CN104439261A - Preparation method for ultrapure Al3Ti intermetallic compound powder - Google Patents
Preparation method for ultrapure Al3Ti intermetallic compound powder Download PDFInfo
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- CN104439261A CN104439261A CN201410826981.5A CN201410826981A CN104439261A CN 104439261 A CN104439261 A CN 104439261A CN 201410826981 A CN201410826981 A CN 201410826981A CN 104439261 A CN104439261 A CN 104439261A
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- paper tinsel
- intermetallic compound
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Abstract
The invention provides a preparation method for ultrapure Al3Ti intermetallic compound powder. According to the method, Al foil and Ti foil are overlaid in a staggered mode, the uppermost layer and the lowermost layer are provided with the Ti foil, then, the overlaid Al foil and Ti foil are placed in a vacuum hot-pressing furnace, heating is gradually performed after vacuumization is performed till the highest temperature ranges from 675 DEG C to 685 DEG C, then, the temperature is preserved for seven hours, Al and Ti fully react to generate fragile blocky Al3Ti, the remaining thin layer parts of the Ti foil on the upper surface and the lower surface are removed, and different pressing head pressures are applied in the heating and heat-preserving process; the fragile blocky Al3Ti is mechanically pulverized and placed in a ball grinder to be ground into powder in a ball grinding mode. The commercial pure Al foil and the commercial pure Ti foil are adopted as raw materials, sources are wide, and production cost is effectively reduced; the highest temperature in the vacuum hot-pressing process is only 685 DEG C, the temperature is low, process is simple, production efficiency is greatly improved, and large-scale application and popularization and industrialization are easy; the purity of the Al3Ti can be guaranteed.
Description
Technical field
That the present invention relates to is a kind of preparation method of metal alloy compositions, the specifically ultrapure Al of a kind of low-temperature growth
3the method of Ti intermetallic compound powder.
Background technology
Ti-Al series intermetallic compound due to its density is low, higher than fusing point, specific strength is high, elastic modelling quantity is high and excellent non-oxidizability and corrosion resistance etc., and becomes the focus of Recent study exploitation.In Ti-Al series intermetallic compound, Al
3the thermodynamic property of Ti and dynamic performance are better than other forms of intermetallic compound.With the Ti-Al intermetallic compound of other types (as Ti
3al or TiAl) compare, Al
3ti elastic modelling quantity higher (216GPa), oxidation resistance is stronger, density lower (3.3g/cm3), thus becomes very promising high-temperature structural material in aerospace industry.On the other hand, intermetallic compound and metallic matrix have similar lattice structure and close thermal coefficient of expansion, and its particle well can infiltrate with matrix, and interface cohesion is firm, are to replace ceramic particle to prepare the good wild phase of metal-base composites as wild phase.Can by Al
3ti intermetallic compound powder particle joins in molten metal prepares metal-base composites (as aluminium base, magnesium base composite material etc.) as wild phase.In addition, Al
3ti intermetallic compound powder has important purposes in the preparation of abrasion-resistant metal coating.
Current Al
3the preparation method of Ti intermetallic compound powder mainly contains direct sintering and mechanical ball milling-reaction method.Direct sintering is prepared burden by certain mol proportion by Ti, Al powder; direct sintering reaction under Ar gas shielded, and be incubated a period of time, sintering temperature is generally at 800 DEG C ~ 1000 DEG C; Al melts at this temperature, Gu liquid Al surrounds Ti particle generation liquid/reaction generate Al
3ti layer, releases a large amount of reaction heat, impels Al
3ti and Ti is at Al
3the interface of Ti/Ti generates TiAl or TiAl
2, but along with the inside diffusion of Al, TiAl or TiAl
2be transformed into Al again
3ti, and then constantly form Al
3ti layer, but work as Al
3when Ti layer is very thick, Al is just difficult to through Al
3ti layer and Ti react, and so last possibility will at Al
3unreacted Ti core under the internal residual of Ti layer, or Al
3tiAl, TiAl that Ti and Ti generates
2layer.Therefore, that adopt direct sintering to prepare is not single Al
3ti phase, at Al
3the inside of Ti particle may include other phases.Machinery ball milling-reaction method be by Ti powder, Al powder carries out mixing by mechanical ball milling, powder is deformed, cold welding and fragmentation, produce a large amount of faying faces, form the multilayer shape composite powder of refinement, then reaction-sintered process is carried out to the composite powder after mechanical ball milling.But the activity of Ti powder, Al powder is large, be subject in Mechanical Milling Process polluting relatively large from the atmosphere in ball-milling medium, inner liner of bowl mill, ball grinder and process control agent etc.And ball milling needs for a long time, at least more than 60h just can obtain submicron order Ti, Al composite powder, makes it fully contact, reacts, noresidue Ti core.And the remarkable refinement of Ti, Al composite powder after mechanical ball milling, from ball grinder, be transferred to the pollution being more easily subject to air in reaction unit process.This preparation method's process is very long, is unfavorable for promoting.
