CN102041404B - Method for preparing low-oxygen titanium-zirconium-molybdenum (TZM) alloy and application - Google Patents
Method for preparing low-oxygen titanium-zirconium-molybdenum (TZM) alloy and application Download PDFInfo
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- CN102041404B CN102041404B CN 200910308745 CN200910308745A CN102041404B CN 102041404 B CN102041404 B CN 102041404B CN 200910308745 CN200910308745 CN 200910308745 CN 200910308745 A CN200910308745 A CN 200910308745A CN 102041404 B CN102041404 B CN 102041404B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 52
- 239000000956 alloy Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000001301 oxygen Substances 0.000 title abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 title abstract description 22
- CPTCUNLUKFTXKF-UHFFFAOYSA-N [Ti].[Zr].[Mo] Chemical compound [Ti].[Zr].[Mo] CPTCUNLUKFTXKF-UHFFFAOYSA-N 0.000 title abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000007493 shaping process Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 206010021143 Hypoxia Diseases 0.000 claims description 23
- 208000018875 hypoxemia Diseases 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 150000004678 hydrides Chemical class 0.000 claims description 11
- -1 titanium hydride Chemical compound 0.000 claims description 11
- 229910000048 titanium hydride Inorganic materials 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 18
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052719 titanium Inorganic materials 0.000 abstract description 7
- 239000010936 titanium Substances 0.000 abstract description 7
- 238000005242 forging Methods 0.000 abstract description 4
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 235000019241 carbon black Nutrition 0.000 description 5
- 238000005728 strengthening Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- 239000005417 food ingredient Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Abstract
The invention provides a method for preparing a low-oxygen titanium-zirconium-molybdenum (TZM) alloy, which comprises the following steps of: 1) selecting raw materials, namely, uniformly mixing industrial molybdenum powder with the Fisher particle size of 4 to 50 mu m, powder containing titanium and zirconium and with the Fisher particle size of 3 to 10 mu m, and simple substance carbon powder with the Fisher particle size of 0.1 to 3 mu m according to a certain mass ratio; 2) shaping the raw materials, namely, treating the mixed raw materials under the pressure of 100 to 300 Mpa to obtain a shaped blank; and 3) sintering the raw materials, namely, sintering the shaped blank in the environment of vacuum, hydrogen or inert gas at the temperature of 1,800 to 2,300 DEG C for 5 to 15h to obtain the low-oxygen TZM alloy. The method solves the problem of high oxygen content of the TZM alloy prepared by a powder metallurgy method. The low-oxygen TZM alloy prepared by the method can be used for the preparation of a rotating anode of an X-ray tube, a composite target substrate, a high-temperature crucible, a hot-forging die and a high-temperature ceramic pad.
Description
Technical field
The present invention relates to method and hypoxemia TZM Alloyapplication thereof that a kind of powder metallurgy process prepares hypoxemia TZM alloy, adopt the TZM alloy of the method preparation, oxygen level can be low to moderate below the 20ppm, and optimum can reach 1ppm.
Background technology
TZM alloy (Titanium-Zirconium-Molybdenum Alloy) is a kind of superalloy commonly used in the molybdenum base alloy, also is a kind of important superalloy in the present commercial use.Because the TZM alloy has good high-temperature behavior, thereby is used widely in the industries such as medicine equipment, aerospace, electronic industry and glass-ceramic production.
Studies show that in a large number, the plastic brittle transition temperature of TZM alloy, recrystallization temperature, toughness are all relevant with oxygen level.Oxygen in the TZM alloy easily is combined with strengthening element titanium, zirconium, and the oxide particle of titanium, zirconium is larger, is difficult to disperse even, and strengthening effect is poor, and easily forms formation of crack.When oxygen level is high in the TZM alloy, alloy plasticity-brittle transition temperature is raise, recrystallization temperature reduces, and directly causes the alloy toughness drop, and workability is poor, has a strong impact on alloy property.Oxygen level is higher in the TZM alloy, and alloy property is poorer, otherwise alloy property is just better, and therefore, oxygen is the impurity element that will strictly control.
The main method of producing above-mentioned alloy has two kinds: smelting process and powder metallurgic method.
