CN101787498B - Method for directional heating crystallization on block amorphous alloy - Google Patents
Method for directional heating crystallization on block amorphous alloy Download PDFInfo
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- CN101787498B CN101787498B CN201010122796XA CN201010122796A CN101787498B CN 101787498 B CN101787498 B CN 101787498B CN 201010122796X A CN201010122796X A CN 201010122796XA CN 201010122796 A CN201010122796 A CN 201010122796A CN 101787498 B CN101787498 B CN 101787498B
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Abstract
The invention relates to a method for directional heating crystallization on block amorphous alloy. The method is characterized in that preparation process is completed in a directional heating-cooling device, the device is composed of four parts of a preservation zone (1), a heating zone (2), a cooling zone (3) and a draw bar (4), strip platy block amorphous alloy sample (5) is immersed in liquid medium in the preservation zone (1), under the driving of the draw bar (4), the sample (5) is moved into the heating zone (2) below the heating zone (2) at set speed and then moved out from the heating zone (2) above after heating crystallization, the sample (5) immediately enters into the cooling zone (3) to be cooled by inert gas after being moving out from the heating zone (2), so as to prevent oxidation of the sample (5) and further crystal growth. The method of the invention has low technological temperature and convenient operation; crystal shape can be flexibly selected, both fibroid unidirectional crystal and beaded and stub unidirectional crystal can be obtained by adjusting technological parameter. Besides, production process of the method of the invention is easy to automatize, production efficiency is high, and production cost is low.
Description
Technical field
The present invention relates to the amorphous alloy crystallization method, particularly for relating to the method that a kind of directional heating crystallization strengthens block amorphous alloy.
Technical background
Non-crystaline amorphous metal is claimed metallic glass again, has short range order, the unordered metastable state constitutional features of long-range.Its atom is the topological disorder arrangement at three-dimensional space when solid-state, and in certain temperature range, keeps this state relatively stable.Compare with crystal alloy, non-crystaline amorphous metal possesses many excellent properties, like high firmness, HS, high resistance, anti-corrosion and wear-resisting etc., is one of emphasis of material researcher and industry member research and development high performance structures and functional materials concern.Yet non-crystaline amorphous metal often has bigger fragility, because its thermodynamic (al) unstable adds problems such as manufacturing cost, has influenced its practical application simultaneously.The crystallization of non-crystaline amorphous metal is an important channel of improving its comprehensive mechanical property.Simultaneously; Crystallization through block amorphous alloy; Can obtain nanometer crystal alloy or nanocrystalline enhanced amorphous alloy composite material with comparalive ease, therefore, the nano-crystallization of block amorphous alloy has become one of important means of preparation Bulk Metal Matrix Nano-composites.And in the process of solidification of metal melt, only if very high rate of cooling is arranged (greater than 10
4K/s), not so be difficult to directly obtain nanocrystal from metal melt.
In metal-base composites, except the particle reinforced composite materials, also having with the fiber is the matrix material that strengthens body.Fiber-reinforced metal matrix composite has better unidirectional mechanical property, adds and the enhancing body in this type matrix material is normally outside at present, has that interface wet ability is poor, the interface combines problems such as bad.Aspect the preparation of fiber-reinforced metal matrix composite, adopt the melt directional solidification process unidirectional crystal of can growing, can obtain that good interface combines between matrix and the enhancing body.In different-alloy systems such as Sn base, Cu base, all obtained very outstanding result of study.Because non-crystaline amorphous metal possesses many excellent properties, therefore, if in block amorphous alloy, grow unidirectional crystal, is expected obviously to improve its temperature-room type plasticity and comprehensive mechanical property.For this reason, on the basis of non-crystaline amorphous metal thermic crystallization,, crystal is further developed to unidirectional crystal, then can prepare original position fiber reinforcement amorphous alloy-based composite material if through the control heating condition.Yet, up to the present, also not about from block amorphous alloy, obtaining the report of directional crystal through the crystallization mode.
Summary of the invention
To the problems referred to above, the inventive principle that the present invention proposes is: through block amorphous alloy being carried out the orientation heating, make amorphous alloy crystallization, and guarantee to form directional crystal in the non-crystaline amorphous metal through the adjustment crystallization process.
The present invention proposes the method that a kind of directional heating crystallization strengthens block amorphous alloy; It is characterized in that: the preparation process is accomplished in orientation heating-refrigerating unit; This device is immersed in strip of sheet block amorphous alloy sample 5 in the liquid medium that keeps district 1 by keeping district 1, heating zone 2, cooling zone 3 and 4 four parts of towbar to form, and under the drive of towbar 4; 2 belows move into heating zone 2 from the heating zone with the speed set with sample 5; Shifted out by the top of heating zone 2 behind the heating crystallization, sample 5 goes out heating zone 2 and promptly gets into rare gas element refrigerative cooling zone 3 is arranged, and further grows up with the crystal that prevents sample oxidation and generation.
