CN107760897A - To hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts - Google Patents
To hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts Download PDFInfo
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- CN107760897A CN107760897A CN201711030580.9A CN201711030580A CN107760897A CN 107760897 A CN107760897 A CN 107760897A CN 201711030580 A CN201711030580 A CN 201711030580A CN 107760897 A CN107760897 A CN 107760897A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 91
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 80
- 239000010936 titanium Substances 0.000 title claims abstract description 47
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 39
- 239000002994 raw material Substances 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 111
- 230000008569 process Effects 0.000 claims abstract description 58
- 239000000956 alloy Substances 0.000 claims abstract description 51
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 47
- 239000012298 atmosphere Substances 0.000 claims abstract description 37
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000001301 oxygen Substances 0.000 claims abstract description 28
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 28
- 239000011812 mixed powder Substances 0.000 claims abstract description 27
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 26
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 21
- -1 titanium hydride Chemical compound 0.000 claims abstract description 20
- 238000007493 shaping process Methods 0.000 claims abstract description 19
- 238000007596 consolidation process Methods 0.000 claims abstract description 16
- 230000001360 synchronised effect Effects 0.000 claims abstract description 15
- 230000000930 thermomechanical effect Effects 0.000 claims abstract description 13
- 238000005275 alloying Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
- 238000005242 forging Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001125 extrusion Methods 0.000 claims description 9
- 238000011282 treatment Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000000280 densification Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000003856 thermoforming Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- 238000003795 desorption Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004663 powder metallurgy Methods 0.000 abstract description 12
- 238000000605 extraction Methods 0.000 abstract description 6
- 235000013312 flour Nutrition 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 28
- 238000012545 processing Methods 0.000 description 18
- 229910052786 argon Inorganic materials 0.000 description 14
- 239000007789 gas Substances 0.000 description 14
- 150000004678 hydrides Chemical class 0.000 description 10
- 230000007246 mechanism Effects 0.000 description 9
- 241001417495 Serranidae Species 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 230000032683 aging Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000005266 casting Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 238000002161 passivation Methods 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 238000005272 metallurgy Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000010334 sieve classification Methods 0.000 description 2
- 229910001040 Beta-titanium Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 150000002821 niobium Chemical class 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical class [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the preparation of titanium and titanium alloy and shape technical field, and in particular to a kind of to hydrogenate titanium sponge as raw material manufacture powder metallurgy titanium and the method for titanium alloy and its parts, its technological process：Titanium sponge hydrogenation → synchronous ball powder-grinding titanium hydride powders either vacuum dehydrogenation → alloy product of mixed-powder → powder compact → Fast Sintering and synchronous dehydrogenation → thermomechanical consolidation or shaping → thoroughly.This method realizes that the synchronous ball mill of hydrogenation titanium sponge and alloyed feedstock prepares mixed-powder, and powder need not sieve, and flour extraction is more than 96%；The pressed compact of powder is completed under inert atmosphere protection, quickly heats alloying, thermomechanical consolidation and shaping.The technological process of the present invention is short, efficiency high, it is possible to produce the titanium and titanium alloy product of high-compactness (>=99.8%) and low oxygen content (≤0.26%)；The Main Mechanical of alloy is higher than the level of common variation titanium alloy, and cost is significantly lower than conventional powder metallurgy titanium alloy.
Description
Technical field
The invention belongs to the preparation of titanium and titanium alloy and shape technical field, and in particular to a kind of to hydrogenate titanium sponge
The method that powder metallurgy titanium and titanium alloy and its parts are manufactured for raw material.
Background technology
Titanium alloy has highest specific strength in low-density, structural metallic materials, excellent corrosion-resistant and heat resistance, nothing
Outstanding advantages of magnetic, in Aero-Space, weaponry lightweight, petrochemical industry, ocean engineering and naval vessel industry, automobile system
Make, the field such as bio-medical and Leisure Sport shows very tempting wide application prospect, be a kind of extremely important knot
Structure material and strategic material.However, because titanium alloy high-temperature activity is big, resistance of deformation is high and processing characteristics is poor, make titanium alloy
Condition is harsh in terms of preparation, processing and shaping, ultimately causes the high cost of titanium alloy parts.Currently, high cost has been
As the biggest obstacle of titanium alloy large-scale industrial application.