Smelting process is that pure molybdenum and a certain amount of titanium, zirconium, carbon are carried out the method that melting obtains the TZM alloy under vacuum.Smelting process can make in the TZM alloy oxygen level drop to 30ppm even below the 20ppm.But the above-mentioned alloy grain that smelting process is produced is thick, complex process, and yield rate is low, and cost is high.
Powder metallurgic method is evenly to mix by a certain percentage the method that obtains the TZM alloy by static pressure shaping, sintering, rolling (forging), annealing with molybdenum powder and titanium, zirconium powder end or titanium hydride, zircoium hydride powder and carbon black powder.The TZM alloy grain that powder metallurgic method is produced is tiny, and operation and equipment are simple, and is with short production cycle, and yield rate is high.But powder metallurgy technology in the past is difficult to reduce the oxygen level in the TZM alloy, and the TZM alloy oxygen level of powder metallurgic method production is all more than 200ppm usually.
Summary of the invention
The invention provides a kind of preparation method and application thereof of hypoxemia TZM alloy, mainly solved the high problem of TZM alloy oxygen level that the method system of applied powder metallurgy is produced.
Technical solution of the present invention is as follows:
The preparation method of this hypoxemia TZM alloy may further comprise the steps:
1) raw material is chosen
Choosing Fisher particle size is the industrial molybdenum powder of 4 μ m～50 μ m, the mixture of the ti powder of Fisher particle size 3 μ m～10 μ m and zirconium powder end or titanium hydride and zircoium hydride powder or ti powder, zirconium powder end and titanium hydride, zircoium hydride powder, and Fisher particle size is the carbon simple substance powder of 0.1 μ m～3 μ m.Theoretically, the molybdenum powder powder Fisher particle size of choosing is larger, and the TZM alloy oxygen level that obtains is lower, but the Fisher particle size of powder is larger, and the powder process difficulty is larger, and the powder process cost is higher, and moulding is more difficult, and sintering temperature is high, and the time is long.Described mixing raw material is counted in mass ratio, contain mixture, 0.01%～0.15% carbon simple substance powder and 97.85%～99.89% industrial molybdenum powder that 0.1%～2.0% titanium, zirconium powder end, titanium hydride, zircoium hydride powder or titanium, zirconium powder end, powder and titanium hydride, zircoium hydride powder are mixed with arbitrary proportion.
2) material forming
To through step 1) raw material that mixes waits static pressure or mold pressing to obtain shaping blank, and the pressure size of choosing is relevant with the powder size size, usually chooses 100MPa～300MPa, preferably 220MPa～300MPa.
3) raw material sintering
In vacuum, hydrogen or inert gas environment, shaping blank is carried out sintering, sintering temperature is 1800 ℃～2300 ℃, and sintering time is relevant with size and the powder size of base to be sintered with sintering temperature, and powder size is larger, sintering temperature is higher, and sintering time is 5～15 hours usually.
Above-described carbon simple substance powder is that carbon black, graphite or carbon dust are arbitrary or arbitrarily multiplely mix with arbitrary proportion; When the powder Fisher particle size was excessive, tooling cost will significantly promote.The preferable range that the factors such as the cost that therefore, comprehensive powder process, moulding, sintering are required and material performance consider to draw the molybdenum powder granularity is 10 μ m～30 μ m.
Use the hypoxemia TZM alloy of aforesaid method preparation, be used for the preparation of X ray tube rotary anode target, composition target base target, high-temperature crucibles, hot forged mould and pyroceramic pad.
The invention has the advantages that:
1. the hypoxemia TZM alloy that utilizes the preparation method of hypoxemia TZM alloy provided by the invention to prepare, its oxygen level can be reduced to and be lower than 20ppm, oxygen level impurity is few in the alloy, prevented that the strengthening element hafnium from forming oxide compound, and the disperse that causes because oxide particle is thick is inhomogeneous, the defective such as easily cracks.
2. particle is tiny after utilizing the preparation method of hypoxemia TZM alloy provided by the invention to prepare the strengthening element hafnium carburet of hypoxemia TZM alloy inside, and particle diameter is less than 1 μ m, and disperse is even, and strengthening effect is remarkable.
3. hypoxemia TZM alloy plasticity-brittle transition temperature of utilizing the preparation method of hypoxemia TZM alloy provided by the invention to prepare is low, and normal temperature toughness is strong, and workability is strong, and lumber recovery is high, and the simple cost of production technique is low.