Summary of the invention
The object of the present invention is to provide that a kind of cost is low, technique be simple, the high ultrapure Al of product purity
3the preparation method of Ti intermetallic compound powder.
The object of the present invention is achieved like this:
By staggered to Al paper tinsel and Ti paper tinsel superposition, most above and below one deck is Ti paper tinsel, then puts into vacuum hotpressing stove, is progressively heated to maximum temperature 675 DEG C ~ 685 DEG C after vacuumizing, be finally incubated 7 hours, allow Al and Ti fully react and generate Al
3ti forms the block Al of fragility
3ti, removes the titanium foil residual fraction thin layer on upper and lower surface, heats and applies different ram pressures in insulating process; By block for fragility Al
3ti mechanical crushing, puts into ball mill and carries out ball milling powdered.
The present invention can also comprise:
1, described Al paper tinsel and Ti paper tinsel to be the Thickness Ratio of Al and Ti be commercialization pure Al paper tinsel and the pure Ti paper tinsel of commercialization of 3.6 ~ 4.4 times.
2, be progressively heated to maximum temperature 675 DEG C ~ 685 DEG C after vacuumizing described in, finally insulation specifically comprises for 7 hours: vacuumize, air pressure is down to below 0.03Pa, and start heating, by room temperature to 640 DEG C, the time is 1h, is then incubated 10min; Be warming up to 660 DEG C from 640 DEG C, the time is 10min, is then incubated 10min; Be warming up to 685 DEG C from 660 DEG C, the time is 30min, insulation 7h; Stove is cold.
3, described heating from apply different ram pressures in insulating process and specifically comprise: be 2.5t ~ 3t from room temperature to the ram pressures that 500 DEG C of periods apply; The ram pressures of 500 DEG C to 650 DEG C period applyings is 1.5t ~ 2.3t; The after-applied ram pressures of 650 DEG C is 1t ~ 1.5t; 660 DEG C be warming up to the front 10min in 685 DEG C of stages after stop pressure head; 685 DEG C of insulations 5h, Al and Ti fully react and generate Al
3step-down head after Ti, tune ram pressures is 2t ~ 3t, extrudes the remaining Al of unreacted, then continues reaction one section.
4, before superposing, first remove the oxide-film on Al paper tinsel and Ti paper tinsel surface, and carry out Ultrasonic Cleaning, dry up.
The invention provides a kind of Al
3the novel processing step of Ti intermetallic compound, to solve Al
3the problems such as Ti intermetallic compound customary preparation methods production cost is high, complex process, composition are impure.
The present invention adopts commercially pure Al paper tinsel and commercially pure Ti paper tinsel low temperature under vacuum hotpressing condition to carry out liquid-solid reaction and generates the single-phase Al of high-purity
3ti intermetallic compound, recycling Mechanical Crushing and ball-milling method prepare highly purified Al
3ti powder.These technology of preparing raw material adopt commercially pure Al paper tinsel and commercially pure Ti paper tinsel, and wide material sources, significantly reduce production cost; The maximum temperature of vacuum hotpressing process only has 685 DEG C, and low temperature and technique are simple, substantially increase production efficiency, is easy to large-scale promotion application and carries out industrialization; Maximum temperature 685 DEG C insulation 5h, Ti and Al fully react and generate Al
3after Ti, remaining Al is extruded in pressurization, continues insulation 2h ~ 3h, just can guarantee Al
3the purity of Ti.