Ingot metallurgy method and powder metallurgic method are the two big main stream approach that prepared by titanium alloy and parts manufacture.Ingot metallurgy
Method melts out titanium alloy casting by the methods of vacuum consumable electrode arc furnace, vacuum induction melting furnace or electron-beam cold bed furnace first
Ingot, ingot casting is then subjected to the secondary operation such as cogging forging and forging, extruding, rolling or shaping obtains titanium or part blank,
The processing such as finally it is heat-treated, welded and machined and obtains required titanium alloy parts.It is obvious that ingot metallurgy method manufactures
Titanium alloy material and parts, technological process length, complex process, equipment investment is big, energy consumption is big, stock utilization is very low, and this is straight
Connecing causes the cost of titanium alloy too high.Currently, in low-cost titanium alloy design, short route manufacture (such as：Graphite mould or ceramic mould essence
Close casting), the electronic beam cold hearth production cost degradation manufacture view such as titanium ingot and titanium material recycling obtain it is significant
Progress, but still it is not enough to fundamentally solve the too high obstacle brought to its scale application of titanium alloy cost.
Powder metallurgic method is to realize the breach of titanium alloy cost degradation manufacture.Current low-cost titanium alloy powder metallurgy skill
The raw material that art uses are mainly the pure titanium powder of hydrogenation and dehydrogenization, also have a small amount of research institution directly to use titanium hydride powders.This
By the titanium valve of hydrogenation and dehydrogenization, either hydride powder and alloying element powder carry out mechanical ball mill to kind technology or mechanical mixture is uniform
Change, powder mix is then carried out pressed compact or near-net-shape pressed compact, eventually through vacuum/protective atmosphere sintering or hot pressing
Sintering completes alloying and the densification of titanium.This conventional titanium alloy powder metallurgical technology, although titanium conjunction can be reduced substantially
The cost of golden material and parts manufacture, but still following typical deficiency be present：
1. cost is still higher.Such as：The hydrogenation dehydrogenation titanium powder or hydride powder price of -200 mesh just 200 yuan/kg with
On, high temperature sintering time length (2~6 hours), energy consumption is big；
2. oxygen content is higher, generally in 0.40%~0.60% (mass ratio, similarly hereinafter).It is primarily due to the hydride powder used
End, the raw material of titanium powder and alloying powder, generally by Passivation Treatment, the oxygen on particle top layer is molten during high-temperature alloy
Solution enters inside alloy；
3. consistency is not high enough to (≤98%).The pressure of sintering is low, it is impossible to passes through enough thermoplastic deformation eliminations
Hole inside the space of intergranular and alloy.If improving consistency by high temperature forging or high temperature insostatic pressing (HIP), cost can be caused to show again
Write and improve；
4. crystal particle scale is thicker, average colony size is generally higher than 100 μm.Because initial powder still relatively thick (- 200
Mesh or -300 mesh), and high temperature sintering temperature is high (1300~1400 DEG C), sintering time is longer (2~6 hours)；
5. although powder metallurgy titanium alloy tensile strength and hardness number are significantly improved, because oxygen content is high and fine and close
Spend low, cause room temperature elongation percentage universal relatively low (powder metallurgy TC4 elongation percentage≤9%), far below the forging titanium alloy of routine；
6. the production cycle is still longer.It is mainly reflected in powder sieving and two links of mixed powder and vacuum-sintering.
The content of the invention
It is an object of the invention to provide one kind titanium and titanium alloy material and synchronous are prepared to hydrogenate titanium sponge as raw material
The method for manufacturing parts, specific aim solve current powder metallurgy titanium alloy oxygen content is high, consistency is relatively low, room temperature elongation percentage
Deficiency, the problem of crystal grain is thicker, the production cycle is long and cost is still too high etc., realize inexpensive low oxygen content powder
The quick preparation and shaping of metallurgical titanium and titanium alloy.