Described maintenance district 1; Be in the below of heating zone; Have the cavity that holds sample 5, be full of in the cavity not and with non-crystaline amorphous metal sample 5 chemical reactions and fusing point take place and be lower than the liquid cooling medium that non-crystaline amorphous metal glass transition temperature Tg, boiling point are higher than the Heating temperature of setting.
Described heating zone 2 is heating members that a both ends open can supply the sample turnover, and its lower ending opening directly immerses 1～2mm in the liquid medium that keeps in the district 1, and the upper end links to each other with cooling zone 3; Heating member constant temperature partial-length is 5～20mm, and the upper and lower of heating zone all is provided with the thermal baffle of allowing the sample opening; The Heating temperature of heating zone constant temperature part is chosen in below the above alloy solidus temperature of non-crystaline amorphous metal glass transition temperature Tg as required; When crystalline size little (≤1 μ m) that needs obtain; Selection is in the temperature below the interval Tg of non-crystaline amorphous metal high undercooling fluid temperature above (0.9Tx+0.1Tg), otherwise selects to be higher than the temperature of (0.9Tx+0.1Tg); Wherein, Tx is that non-crystaline amorphous metal begins crystallization temperature, and temperature unit is K.
Described cooling zone 3 is in the top of heating zone 2, adopts the cooling of mobile rare gas element, for preventing the sample oxidation, when sample moves into heating zone 2, opens gas cooling.
Described towbar 4 is driven by Ultralow speed motor, and is connected with strip of sheet sample 5 through the whole bag of tricks, and the drive sample is done constant speed and moved, and as required the translational speed of sample is controlled in 0.05～5 μ m/s scope.
This patent method has following advantage:
1, technological temperature is low, and is easy and simple to handle;
2, can select crystal habit neatly,, both can obtain fibrous unidirectional crystal, also can obtain beading, the unidirectional crystal of corynebacterium through the adjusting process parameter;
3, production process easily is automated, and production efficiency is high, and production cost is low.
In a word, can successfully prepare the various interior directional crystals of giving birth to through aforesaid method and strengthen the block amorphous alloy matrix material.
Description of drawings
Fig. 1 directional nano crystallization system synoptic diagram
1 keeps district, 2 heating zone, 3 cooling zones, 4 towbars, 5 samples
Grow the SEM photo of fibrous directional crystal in Fig. 2 block magnesium base amorphous alloy
Embodiment
Employed in the present invention term only if other explanation is arranged, generally has the implication of those of ordinary skills' common sense.Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these embodiment just in order to demonstrate the invention, but not limit scope of the present invention by any way.In following embodiment, various processes and the method do not described in detail are ordinary methods as known in the art.
Embodiment 1
Magnesium base block amorphous alloy Mg
65Cu
25Y
10The directed crystallization of band (long 200mm, wide 6mm, thick 30 μ m) is carried out on orientation heating-refrigerating unit, and this device is by keeping district 1, heating zone 2, cooling zone 3,4 four major portions of towbar to form.Keep district 1 to be in the below of heating zone, have the dark cavity of 220mm, be full of heat-eliminating medium silicone oil in the cavity, its burning-point is 210 ℃.Heating zone 2 is heating members that a both ends open can supply the sample turnover, and its lower ending opening immerses 1mm in the silicone oil that keeps in the district 1, and the upper end links to each other with cooling zone 3; Heating member constant temperature partial-length is 5mm, and the upper and lower of heating zone is provided with the thermal baffle of allowing the sample opening; The temperature of the constant temperature part of heating zone 2 is made as 190 ℃.Cooling zone 3 is in the top of heating zone 2, adopts the cooling of mobile inert nitrogen gas, for preventing Mg
65Cu
25Y
10Gas cooling is opened in the oxidation of band sample when sample moves into heating zone 2.Towbar 4 is driven by Ultralow speed motor, and passes through chuck with Mg
65Cu
25Y
10The band sample is attached thereto, and towbar 4 moves drive sample constant speed from the bottom up and moves up, and the translational speed of sample is controlled at 0.05 μ m.
Strip of sheet block amorphous alloy sample is immersed in the silicone oil medium that keeps district 1; And under the drive of towbar 4; 2 belows move into heating zone 2 from the heating zone with the speed set with sample; The other end by heating zone 2 behind the heating crystallization shifts out, and sample goes out heating zone 2 and promptly gets into nitrogen refrigerative cooling zone 3 is arranged, and further grows up to prevent crystal.SEM photo such as Fig. 2 of the sample that obtains, wherein grey form and aspect are Mg
2Cu is the directional fiber shape, and the crystalline diameter is 0.5～1.0 μ m.