Accompanying drawing explanation
Fig. 1 prepares the block Al of gained
3the optical microscope photograph of Ti, can see without any defect;
Fig. 2 prepares the block Al of gained
3the XRD analysis result of Ti, can see that obtain is single-phase Al
3ti, does not have impurity;
Fig. 3 is SEM photo after 3h ball milling;
Fig. 4 is SEM photo after 6h ball milling;
Fig. 5 is XRD analysis result after 3h ball milling;
Fig. 6 is XRD analysis result after 6h ball milling.
Detailed description of the invention
A kind of Al
3the novel processing step of Ti intermetallic compound comprises: one, select the Thickness Ratio of Al and Ti to be that the commercialization pure Al paper tinsel of 3.6 ~ 4.4 times and the pure Ti paper tinsel of commercialization are cut into formed objects; Two, remove the oxide-film on Al paper tinsel and Ti paper tinsel surface, and carry out Ultrasonic Cleaning, dry up; Three, by staggered to Al paper tinsel and Ti paper tinsel superposition, most above and below one deck is Ti paper tinsel, then puts into vacuum hotpressing stove, is progressively heated to maximum temperature 675 DEG C ~ 685 DEG C after vacuumizing, be incubated and within 7 hours, allow Al and Ti fully react generation Al
3(the titanium foil residual fraction thin layer on upper and lower surface, finally removes Ti.), heat and in insulating process, apply different ram pressures; Four, by block for fragility Al
3ti mechanical crushing, puts into ball mill and carries out ball milling powdered.Al
3ti fusing point is high, good in oxidation resistance, and mechanical milling process does not react, than the Al that direct ball milling Ti powder, Al powder obtain
3ti powder purity is much higher.
This preparation method should adopt following technological parameter to be good:
Vacuumize, air pressure is down to below 0.03Pa, starts heating.By room temperature to 640 DEG C, the time is 1h, is then incubated 10min; Be warming up to 660 DEG C from 640 DEG C, the time is 10min, is then incubated 10min; Be warming up to 685 DEG C from 660 DEG C, the time is 30min, insulation 7h; Stove is cold.Ram pressures from room temperature to 500 DEG C of period applyings is 2.5t ~ 3t; The ram pressures of 500 DEG C to 650 DEG C period applyings is 1.5t ~ 2.3t; The after-applied ram pressures of 650 DEG C is 1t ~ 1.5t; 660 DEG C be warming up to the front 10min in 685 DEG C of stages after stop pressure head; 685 DEG C of insulations 5h, Al and Ti fully react and generate Al
3step-down head after Ti, tune ram pressures is 2t ~ 3t, extrudes the remaining Al of unreacted, then continues reaction a period of time (2h ~ 3h), to guarantee Al
3the purity of Ti.
Illustrate below and the present invention is described in more detail.
Steps A: the removal of Ti paper tinsel and Al paper tinsel surface film oxide.First all burrs of Ti paper tinsel are polished with 180 order sand paper, avoid scratching hand.Carry out frosted with 180 order sand paper along two vertical directions on a face, change two vertical diagonally opposing corner direction frosteds after the wet look being milled to Ti is dimmed gradually into, local emphasis frosted is carried out in the place being finally difficult to keeping to the side be ground to.When Ti surface whole dimmed by original light time, oxide-film has just been completely removed.Ti paper tinsel is turned over, the oxide-film of another side is removed.The method that oxide-film removed by Al paper tinsel is the same with Ti paper tinsel.
The cutting of step B:Ti paper tinsel and Al paper tinsel.To get the processed thickness in metal foil surface be the Ti paper tinsel of 0.5mm and thickness is that the Al paper tinsel plate shearing machine of 1.1mm is aimed at cut-off rule Ti paper tinsel and Al paper tinsel are all cut into the square that size is 100mm × 100mm.