The technical scheme is that：
A kind of method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, includes following process：
1. the hydrogenation of titanium sponge；2. synchronous ball mill prepares titanium hydride powders or mixed-powder；3. powder compact；4. Fast Sintering is simultaneously same
Walk partial；5. thermomechanical consolidation or shaping；6. thorough vacuum dehydrogenation；7. alloy product.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 1. middle sponge
The hydrogenation treatment of titanium, be in hydrogenation furnace, under conditions of 350~750 DEG C of temperature and 0.9~1.5atm Hydrogen Vapor Pressures, keep 1~
Complete within 6 hours.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 2. in it is same
Step ball milling prepares titanium hydride powders or mixed-powder, refer to will hydrogenation titanium sponge or hydrogenation titanium sponge and alloyed feedstock by
It is fitted into together in ball grinder according to stoichiometric proportion, synchronizes ball mill grinding and well mixedization；The alloying raw material of addition,
It is pure element powder, breakable master alloy particle or powder, or hydride particle or powder.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 2. in it is same
Step ball milling prepares titanium hydride powders or mixed-powder, is carried out under inert atmosphere protection, ball mill uses planetary ball
Grinding machine, stirring ball mill or tumbling ball mill；The mixed-powder of titanium hydride powders made from ball milling or alloy, is not required to
Carry out screening process.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 3. in powder
Last pressed compact, it is under inert atmosphere protection, takes the mixed-powder of 2. titanium hydride powders that process is prepared or alloy to load mould
In, complete compacting within 1~60 minute in the pressurize of 300~1500MPa pressure.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 4. middle powder
The Fast Sintering of pressed compact and sync section dehydrogenation, be under inert gas shielding, by sensing heating, plasma discharging heating or
Heated in person's direct current, be warming up to 1000~1350 DEG C with 30~200 DEG C/min speed and be incubated what is completed within 0~60 minute；It hurry up
Fast sintering process realizes the dehydrogenation of part, and hydrogen content is reduced to 0.6~1.2% in agglomerate.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 5. in heat
Machinery consolidation or shaping, completed on the hydraulic press of closed work box for being equipped with adjustable atmosphere, by process 4. in it is complete
Powder compact into high temperature sintering and insulation is directly quickly transferred in extrusion die or forging mold, by extruding or forging
Affected completion sufficiently densification and thermoforming.
2. described arrives process to hydrogenate titanium sponge as raw material manufacture titanium and the method for titanium alloy and its parts, process
Powder ball milling, powder compact, Fast Sintering, thermomechanical consolidation or the shaping being related to during 5., are controlled in inert atmosphere
Oxygen content in 0~200ppm.
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 6. in it is true
Empty dehydrogenation, desorption temperature are controlled at 400~850 DEG C, and vacuum is maintained at 1.0 × 10-2~1.0 × 10-4Pa, dehydrogenation time 4~
10h。
The described method for manufacturing titanium and titanium alloy and its parts to hydrogenate titanium sponge as raw material, process 7. in conjunction
Golden product, it is the extruding long profiles of bar, tubing or slab, either according to difference when densification and shaping using mould
The parts of forging molding, types of alloys cover pure titanium or the titanium alloy of any condition.
Advantages of the present invention and beneficial effect are：
The present invention to hydrogenate titanium sponge as raw material, by synchronization mechanism ball milling quickly prepare titantium hydride or titantium hydride with
The mixed-powder of alloy element, cost be market purchasing titantium hydride or hydrogenation dehydrogenation titanium powder end price 40%.Also,
Milling efficiency, flour extraction and the powder properties of the present invention are all very high.Powder preparation, pressed compact, sintering and thermomechanical consolidation are fine and close
Change or be molded, carried out under inert atmosphere protection, be advantageous to control the oxygen content of alloy.Average powder size is only
Be about 4 μm, powder compact using be rapidly heated means sintering, and with reference to thermomechanical consolidation means be directly densified and into
Type, this can significantly improve the consistency and metallurgical quality of alloy product, improve production efficiency, realize that short route manufactures.It is overall next
Say, the present invention can produce oxygen mass content within more than 99.8% consistency, 0.25%, Main Mechanical index is higher than
Forge titanium alloy, cost is less than the high-quality powder metallurgy titanium alloy material and its parts of common alloy of titanium casting.
Brief description of the drawings
Fig. 1 is the distribution diagram of element of hydrogenation titanium sponge and AlV40 intermediate alloy synchronization mechanisms ball milling after 2 hours；Wherein,
(a) Ti elements；(b) Al elements；(c) V element.
Fig. 2 is the As-extruded tissue of powder metallurgy TC4 titanium alloy extruded barses.
Fig. 3 is the solid solution aging state tissue of powder metallurgy TC4 titanium alloy extruded barses.
