material, more makes material show fragility at normal temperature.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, and a kind of homogeneity that can effectively improve the sintering process material structure is provided, the method for the preparing molybdenum alloy TZM by powder metallurgy of the performance of raising material.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of preparing molybdenum alloy TZM by powder metallurgy is characterized in that it being to select for use Fisher particle size at 5-10 μ m, and largest particle is not more than titanium hydride and the zircoium hydride particle of 10 μ m, adopts powder metallurgy method to prepare the TZM molybdenum alloy.
Adopt the molybdenum alloy TZM of method preparation of the present invention, can prepare TZM sheet material, bar and the foil of excellent property.
The method of a kind of preparing molybdenum alloy TZM by powder metallurgy of the present invention is characterized in that its preparation process comprises following process successively:
(1) in molybdenum powder, adds titanium hydride, zircoium hydride and carbon black, make its shared part by weight in alloy be: 0.4%～0.55% titanium hydride, 0.06%～0.12% zircoium hydride, 0.01%～0.04% carbon black; Adopt ball milling or V-type machine batch mixing that molybdenum powder, titanium hydride, zircoium hydride and carbon black ground and mixed is even; Ball material weight ratio is 2～0.5: 1, mixing time 1～24 hour.
(2) material after the method ground and mixed of static pressure such as employing or mold pressing is 1.80～3t/cm at pressure
2Under the condition, pressurize was pressed into blank in 0.5～2 minute;
(3) adopt vacuum or hydrogen shield atmosphere sintering compacting blank, sintering temperature is 1800-2000 ℃, soaking time 2～8 hours;
(4) adopt known method forgings, rolling TZM molybdenum alloy bar material, sheet material and foil, cogging temperature is controlled to be 1400～1600 ℃, and amount of finish is to carry out the stress-removal processing at 50～95% o'clock.
Employing powder metallurgical technique of the present invention prepares the method for molybdenum alloy TZM, by adding the tiny alloying element powder of particle; Because the second phase particle size is little, make the sintering process diffusion evenly; Improve the homogeneity of material structure, improved the high-temperature behavior and the cold-shortness of material; The TZM molybdenum alloy that has prepared excellent property.
Description of drawings
Fig. 1 is for adopting method of the present invention, the stereoscan photograph of alloy behind the sintering;
The metallograph of Fig. 2 after for 1550 ℃ of annealing of alloy of adopting method preparation of the present invention;
Fig. 3 processes back 1150 ℃ of metallographs behind 1 hour stress-removal for the alloy forging that adopts method preparation of the present invention.
Embodiment
A kind of method of preparing molybdenum alloy TZM by powder metallurgy selects for use Fisher particle size at 5～10 μ m, and largest particle is not more than titanium hydride and the zircoium hydride particle of 10 μ m, adopts powder metallurgy method to prepare the TZM molybdenum alloy.Its preparation process comprises following process successively: (1) adds titanium hydride, zircoium hydride and carbon black in molybdenum powder, make its shared part by weight in alloy be: 0.4%～0.55% titanium hydride, 0.06%～0.12% zircoium hydride, 0.01%～0.04% carbon black; Adopt ball milling or V-type machine batch mixing that molybdenum powder, titanium hydride, zircoium hydride and carbon black ground and mixed is even; Ball material weight ratio is 2～0.5: 1, mixing time 1～24 hour.(2) material after the method ground and mixed of static pressure such as employing or mold pressing is 1.80～3t/cm at pressure
2Under the condition, pressurize was pressed into blank in 0.5～2 minute; (3) adopt vacuum or hydrogen shield atmosphere sintering compacting blank, sintering temperature is 1800～2000 ℃, soaking time 2～8 hours; (4) adopt known method forgings, rolling TZM molybdenum alloy bar material, sheet material and foil, cogging temperature is controlled to be 1400～1600 ℃, and amount of finish is to carry out the stress-removal processing at 50～95% o'clock.
Embodiment 1
10 kilograms of molybdenum powders, titanium hydride 50 grams, zircoium hydride 10 grams, carbon black 6 grams.In the V-type mixer, mix ratio of grinding media to material 0.2: 1, mixing time 24 hours.Select the gum cover of diameter 90mm for use, charging, isostatic pressing, pressure 2.2t/cm
2, 2 minutes dwell times.In vacuum induction furnace, carry out sintering, 1900 ℃ of sintering temperatures, soaking time 4 hours.The density of material is 9.5g/cm behind the sintering
3, metallographic as shown in Figure 1.The carbon content of material is 0.01% behind the sintering, and oxygen level is 0.02%, and titanium content is 0.45%, and zirconium content is 0.06%.
