CN108500240A - A kind of preparation method of large-size bulk amorphous alloy - Google Patents
A kind of preparation method of large-size bulk amorphous alloy Download PDFInfo
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- CN108500240A CN108500240A CN201710099934.9A CN201710099934A CN108500240A CN 108500240 A CN108500240 A CN 108500240A CN 201710099934 A CN201710099934 A CN 201710099934A CN 108500240 A CN108500240 A CN 108500240A
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Abstract
The invention discloses a kind of preparation method of large-size bulk amorphous alloy, step is：By by getting rid of the amorphous thin ribbon prepared with method, the amorphous powder prepared by atomization or ball-milling method or the amorphous small blocks prepared by fusion casting, it is put into mold, a certain temperature T of supercooling liquid phase region is heated to according to the heating speed of 10 ~ 30 DEG C/minn(Tg＜ Tn＜ Tx, wherein TgFor glass transformation temperature, TxTo start crystallization temperature）0.5min ~ 60min is kept the temperature afterwards, and applies the pressure of 2 ~ 200MPa to it simultaneously, and then cooling and demolding, obtains large-sized block amorphous alloy.Preparation process of the present invention is simple, breaches the size limitation that fusion casting prepares block amorphous alloy, can obtain larger sized block amorphous alloy.
Description
Technical field
The present invention relates to the preparation methods of large-size bulk amorphous alloy, belong to block amorphous alloy preparation field.
Background technology
Non-crystaline amorphous metal (amorphous alloy) be avoided during solidification by metal liquid crystallize and generate one
Class new metallic material.Its internal atom is presented unlike as in crystal it is periodic, long-range order regularly arranged,
But (SRO) of a kind of short distance or (MRO) ordered arrangement of intermediate range are presented to a certain extent.This long-range of non-crystaline amorphous metal
Disordered structure, the characteristic in certain temperature range with softening and there is no as knots such as dislocation, crystal boundary, faults in crystal
A series of structure defect so that it is with performances better than crystalline material, intensity, hardness such as superelevation, and the elastic limit of bigger is excellent
Different machine-shaping property（Due to supercooling liquid phase region）, excellent magnetic property, more resistant to corrosion and better tribology
Energy is equal.
Since preparing Au-Si non-crystaline amorphous metals using quick chilling method from nineteen sixty Duwez, people have been developed a variety of
Prepare the technology of amorphous.These technologies are mostly by obtaining high cooling velocity, the formation of crystalline phases being inhibited to obtain amorphous.
Non-crystaline amorphous metal its cooling rate is such as prepared by the way of fast melt-quenching can reach 105~107K/s, and picosecond laser is used to quench
Highest cooling rate can reach 10 when method prepares amorphous12k/s.However, the acquisition of so high cooling velocity needs the sample prepared
It at least can fully radiate in one direction, therefore amorphous prepared by early stage is mostly ribbon, filament, film or powder
Shape.Jones et al. is estimated more than 104K/s and 108Under the cooling condition of k/s, the amorphous ribbon maximum gauge point of formation
1mm and 10um are not exceeded.Since the nineties in 19th century, the Akihisa Inoue from northeastern Japan university and California, USA reason
Johnson of work et al. is changed over obtains the think of of the strong non-crystaline amorphous metal system of amorphous formation ability from process conditions are improved
Road, and from the angle of design of alloy, by more alloyings, microalloying come increase the complexity of alloy system with
And the viscosity of melt, and then large-sized block amorphous alloy is obtained, but it is big to be obtained by the thinking of composition design
The block amorphous alloy of size needs a large amount of trial and error to test, and many achievements on well are exactly to establish on this basis, this nothing
It is suspected to be time-consuming and laborious.In addition, for special component composition, it always will appear a full-size, under this size
Block sample can be full non-crystaline amorphous metal, crystal phase occur more than this size, solidifying using melts such as copper mold casting, water quenchings
Block amorphous alloy prepared by solid method is no more than this full-size.Meanwhile typical close is prepared by copper mold casting method
The minimum cooling velocity of the block amorphous alloy of golden system is generally also close to 103K/s so that obtained block amorphous alloy
Size cannot meet engineering demand.