Fig. 4 is hydrogenation titanium sponge and the distribution diagram of element of pure aluminium powder and electrolytic iron powder synchronization mechanism ball milling after 2 hours；Its
In, (a) Fe elements；(b) Al elements.
Fig. 5 is the process chart of the present invention.
Embodiment
As shown in figure 5, it is of the invention to hydrogenate technology of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, its
Technological process is as follows：The hydrogenation of titanium sponge → synchronization mechanism ball milling is prepared under titanium hydride powders or mixed-powder → inert atmosphere
It is thermomechanical under Fast Sintering and sync section dehydrogenation → inert atmosphere under powder compact or near-net-shape base → inert atmosphere
Consolidation or shaping → thorough vacuum dehydrogenation → alloy product.Wherein：
1. the hydrogenation of titanium sponge：In hydrogenation furnace, by titanium sponge in 350~750 DEG C of temperature and 0.9~1.5atm hydrogen pressures
Under conditions of power, kept for 1~8 hour, prepare hydrogenation titanium sponge；
2. synchronization mechanism ball milling prepares titanium hydride powders or mixed-powder：Under inert atmosphere protection, sponge will be hydrogenated
Titanium or hydrogenation titanium sponge are fitted into the ball grinder of ball mill together with alloying raw material, it is synchronous carry out mechanical ball mill it is broken and
Powder well mixedization.The alloying raw material of addition, can be pure element powder, breakable master alloy particle or powder
End or hydride particle or powder；Ball mill used can be planetary ball mill, stirring ball mill or rolling
Ball tube mill etc.；
Due to hydrogenating the fragility of titanium sponge, it is easy to which ball mill crushing is simultaneously synchronously quickly well mixed with alloyed feedstock.
Grain crushes and need not use any process control agent in powder mixed process, and cold welding will not occur for powder.This causes powder processed
Efficiency and flour extraction significantly improve, and powder granule size is thinner, and ensure the degree of purity of powder；
3. powder compact：Under inert atmosphere protection, the mixing of titanium hydride powders or alloy prepared by mechanical ball mill
Powder, it is fitted into the mould of given shape, the pressurize completion in 0~1.0 hour under 300~1500MPa pressure.
Wherein, it the titanium hydride powders of step 2. mechanical ball mill, can be used directly without screening process, and powder can be controlled
End goes out during powder, encapsulation, transfer and pressed compact after ball milling, all the time under inert atmosphere protection, can be not subjected at passivation
Reason.The mixed-powder of step 2. mechanical ball mill, reused after being passivated processing if desired, then specific passivation technology is：
In the argon gas atmosphere case of 500ppm oxygen contents, holding atmosphere pressures are 0.9-1.05atm, are passivated 60 minutes.In passivating process, often
Powder is stirred once every 10 minutes, ensures that the surface of powder particle is all passivated.
4. the Fast Sintering of powder compact and sync section dehydrogenation：Under inert atmosphere protection, by sensing heating, electric discharge
One kind in heating plasma and direct current in the general quick mode of heating such as heating, is heated up with 30~200 DEG C/min speed
To 1000~1350 DEG C and it is incubated what is completed within 0~60 minute；In sintering process powder base hydrogen mass content be reduced to 0.6~
1.5%；
5. thermomechanical consolidation or shaping：Be on the hydraulic press of exercisable closed atmosphere case is equipped with, by process 4. in
The powder compact of soak is completed, is directly quickly transferred in extrusion die or forging mold, by extruding or forging
Effect synchronously completes densification and thermoforming.The whole process of process 4. and 5. all keeps the oxygen of inert atmosphere in closed atmosphere case
Content is less than 200ppm；
6. vacuum dehydrogenation：By step, 5. the alloy material of middle manufacture or parts carry out thorough dehydrogenation, ensure in alloy
Hydrogen mass content is less than 0.01%.Certain embodiments are at 400~850 DEG C and 1.0 × 10-2~1.0 × 10-4Protected under Pa vacuums
Hold 4~10h completions；
7. alloy product：Types of alloys covers pure titanium and the titanium alloy of any condition；According to powder compact and powder consolidation
Or using the difference of mould during shaping, alloy product can be the extrudate of the certain cross sections such as bar, tubing and slab,
Can be the parts of forging molding.