The cleaning of step C:Ti paper tinsel and Al paper tinsel.Rinse Ti paper tinsel and Al paper tinsel simply with clear water, then paillon foil is put into the ultrasonic cleaner filling water purification and clean.Finally clamp paillon foil one by one with tweezers to put into and fill spirituous box and wash away.
Step D: open cold wind with hair-dryer and the paillon foil after cleaning is carried out dry tack free, prevents surface from producing oxidation.After dry, Ti paper tinsel is placed on orlop, being then Al paper tinsel, is subsequently Ti, like this Ti paper tinsel and Al paper tinsel is carried out staggered superposition successively, ensures that one deck is also Ti paper tinsel topmost, as shown in Figure 1.Paillon foil after superposition is put well with on clean paper bag, prepares to sinter into stove.
Step F: corrosion resistant plate on the top and bottom pad of the paillon foil of superposition, puts into stove mould.Vacuumize air pressure and be down to below 0.03Pa, undertaken programming, heating by optimised process.
Step G: the block Al that reaction-sintered is obtained
3ti carries out mechanical crushing, puts into omnidirectional planetary ball mill and carries out ball milling powder process, and ball and ball grinder are zirconia, and ratio of grinding media to material is 20:1, and rotating speed is 400r/min.As requested, adjustment Ball-milling Time, obtains the high-purity Al of different size
3ti powder.
Embodiment is for illustration of the present invention, instead of limitation of the present invention, does simple modifications, all belong to the scope of protection of present invention under concept thereof of the present invention to the present invention.
Claims (7)
1. a ultrapure Al
3the preparation method of Ti intermetallic compound powder, is characterized in that: by staggered to Al paper tinsel and Ti paper tinsel superposition, and most above and below one deck is Ti paper tinsel, then vacuum hotpressing stove is put into, progressively be heated to maximum temperature 675 DEG C ~ 685 DEG C after vacuumizing, be finally incubated 7 hours, allow Al and Ti fully react and generate Al
3ti forms the block Al of fragility
3ti, removes the titanium foil residual fraction thin layer on upper and lower surface, heats and applies different ram pressures in insulating process; By block for fragility Al
3ti mechanical crushing, puts into ball mill and carries out ball milling powdered.
2. ultrapure Al according to claim 1
3the preparation method of Ti intermetallic compound powder, is characterized in that: described Al paper tinsel and Ti paper tinsel to be the Thickness Ratio of Al and Ti be commercialization pure Al paper tinsel and the pure Ti paper tinsel of commercialization of 3.6 ~ 4.4 times.
3. ultrapure Al according to claim 1 and 2
3the preparation method of Ti intermetallic compound powder, maximum temperature 675 DEG C ~ 685 DEG C is progressively heated to after vacuumizing described in it is characterized in that, finally insulation specifically comprises for 7 hours: vacuumize, air pressure is down to below 0.03Pa, start heating, by room temperature to 640 DEG C, the time is 1h, is then incubated 10min; Be warming up to 660 DEG C from 640 DEG C, the time is 10min, is then incubated 10min; Be warming up to 685 DEG C from 660 DEG C, the time is 30min, insulation 7h; Stove is cold.
4. ultrapure Al according to claim 3
3the preparation method of Ti intermetallic compound powder, is characterized in that described heating and applies different ram pressures in insulating process and specifically comprise: be 2.5t ~ 3t from room temperature to the ram pressures that 500 DEG C of periods apply; The ram pressures of 500 DEG C to 650 DEG C period applyings is 1.5t ~ 2.3t; The after-applied ram pressures of 650 DEG C is 1t ~ 1.5t; 660 DEG C be warming up to the front 10min in 685 DEG C of stages after stop pressure head; 685 DEG C of insulations 5h, Al and Ti fully react and generate Al
3step-down head after Ti, tune ram pressures is 2t ~ 3t, extrudes the remaining Al of unreacted, then continues reaction one section.