4. the hypoxemia TZM alloy recrystallization temperature of utilizing the preparation method of hypoxemia TZM alloy provided by the invention to prepare is high, excellent property and stable under the high temperature.
Embodiment
1) gets the industrial molybdenum powder that Fisher particle size is respectively 4 μ m, 5 μ m, 7 μ m, 9 μ m, 11 μ m, 13 μ m, 15 μ m, 20 μ m, 30 μ m, 40 μ m, 50 μ m, Fisher particle size is the titanium hydride powders of 3 μ m～10 μ m, Fisher particle size is the zircoium hydride powder of 3 μ m～10 μ m, and Fisher particle size is 0.1 μ m～3 μ m carbon blacks.It is 0.50% that titanium hydride powders adds quality, and it is 0.10% that the zircoium hydride powder adds quality, and the interpolation quality of carbon black powder is 0.12%, and all the other are molybdenum powder.Molybdenum powder after choosing, titanium hydride, zircoium hydride powder and carbon black powder are mixed.
2) material forming
To through step 1) raw material that mixes carries out hydrostatic profile and obtains blank under 200MPa pressure, and billet size is Φ 120mm * 130mm.
3) raw material sintering
In hydrogen shield atmosphere shaping blank is carried out sintering, sintering temperature is as shown in the table, and the billet size behind the sintering is Φ 100mm * 120mm.
4) blank behind the sintering is forged, sample size is Φ 230mm * 18mm after forging.
Composition and performance to sample are tested, and test for tensile strength carries out under 1000 ℃.Testing data such as following table:
| The sample sequence number | The molybdenum powder granularity | Food ingredient (mass ratio)/% | The highest sintering temperature/℃ | Carbon content/ppm | Oxygen level/ppm | Tensile strength/MPa | Hardness 2/HV |
| 1 | 4 | 0.50Ti-0.10Zr-0.12C | 2100 | 320 | 180 | 407 | 280 |
| 2 | 5 | 0.50Ti-0.10Zr-0.12C | 2120 | 350 | 54 | 420 | 285 |
| 3 | 7 | 0.50Ti-0.10Zr-0.12C | 2130 | 350 | 18 | 437 | 290 |
| 4 | 9 | 0.50Ti-0.10Zr-0.12C | 2150 | 380 | 15 | 442 | 290 |
| 5 | 11 | 0.50Ti-0.10Zr-0.12C | 2170 | 400 | 13 | 445 | 295 |
| 6 | 13 | 0.50Ti-0.10Zr-0.12C | 2180 | 390 | 10 | 440 | 295 |
| 7 | 15 | 0.50Ti-0.10Zr-0.12C | 2180 | 390 | 9 | 458 | 295 |
| 8 | 20 | 0.50Ti-0.10Zr-0.12C | 2190 | 400 | 7 | 454 | 300 |
| 9 | 30 | 0.50Ti-0.10Zr-0.12C | 2210 | 400 | 6 | 452 | 300 |
| 10 | 40 | 0.50Ti-0.10Zr-0.12C | 2250 | 400 | 5 | 459 | 300 |
| 11 | 50 | 0.50Ti-0.10Zr-0.12C | 2300 | 400 | 4 | 455 | 300 |
Annotate 2: the hardness value of sample is for forging rear 1350 ℃ of hardness that annealing recorded under the room temperature after 1 hour
Use the hypoxemia TZM alloy that preparation method provided by the invention prepares, can be for the bar that uses under processing X ray tube rotary anode target, compound x-ray target base material, high-temperature resistant container, hot forged mould, sintering high temperature ceramic backing and the hot conditions, sheet material, shaped piece etc.
Wherein, the X ray tube rotary anode target is mainly used in the non-destructive testing apparatus such as medical CT examination device, luggage and articles inspection and metal, equipment flaw detection etc.For make inspection units can high output, high-definition, rotating anode target is just gradually to large scale development, general diameter even reaches about 260mm more than 100mm.