Below, the present invention is further elaborated on by embodiment.
Embodiment 1
The concrete technology flow process of the present embodiment is：
1. the hydrogenation of titanium sponge：In hydrogenation furnace, by titanium sponge of the particle size less than 30mm 450 DEG C and 1.0~
Under conditions of 1.2atm Hydrogen Vapor Pressures, kept for 2 hours, prepare hydrogenation titanium sponge (the content 4.3wt.% of hydrogen)；
2. synchronization mechanism ball milling prepares titanium hydride powders：Under argon gas protection, hydrogenation titanium sponge raw material are loaded into planet
In the ball grinder of formula ball mill or stirring ball mill, the synchronous mechanical ball mill that carries out crushes and prepares titanium hydride powders.Its
In, ball material mass ratio is 2.5:Under the conditions of 1 and drum's speed of rotation 300rpm, ball milling 30min can prepare particle size and be less than
25 μm of titanium hydride powders, ball milling 1h can prepare the titanium hydride powders that particle size is less than 15 μm, and average particle size particle size
Less than 4 μm；Sieve classification processing is not needed, powder flour extraction is up to 97%.
3. powder compact：Under argon gas protection, by the titanium hydride powders of mechanical ball mill preparation, the mould of loading φ 60mm internal diameters
In tool, pressurize 1min completes compacting under 950MPa hydraulic press pressures.Control powder is going out powder, encapsulation, transfer and pressed compact process
In, all the time under argon gas protection of the oxygen content less than 120ppm；
4. the Fast Sintering of powder compact and sync section dehydrogenation：It is less than 120ppm argon atmosphere case in oxygen content
In, by Frequency Induction Heating, it is warming up to 1000 DEG C with 100 DEG C/min speed and is incubated 1 minute；Powder pressure in sintering process
The content of hydrogen is reduced to 0.95wt.% in base；
5. thermomechanical consolidation or shaping：Be on the hydraulic press of exercisable closed atmosphere case is equipped with, by process 4. in
The powder compact of soak is completed, is directly quickly transferred in extrusion die cylinder, with 16:1 extrusion ratio extrusion, is completed fine and close
Change.Whole process all keeps the oxygen content of argon gas atmosphere in closed atmosphere case to be less than 120ppm；
6. vacuum dehydrogenation：By the titanium extruded rod of step 5. middle manufacture at 700 DEG C, 1.0 × 10-3~1.0 × 10-4Pa vacuum
Degree is lower to keep 6h, and the hydrogen for making to remain in pure titanium extruded rod is thoroughly discharged, and the content of final hydrogen is 0.085wt.%；
7. alloy product：By step 1.~6. process, produce the extruded rod of pure titanium；
The pure titanium extruded barses of powder metallurgy manufactured in the present embodiment, oxygen mass content is only 0.20%, and consistency is up to
99.8%, tensile strength 620MPa, elongation percentage reach 35%, and cost is close to the pure titanium ingot castings of TA1.
Embodiment 2
The concrete technology flow process of the present embodiment is：
1. the hydrogenation of titanium sponge：In hydrogenation furnace, by zero level titanium sponge in 450 DEG C and 1.0~1.2atm Hydrogen Vapor Pressures
Under the conditions of, 2h is kept, prepares hydrogenation titanium sponge (the content 4.3wt.% of hydrogen)；
2. synchronization mechanism ball milling prepares the mixed-powder of alloy：, will according to the quality proportioning of TC4 Titanium alloy Ti-6Al-4Vs
Hydrogenation titanium sponge and brittle AlV40 master alloy particles are fitted into the ball grinder of stirring ball mill together, are protected in argon gas
Lower synchronous mechanical ball mill crushes and being well mixed prepares titantium hydride and AlV40 mixed-powder.Wherein, ball material mass ratio is
2.4:1st, drum's speed of rotation 300rpm, ball milling 2h, the mixed-powder particle size prepared are less than 15 μm, and average particle size particle size is small
In 4 μm；Sieve classification processing is not needed, powder flour extraction is up to 98%.As shown in figure 1, TC4 titanium alloys prepared by this step
In mixed-powder raw material, AlV40 particle size is less than 1.0 μm, and is evenly distributed.