5. ultrapure Al according to claim 1 and 2
3the preparation method of Ti intermetallic compound powder, is characterized in that: the oxide-film first removing Al paper tinsel and Ti paper tinsel surface before superposing, and carries out Ultrasonic Cleaning, dries up.
6. ultrapure Al according to claim 3
3the preparation method of Ti intermetallic compound powder, is characterized in that: the oxide-film first removing Al paper tinsel and Ti paper tinsel surface before superposing, and carries out Ultrasonic Cleaning, dries up.
7. ultrapure Al according to claim 4
3the preparation method of Ti intermetallic compound powder, is characterized in that: the oxide-film first removing Al paper tinsel and Ti paper tinsel surface before superposing, and carries out Ultrasonic Cleaning, dries up.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410826981.5A CN104439261A (en) | 2014-12-25 | 2014-12-25 | Preparation method for ultrapure Al3Ti intermetallic compound powder |
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| CN201410826981.5A CN104439261A (en) | 2014-12-25 | 2014-12-25 | Preparation method for ultrapure Al3Ti intermetallic compound powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002450A (en) * | 2015-07-31 | 2015-10-28 | 哈尔滨工程大学 | Method for improving room-temperature plasticity and strength of Al3Ti intermetallic compound |
| CN109913678A (en) * | 2019-03-15 | 2019-06-21 | 武汉大学 | A kind of TiAl3Particle enhanced aluminum-based composite material and its preparation method and application |
| CN113458400A (en) * | 2021-07-23 | 2021-10-01 | 中北大学 | Ti-Al3Ti intermetallic compound laminated composite board preparation method |
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| JPH01301801A (en) * | 1988-05-31 | 1989-12-06 | Sumitomo Light Metal Ind Ltd | Production of ti-al intermetallic compound powder |
| CN1535812A (en) * | 2003-04-11 | 2004-10-13 | 中国科学院金属研究所 | Preparation method of Ti-AL-Ti multi-layer laminated composite material |
| CN103572187A (en) * | 2013-11-14 | 2014-02-12 | 哈尔滨工程大学 | Preparation method of light-weight intermetallic compound based layered composite material |
| CN104099540A (en) * | 2014-08-06 | 2014-10-15 | 哈尔滨工程大学 | Preparation method of NiTi fiber reinforced intermetallic compound-based laminar composite material for vibration and noise reduction |
-
2014
- 2014-12-25 CN CN201410826981.5A patent/CN104439261A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01301801A (en) * | 1988-05-31 | 1989-12-06 | Sumitomo Light Metal Ind Ltd | Production of ti-al intermetallic compound powder |
| CN1535812A (en) * | 2003-04-11 | 2004-10-13 | 中国科学院金属研究所 | Preparation method of Ti-AL-Ti multi-layer laminated composite material |
| CN103572187A (en) * | 2013-11-14 | 2014-02-12 | 哈尔滨工程大学 | Preparation method of light-weight intermetallic compound based layered composite material |
| CN104099540A (en) * | 2014-08-06 | 2014-10-15 | 哈尔滨工程大学 | Preparation method of NiTi fiber reinforced intermetallic compound-based laminar composite material for vibration and noise reduction |
Non-Patent Citations (1)
| Title |
|---|
| 常云鹏等: "金属间化合物基层状复合材料Ti-Ai3Ti制备及其力学行为", 《第17届全国复合材料学术会议论文》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002450A (en) * | 2015-07-31 | 2015-10-28 | 哈尔滨工程大学 | Method for improving room-temperature plasticity and strength of Al3Ti intermetallic compound |
| CN109913678A (en) * | 2019-03-15 | 2019-06-21 | 武汉大学 | A kind of TiAl3Particle enhanced aluminum-based composite material and its preparation method and application |
| CN109913678B (en) * | 2019-03-15 | 2020-10-30 | 武汉大学 | TiAl3Particle reinforced aluminum-based composite material and preparation method and application thereof |
| CN113458400A (en) * | 2021-07-23 | 2021-10-01 | 中北大学 | Ti-Al3Ti intermetallic compound laminated composite board preparation method |
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