The hypoxemia TZM alloy oxygen level that the method for preparing hypoxemia TZM alloy provided by the invention is prepared can reach below the 20ppm, therefore discharge quantity is extremely low, and the lower limit indefinite of TZM alloy oxygen level, under the lower hot conditions of oxygen level in the use procedure gas emit fewer, high-temperature behavior is better, can satisfy the working conditions of the high temperature purposes members such as X ray tube rotary anode target, high-temperature crucibles, hot forged mould and sintering high temperature ceramic backing.
Claims (5)
1. the preparation method of a hypoxemia TZM alloy is characterized in that, may further comprise the steps:
1) raw material is chosen
Choosing Fisher particle size is the industrial molybdenum powder of 5～50 μ m, and Fisher particle size is that the titanium hydride powders of 3 μ m～10 μ m mixes with the zircoium hydride powder, and Fisher particle size is the carbon simple substance powder of 0.1～3 μ m;
Described industrial molybdenum powder, titanium hydride powders, zircoium hydride powder and carbon simple substance powder mix the formation mixing raw material;
With described mixing raw material by mass, contain titanium hydride powders and the zircoium hydride powder of 0.1～2.0%wt, 0.01～0.15% carbon simple substance powder, surplus is 97.85%～99.89% molybdenum powder;
2) material forming
Wait static pressure or mold pressing to process mixing raw material, obtain shaping blank; The described pressure that waits static pressure or mold pressing processing to choose is 100MPa～300MPa;
3) raw material sintering
In vacuum, hydrogen or inert gas environment shaping blank is carried out sintering, sintering temperature is 2100 ℃～2300 ℃, and sintering time is 5～15 hours, obtains hypoxemia TZM alloy after sintering is finished.
2. the preparation method of described hypoxemia TZM alloy according to claim 1 is characterized in that: described carbon simple substance powder is that carbon black, graphite or carbon dust are arbitrary or multiplely arbitrarily mix with arbitrary proportion.
3. the preparation method of described hypoxemia TZM alloy according to claim 1 and 2, it is characterized in that: the Fisher particle size of described industrial molybdenum powder is 10 μ m ~ 30 μ m.
4. the preparation method of described hypoxemia TZM alloy according to claim 3, it is characterized in that: the pressure that described static pressure or mold pressing are processed is 220MPa ~ 300 MPa.
5. the hypoxemia TZM alloy that right to use requires 1-4 arbitrary described methods to prepare is used for the preparation of X ray tube rotary anode target, composition target base target, high-temperature crucibles, hot forged mould and pyroceramic pad.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102699327B (en) * | 2012-01-04 | 2015-03-25 | 洛阳科威钨钼有限公司 | Process for manufacturing molybdenum crucibles |
| CN103060760A (en) * | 2012-11-28 | 2013-04-24 | 厦门虹鹭钨钼工业有限公司 | Preparation method for molybdenum-titanium alloy target |
| CN103320634B (en) * | 2013-06-08 | 2015-07-29 | 金堆城钼业股份有限公司 | A kind of preparation method of TZM alloy material |
| CN103276266B (en) * | 2013-06-08 | 2015-07-29 | 金堆城钼业股份有限公司 | A kind of spraying dry prepares the method for TZM alloy material |
| CN103421969B (en) * | 2013-09-06 | 2015-04-15 | 金堆城钼业股份有限公司 | Preparation method of molybdenum alloys for isothermal forging die |
| CN105234389A (en) * | 2015-10-09 | 2016-01-13 | 西安思源学院 | Method for preparing titanium-zirconium-molybdenum (TZM) alloy by mixing superfine powder through ultrasonic waves |
| CN105618768B (en) * | 2015-12-28 | 2018-09-25 | 安泰天龙（天津）钨钼科技有限公司 | A kind of preparation method of high-compactness pure tungsten, pure molybdenum and its alloy material |
| CN106531599B (en) * | 2016-10-28 | 2018-04-17 | 安泰天龙钨钼科技有限公司 | A kind of X-ray tube W-Re molybdenum alloy rotary anode target and preparation method thereof |
| CN109763047A (en) * | 2019-01-28 | 2019-05-17 | 合肥工业大学 | A kind of Mo-Ti-Zr-CNT molybdenum alloy composite material and preparation method of high intensity |
| CN114523100B (en) * | 2022-03-08 | 2022-10-28 | 西北有色金属研究院 | High-pressure reduction preparation method of molybdenum-hafnium-carbon alloy powder containing hafnium hydride |
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