3. powder compact：The powder mix for taking mechanical ball mill to prepare, is fitted into the mould cylinder of φ 200mm internal diameters,
Pressurize 2min completes compacting under 950MPa hydraulic press pressures.Control powder after ball milling go out powder, encapsulation, transfer and pressed compact process
In, all the time under argon gas protection of the oxygen content less than 120ppm；
4. the Fast Sintering of powder compact and sync section dehydrogenation：In argon gas atmosphere case of the oxygen content less than 120ppm,
By Frequency Induction Heating, pressed compact is heated to 1200 DEG C with 100 DEG C/min speed and is incubated 2 minutes；Powder in sintering process
The content of hydrogen is reduced to 1.2wt.% in last blank；
5. thermomechanical consolidation or shaping：Be on the hydraulic press of exercisable closed atmosphere case is equipped with, by process 4. in
The powder batch of high temperature sintering is completed, is directly quickly transferred in extrusion die cylinder, with 16:1 extrusion ratio extrusion, is completed fine and close
Change, produce TC4 titanium alloy rod bars.Whole process all keeps the oxygen content of argon gas atmosphere in closed atmosphere case to be less than 120ppm；
6. vacuum dehydrogenation：By the TC4 titanium alloys extruded rod of step 5. middle manufacture at 700 DEG C, 1.0 × 10-3~1.0 × 10- 46h is kept under Pa vacuums, the hydrogen for making to remain in TC4 titanium alloy extruded rods is thoroughly discharged, and final hydrogen content is 90ppm；
7. alloy product：By step 1.~6. process, produce TC4 titanium alloy extruded rods；
TC4 titanium alloys extruded barses manufactured in the present embodiment, oxygen mass content are only 0.22%, and consistency is up to
99.8%；Alloy surveys composition：Ti-6.05Al-4.02V (wt%).+ 580 DEG C/6h/ is dissolved by 950 DEG C/30min/WQ
FC Ageing Treatments, the tensile strength of alloy is 1300MPa, and elongation percentage reaches 15%, and cost of alloy is about 180 yuan/kg.Such as Fig. 2
Shown, the TC4 titanium alloy extruded barses of the present embodiment manufacture, As-extruded is organized as Widmannstatten structure, even tissue, average colony
Size is about 15 μm；By fixation rates, structural transformation is typical basket tissue (see Fig. 3).
Embodiment 3
The difference of the present embodiment and embodiment 2 be processing step 3.~7..
Processing step 3. in powder compact, be the powder mix for taking mechanical ball mill to prepare, load engine link portion
In the mold cavity of part, pressurize 2min completes compacting under 950MPa hydraulic press pressures.Control the wheel of engine link powder base
Wide size is more than actual parts size about 12%.This is actual in view of causing pressed compact volume to receive due to putting hydrogen during sensing heating
Contraction 8% and the allowance of rear renewed treaty 4%.
The processing step 4. Fast Sintering of middle powder compact and sync section dehydrogenation：It is the argon for being less than 120ppm in oxygen content
Gas atmosphere box, by Frequency Induction Heating, the powder compact of connecting rod is heated to by 1250 DEG C and insulation 2 with 80 DEG C/min speed
Minute；The content of hydrogen is reduced to 1.0wt.% in powder batch in sintering process.
Processing step 5. in thermomechanically consolidate or be molded, be on the hydraulic press of exercisable closed atmosphere case is equipped with,
By process 4. it is middle complete high temperature sintering engine link part blank, be directly quickly transferred in finish forge mould die cavity, forge
And pressurize 2min, produce the engine link parts of TC4 titanium alloys.
Processing step 6. in vacuum dehydrogenation, be the TC4 titanium alloys connecting rod by step 5. middle manufacture at 700 DEG C, 1.0 ×
10-3~1.0 × 10-46h is kept in the vacuum drying oven of Pa vacuums, the hydrogen for making to remain in TC4 titanium alloy connecting rods is thoroughly discharged,
Final hydrogen content is 90ppm；
The alloy product of processing step 7., be by step 1.~6. process, produce the engine links of TC4 titanium alloys
Forging；
TC4 titanium alloys engine link manufactured in the present embodiment, oxygen mass content are only 0.22%, and consistency is up to
99.6%；Alloy surveys composition：Ti-6.04Al-4.03V (wt%).By solid solution+Ageing Treatment, the tensile strength of alloy
For 1300MPa, elongation percentage reaches 13%, Vickers hardness 375GPa.