Embodiment 2
10 kilograms of molybdenum powders, titanium hydride 50 grams, zircoium hydride 10 grams, carbon black 6 grams.In ball mill, mix ratio of grinding media to material 1: 1, mixing time 4 hours.Select the gum cover of diameter 90mm for use, charging, isostatic pressing, pressure 2.2t/cm
2, 2 minutes dwell times.In vacuum induction furnace, carry out sintering, 1900 ℃ of sintering temperatures, soaking time 4 hours.The chemical ingredients conformance with standard ASTM387-90 of material behind the sintering, density 9.5g/cm
3Adopting common process is slab with bar forging, about slab thickness 25mm.Adopt that known technology is rolling, annealing and corresponding alkali cleaning handle sheet material, is about 2.4mm up to the thickness of sheet material.Test result shows: the recrystallization temperature of this material is greater than 1550 ℃, and the stereoscan photograph behind this annealing temperature is moulded crisp transition temperature and is lower than normal temperature as shown in Figure 2.Its pyritous mechanical property is shown in Table 1.
Table 1 high-temperature mechanical property
| Annealing temperature (℃) | 1000 | 1200 | 1400 | 1600 | 1800 |
| Yield strength (MPa) | 407 | 117 | 50 | 38 | |
| Tensile strength (MPa) | 470 | 328 | 148 | 69 | 51 |
| Unit elongation (%) | 9.1 | ＞20 | ＞17 | ＞15 | ＞28 |
Embodiment 3
80 kilograms of molybdenum powders, titanium hydride 400 grams, zircoium hydride 80 grams, carbon black 48 grams.In ball mill, mix ratio of grinding media to material 1: 1, mixing time 1 hour.Select the gum cover of diameter 220mm for use, charging, isostatic pressing, pressure 2.2t/cm
2, 2 minutes dwell times.In vacuum induction furnace, carry out sintering, 1900 ℃ of sintering temperatures, soaking time 6 hours.The chemical ingredients conformance with standard ASTM387-90 of material behind the sintering, density 9.5g/cm
3Adopting common process is 80mm with bar forging to diameter.1150 ℃ of 1 hour its yield strengths of annealing back are 785MPa, tensile strength 852MPa, unit elongation 28%.Corresponding metallograph as shown in Figure 3.
Claims (2)
1. the method for a preparing molybdenum alloy TZM by powder metallurgy is characterized in that it being to select for use Fisher particle size at 5～10 μ m, and largest particle is not more than titanium hydride and the zircoium hydride particle of 10 μ m, adopts powder metallurgy method to prepare the TZM molybdenum alloy.
2. the method for a kind of preparing molybdenum alloy TZM by powder metallurgy according to claim 1 is characterized in that its preparation process comprises following process successively:
(1) in molybdenum powder, adds titanium hydride, zircoium hydride and carbon black, make its shared part by weight in alloy be: 0.4%～0.55% titanium hydride, 0.06%～0.12% zircoium hydride, 0.01%～0.04% carbon black; Adopt ball milling or V-type machine batch mixing that molybdenum powder, titanium hydride, zircoium hydride and carbon black ground and mixed is even; Ball material weight ratio is 2～0.5: 1, mixing time 1～24 hour;
(2) material after the method ground and mixed of static pressure such as employing or mold pressing is 1.80～3t/cm at pressure
2Under the condition, pressurize was pressed into blank in 0.5～2 minute;
(3) adopt vacuum or hydrogen shield atmosphere sintering compacting blank, sintering temperature is 1800～2000 ℃, soaking time 2～8 hours;
(4) adopt known method forgings, rolling TZM molybdenum alloy bar material, sheet material and foil, cogging temperature is controlled to be 1400～1600 ℃, and amount of finish is to carry out the stress-removal processing at 50～95% o'clock.
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| CN102796929A (en) * | 2012-08-25 | 2012-11-28 | 安泰科技股份有限公司 | Manufacture method of molybdenum alloy for nuclear fusion device |
| CN103121104A (en) * | 2011-11-21 | 2013-05-29 | 高殿斌 | Production method used for vacuum crystallization furnace heat preservation assembly materials |
| CN102041404B (en) * | 2009-10-23 | 2013-09-18 | 西安格美金属材料有限公司 | Method for preparing low-oxygen titanium-zirconium-molybdenum (TZM) alloy and application |
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- 2006-12-15 CN CN 200610165736 patent/CN1962911A/en active Pending
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| CN103121104A (en) * | 2011-11-21 | 2013-05-29 | 高殿斌 | Production method used for vacuum crystallization furnace heat preservation assembly materials |
| CN102554242B (en) * | 2012-02-09 | 2013-12-11 | 西安宝德粉末冶金有限责任公司 | Method for manufacturing micro-fine spherical titanium powder |
| CN102554242A (en) * | 2012-02-09 | 2012-07-11 | 西安宝德粉末冶金有限责任公司 | Method for manufacturing micro-fine spherical titanium powder |
| CN102796929B (en) * | 2012-08-25 | 2014-06-25 | 安泰科技股份有限公司 | Manufacture method of molybdenum alloy for nuclear fusion device |
| CN102796929A (en) * | 2012-08-25 | 2012-11-28 | 安泰科技股份有限公司 | Manufacture method of molybdenum alloy for nuclear fusion device |
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