Embodiment 2
Iron-base block amorphous alloy Fe
74Al
4Ga
2P
12B
4Si
4The directed crystallization of sample (long 150mm, wide 5mm, thick 1mm) is carried out on orientation heating-refrigerating unit, and this device is by keeping district 1, heating zone 2, cooling zone 3,4 four major portions of towbar to form.Keep district 1 to be in the below of heating zone, have the dark cavity of 200mm, be full of the heat-eliminating medium liquid tin in the cavity, its boiling point is 2270 ℃.Heating zone 2 is heating members that a both ends open can supply the sample turnover, and its lower ending opening immerses 1mm in the silicone oil that keeps in the district 1, and the upper end links to each other with cooling zone 3; Heating member constant temperature partial-length is 10mm, and the upper and lower of heating zone is provided with the thermal baffle of allowing the sample opening; The temperature of the constant temperature part of heating zone 2 is made as 470 ℃.Cooling zone 3 is in the top of heating zone 2, adopts the cooling of mobile inert nitrogen gas, for preventing the oxidation of band sample, when sample moves into heating zone 2, opens gas cooling.Towbar 4 is driven by Ultralow speed motor, and passes through chuck with Mg
65Cu
25Y
10The band sample is attached thereto, and towbar 4 moves drive sample constant speed from the bottom up and moves up, and the translational speed of sample is controlled at 0.1 μ m.
Strip of sheet block amorphous alloy sample is immersed in the silicone oil medium that keeps district 1; And under the drive of towbar 4; 2 belows move into heating zone 2 from the heating zone with the speed set with sample; The other end by heating zone 2 behind the heating crystallization shifts out, and sample goes out heating zone 2 and promptly gets into nitrogen refrigerative cooling zone 3 is arranged, and further grows up to prevent crystal.Finally on the non-crystaline amorphous metal matrix, obtained regularly arranged fibrous crystals.
Embodiment 3
Magnesium base block amorphous alloy Mg
65Cu
25Y
10Band (long 200mm, wide 6mm, thick 25 μ m) is behind 210 ℃, the preparatory crystallization of 5min in the process furnace in protection of inert gas; On orientation heating-refrigerating unit, carry out directed crystallization, this device is by keeping district 1, heating zone 2, cooling zone 3,4 four major portions of towbar to form.Keep district 1 to be in the below of heating zone, have the dark cavity of 220mm, be full of heat-eliminating medium silicone oil in the cavity, its burning-point is 230 ℃.Heating zone 2 is heating members that a both ends open can supply the sample turnover, and its lower ending opening immerses 2mm in the silicone oil that keeps in the district 1, and the upper end links to each other with cooling zone 3; Heating member constant temperature partial-length is 20mm, and the upper and lower of heating zone is provided with the thermal baffle of allowing the sample opening; The temperature of the constant temperature part of heating zone 2 is made as 210 ℃.Cooling zone 3 is in the top of heating zone 2, adopts the cooling of mobile inert nitrogen gas, for preventing Mg
65Cu
25Y
10Gas cooling is opened in the oxidation of band sample when sample moves into heating zone 2.Towbar 4 is driven by Ultralow speed motor, and passes through chuck with Mg
65Cu
25Y
10The band sample is attached thereto, and towbar 4 moves drive sample constant speed from the bottom up and moves up, and the translational speed of sample is controlled at 0.5 μ m.
Strip of sheet block amorphous alloy sample is immersed in the silicone oil medium that keeps district 1; And under the drive of towbar 4; 2 belows move into heating zone 2 from the heating zone with the speed set with sample; The other end by heating zone 2 behind the heating crystallization shifts out, and sample goes out heating zone 2 and promptly gets into nitrogen refrigerative cooling zone 3 is arranged, and further grows up to prevent crystal.Finally in the magnesium base block amorphous alloy, formed directed catenate crystal.
Embodiment 4
Magnesium base block amorphous alloy Mg
65Cu
25Y
10Band (long 200mm, wide 6mm, thick 20 μ m) is behind 210 ℃, the preparatory crystallization of 5min in the process furnace in protection of inert gas; On orientation heating-refrigerating unit, carry out directed crystallization, this device is by keeping district 1, heating zone 2, cooling zone 3,4 four major portions of towbar to form.Keep district 1 to be in the below of heating zone, have the dark cavity of 220mm, be full of heat-eliminating medium silicone oil in the cavity, its burning-point is 230 ℃.Heating zone 2 is heating members that a both ends open can supply the sample turnover, and its lower ending opening immerses 1mm in the silicone oil that keeps in the district 1, and the upper end links to each other with cooling zone 3; Heating member constant temperature partial-length is 10mm, and the upper and lower of heating zone is provided with the thermal baffle of allowing the sample opening; The temperature of the constant temperature part of heating zone 2 is made as 210 ℃.Cooling zone 3 is in the top of heating zone 2, adopts the cooling of mobile inert nitrogen gas, for preventing Mg
65Cu
25Y
10Gas cooling is opened in the oxidation of band sample when sample moves into heating zone 2.Towbar 4 is driven by Ultralow speed motor, and passes through chuck with Mg
65Cu
25Y
10The band sample is attached thereto, and towbar 4 moves drive sample constant speed from the bottom up and moves up, and the translational speed of sample is controlled at 5.0 μ m.