Embodiment 4
2. the present embodiment and the difference of embodiment 2 are processing step, the mixed powder of alloy is prepared in synchronization mechanism ball milling
When last, be according to the proportioning of Ti-29Nb-13Ta-5Zr biological medical titanium alloys, will hydrogenation titanium sponge, hydrogenated niobium, hydrogenated tantal and
The particulate material of hydrogenation sponge zirconium is fitted into the ball grinder of stirring ball mill together, and synchronous mechanical ball mill is broken under argon gas protection
Broken and well mixedization prepares the mixed-powder of several hydride.Correspondingly, processing step 5.~7. in titanium alloy title
It is exactly Ti-29Nb-13Ta-5Zr.
Ti-29Nb-13Ta-5Zr titanium alloys extruded barses manufactured in the present embodiment, oxygen mass content are only 0.20%, are caused
Density is up to 99.9%.It is dissolved state average grain size and is less than 20 μm；+ 500 DEG C/6h/FC is dissolved by 800 DEG C/30min/WQ
Ageing Treatment, the tensile strength of alloy are up to 900MPa, and elongation percentage reaches 28%.
Embodiment 5
2. the present embodiment and the difference of embodiment 2 and embodiment 4 are processing step, alloy is prepared in synchronization mechanism ball milling
Mixed-powder when, be according to beta titanium alloy Ti-2Al-5Fe quality proportioning, will hydrogenate titanium sponge, -300 mesh pure aluminium powder
It is fitted into together in the ball grinder of stirring ball mill with electrolytic iron powder, synchronous mechanical ball mill is crushed and mixed under argon gas protection
Homogenize the mixed-powder raw material for preparing Ti-2Al-5Fe alloys.Correspondingly, processing step 5.~7. in titanium alloy title just
It is Ti-2Al-5Fe.As shown in figure 4, by the mechanical ball mill of 2 hours, alloy element Al and Fe powder particles are tiny (is less than 3 μ
M), and alloying elements distribution is uniform.
Ti-2Al-5Fe titanium alloys extruded barses manufactured in the present embodiment, oxygen mass content are only 0.21%, and consistency is high
Up to 99.8%, alloy actual measurement composition is Ti-1.98Al-5.15Fe.The average grain size of extruded rod solid solution state is 15 μm；By
850 DEG C/30min/WQ is dissolved+500 DEG C/6h/FC Ageing Treatments, and the tensile strength of alloy is up to 1320MPa, and elongation percentage reaches
16%.
Embodiment 6
The difference of the present embodiment and embodiment 2 is the powder compact of processing step 3., used mixed-powder be through
Pressed compact is carried out after transpassivation processing.Specifically passivation technology is：In the argon gas atmosphere case of 500ppm oxygen contents, holding atmosphere pressures are
1atm, it is passivated 60 minutes.In passivating process, powder is stirred once every 10 minutes, ensures that powder particle is all passivated.Powder
During last pressed compact, the oxygen content of closed atmosphere case argon gas inside atmosphere is still controlled less than 120ppm.
TC4 titanium alloys extruded barses manufactured in the present embodiment, oxygen mass content are 0.36%, and consistency is up to 99.6%.
By solid solution+Ageing Treatment, the tensile strength of alloy is 1400MPa, elongation percentage 8%.
Embodiment result shows that the inventive method is realized that hydrogenation titanium sponge is prepared with the synchronous ball mill of alloyed feedstock and mixed
Powder, powder need not sieve, and flour extraction is more than 96%；The pressed compact of powder is completed under inert atmosphere protection, quick heating is closed
Aurification, thermomechanical consolidation and shaping.The technological process of the present invention is short, efficiency high, it is possible to produce high-compactness (>=99.8%)
With the titanium and titanium alloy product of low oxygen content (≤0.26%)；The Main Mechanical of alloy is higher than the water of common variation titanium alloy
It is flat, and cost is significantly lower than conventional powder metallurgy titanium alloy.
Claims (10)
- It is 1. a kind of to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, it is characterised in that to include Following process：1. the hydrogenation of titanium sponge；2. synchronous ball mill prepares titanium hydride powders or mixed-powder；3. powder compact；4. it hurry up Speed sintering and sync section dehydrogenation；5. thermomechanical consolidation or shaping；6. thorough vacuum dehydrogenation；7. alloy product.