Strip of sheet block amorphous alloy sample is immersed in the silicone oil medium that keeps district 1; And under the drive of towbar 4; 2 belows move into heating zone 2 from the heating zone with the speed set with sample; The other end by heating zone 2 behind the heating crystallization shifts out, and sample goes out heating zone 2 and promptly gets into nitrogen refrigerative cooling zone 3 is arranged, and further grows up to prevent crystal.At Mg
65Cu
25Y
10Obtained to be the crystal of corynebacterium in the block amorphous alloy.
Claims (5)
1. the method for a directional heating crystallization on block amorphous alloy; It is characterized in that: the preparation process is accomplished in orientation heating-refrigerating unit; This device is immersed in strip of sheet block amorphous alloy sample (5) in the liquid medium that keeps district (1) by keeping district (1), heating zone (2), cooling zone (3), (4) four parts of towbar to form, and under the drive of towbar (4); Sample (5) is moved the immigration heating zone (2), (2) below from the heating zone with the speed constant speed of setting; The translational speed of sample (5) is controlled in 0.05～5 μ m/s scope as required and selects, and is shifted out by the top of heating zone (2) behind the heating crystallization, and sample (5) goes out heating zone (2) and promptly gets into rare gas element refrigerative cooling zone (3) is arranged; Crystal to prevent sample (5) oxidation and formation is further grown up, and gives birth to directional crystal in obtaining and strengthens the block amorphous alloy matrix material.
2. method according to claim 1; It is characterized in that: described maintenance district (1); Be in the below of heating zone (2); Have the cavity that holds sample (5), be full of in the cavity not and with non-crystaline amorphous metal sample (5) chemical reaction and fusing point take place and be lower than the liquid cooling medium that non-crystaline amorphous metal glass transition temperature Tg, boiling point are higher than the Heating temperature of setting.
3. method according to claim 1 is characterized in that: described heating zone (2) are the heating members that a both ends open can supply the sample turnover, and its lower ending opening directly immerses 1～2mm in the liquid medium that keeps in the district (1), and the upper end links to each other with cooling zone (3); Heating member constant temperature partial-length is 5～20mm, and the upper and lower of heating zone (2) all is provided with the thermal baffle of allowing sample (5) opening; The Heating temperature of heating zone (2) constant temperature part is selected below the above alloy solidus temperature of non-crystaline amorphous metal glass transition temperature Tg as required; During the crystalline size that obtains when needs≤1 μ m; Selection is in more than the interval Tg of non-crystaline amorphous metal high undercooling fluid temperature; Temperature (0.9Tx+0.1Tg), otherwise selection is higher than the temperature of (0.9Tx+0.1Tg); Wherein, Tx is that non-crystaline amorphous metal begins crystallization temperature, and temperature unit is K.
4. method according to claim 1 is characterized in that: described cooling zone (3), be in the top of heating zone (2), adopt the cooling of mobile rare gas element, for preventing the sample oxidation,, opens by sample gas cooling when moving into heating zone (2).
5. method according to claim 1 is characterized in that: described towbar (4) is driven by Ultralow speed motor, and is connected with strip of sheet sample (5).
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| CN201010122796XA CN101787498B (en) | 2010-03-12 | 2010-03-12 | Method for directional heating crystallization on block amorphous alloy |
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| US6254695B1 (en) * | 1998-08-13 | 2001-07-03 | Vacuumschmelze Gmbh | Method employing tension control and lower-cost alloy composition annealing amorphous alloys with shorter annealing time |
| CN1397089A (en) * | 2000-02-15 | 2003-02-12 | 松下电器产业株式会社 | Non-single crystal film, substrate with non-single crystal film, method and apparatus for producing the same, method and apparatus for inspecting the same, thin film transistor, thin film transistor |
| CN1580313A (en) * | 2003-08-01 | 2005-02-16 | 中国科学院金属研究所 | Macro amorphous alloy nano-level preparation method |
| JP2006118040A (en) * | 2004-09-27 | 2006-05-11 | Tohoku Univ | Method for producing nanocrystal magnetic material with oriented crystal grain |
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