- 2. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：The hydrogenation treatment of process 1. middle titanium sponge, is 350~750 DEG C of temperature and 0.9~1.5atm in hydrogenation furnace Under conditions of Hydrogen Vapor Pressure, keep what is completed within 1~6 hour.
- 3. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：Process 2. in synchronous ball mill prepare titanium hydride powders or mixed-powder, refer to will hydrogenation titanium sponge or Titanium sponge is hydrogenated with alloyed feedstock according to being fitted into together with stoichiometric proportion in ball grinder, ball mill grinding is synchronized and mixing is equal Homogenize；The alloying raw material of addition, it is pure element powder, breakable master alloy particle or powder, or hydrogenates Composition granule or powder.
- 4. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：Process 2. in synchronous ball mill prepare titanium hydride powders or mixed-powder, be to enter under inert atmosphere protection Capable, ball mill uses planetary ball mill, stirring ball mill or tumbling ball mill；Titanium hydride powders made from ball milling Or the mixed-powder of alloy, it is not necessary to carry out screening process.
- 5. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：Process 3. in powder compact, be under inert atmosphere protection, take 2. titanium hydride powders that process is prepared or The mixed-powder of alloy is fitted into mould, and compacting is completed within 1~60 minute in the pressurize of 300~1500MPa pressure.
- 6. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：The process 4. Fast Sintering of middle powder compact and sync section dehydrogenation, is under inert gas shielding, by sense It should heat, be heated in plasma discharging heating or direct current, 1000~1350 DEG C are warming up to simultaneously with 30~200 DEG C/min speed What insulation was completed for 0~60 minute；Fast Sintering process realizes the dehydrogenation of part, in agglomerate hydrogen content be reduced to 0.6~ 1.2%.
- 7. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：Process 5. in thermomechanical consolidation or shaping, be the hydraulic pressure in the closed work box for being equipped with adjustable atmosphere Completed on machine, by process, 4. the middle powder compact for completing high temperature sintering and insulation is directly quickly transferred to extrusion die or forging In modeling tool, sufficiently densification and thermoforming are completed by extruding or forging effect.
- 8. manufacture titanium and titanium alloy and its zero as raw material to hydrogenate titanium sponge according to claim 1, one of 3~7 The method of part, it is characterised in that：Powder ball milling that process is related to during 2. arriving process 5., powder compact, Fast Sintering, heat Machinery consolidation or shaping, the oxygen content in inert atmosphere is controlled in 0~200ppm.
- 9. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：Process 6. in vacuum dehydrogenation, desorption temperature control at 400~850 DEG C, vacuum is maintained at 1.0 × 10-2~ 1.0×10-4Pa, 4~10h of dehydrogenation time.
- 10. it is according to claim 1 to hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts, It is characterized in that：Process 7. in alloy product, according to difference when densification and shaping using mould, be bar, tubing or The extruding long profiles of slab, or the parts of forging molding, types of alloys cover pure titanium or the titanium alloy of any condition.
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| PCT/CN2017/116626 WO2019085183A1 (en) | 2017-10-30 | 2017-12-15 | Method for fabricating titanium and titanium alloy metallurgical products |
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| CN114134359A (en) * | 2021-12-01 | 2022-03-04 | 东北大学 | Method for manufacturing titanium alloy material by using spherical titanium alloy coarse powder |
| CN114433859A (en) * | 2022-01-25 | 2022-05-06 | 华中科技大学 | High-quality electrode for titanium alloy powder, and preparation and application thereof |
| CN114433859B (en) * | 2022-01-25 | 2023-02-14 | 华中科技大学 | High-quality electrode for titanium alloy powder, and preparation and application thereof |
| CN115502400A (en) * | 2022-09-06 | 2022-12-23 | 中国航发北京航空材料研究院 | Method for rapidly preparing high-performance powder titanium alloy based on titanium hydride raw material |
| CN116393705A (en) * | 2023-05-11 | 2023-07-07 | 宝鸡市永盛泰钛业有限公司 | Titanium alloy material for 3D printing and preparation method thereof |
| CN116393705B (en) * | 2023-05-11 | 2023-09-08 | 宝鸡市永盛泰钛业有限公司 | Titanium alloy material for 3D printing and preparation method thereof |
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