Invention content
The purpose of the present invention is to provide a kind of methods preparing large-size bulk amorphous alloy.
The technical solution of the object of the invention is：A kind of preparation method of large-size bulk amorphous alloy, will be by getting rid of
The amorphous thin ribbon prepared with method, the amorphous powder prepared by atomization or ball-milling method or the small size block prepared by fusion casting
Non-crystaline amorphous metal is positioned in mold, and a certain temperature T in supercooled liquid phase section is heated to the heating speed of 10 ~ 30 DEG C/minnUnder
(Tg＜ Tn＜ Tx, wherein TgFor glass transformation temperature, TxTo start crystallization temperature）, 0.5min ~ 60min is kept the temperature, in 2 ~ 200MPa
Pressure under carry out thermoplasticity compression, then Slow cooling, you can obtain large-size bulk amorphous alloy.
In the step, amorphous thin ribbon, amorphous powder and small size block amorphous alloy system be zirconium base, titanium-based, it is copper-based,
Ni-based, iron-based, aluminium base, cobalt-based, magnesium-based or auri amorphous any one.
In the step, mold uses steel mold or copper mould.
Compared with traditional fusion casting prepares the technology of block amorphous alloy, the advantageous effect that the present invention obtains is：
（1）The block amorphous alloy that preparation method of the present invention is prepared can keep former amorphous thin ribbon, amorphous powder or
The characteristic of wide supercooling liquid phase region, is conducive to heat ductile forming and prepares small precision component possessed by small size block amorphous alloy；
（2）Preparation method of the present invention is simple for process, and it is relatively low to prepare cooling velocity required when bulk amorphous alloy, breaches
The size for the block amorphous alloy that conventional method is prepared limits and the requirement to cooling condition, also avoids carrying out on ingredient
A large amount of trial and error experiment prepares the cumbersome of large-size bulk amorphous alloy, is conducive to industrialized production, promotes bulk amorphous alloy conjunction
The engineer application of gold.
Description of the drawings
Fig. 1 is the XRD for preparing amorphous thin ribbon used in large-size bulk amorphous alloy described in the embodiment of the present invention 1
Figure.
Fig. 2 is the DSC for preparing amorphous thin ribbon used in large-size bulk amorphous alloy described in the embodiment of the present invention 1
Figure.
Fig. 3 is the XRD diagram of the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 1.
Fig. 4 is the DSC figures of the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 1.
Fig. 5 is to prepare block amorphous alloy used in large-size bulk amorphous alloy described in the embodiment of the present invention 2
XRD diagram.
Fig. 6 is to prepare block amorphous alloy used in large-size bulk amorphous alloy described in the embodiment of the present invention 2
DSC schemes.
Fig. 7 is the XRD diagram of the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 2.
Fig. 8 is the DSC figures of the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 2.
Fig. 9 is the SEM of the linkage interface of the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 2
Figure.
Figure 10 is the XRD diagram for preparing amorphous powder needed for large-size bulk amorphous alloy described in the embodiment of the present invention 3.
Figure 11 is the DSC of the amorphous powder and the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 3
Figure.
Figure 12 is the XRD diagram of the large-size bulk amorphous alloy being prepared described in the embodiment of the present invention 3.
Specific implementation mode
Present disclosure is described further with reference to embodiment.
The amorphous thin ribbon, amorphous powder and the small size block amorphous alloy that are there is provided in the present invention and the big ruler being prepared
The thermal physical property parameter of very little block amorphous alloy can pass through the acquisitions such as DSC, XRD.It uses in an embodiment of the present invention
NETZSCH STA449C Jupiter measure the glass transition temperature and crystallization temperature of amorphous, and heating rate when test is
20K/min, test are carried out under the argon gas protection of purity 99.99%, and it is 26ml/min to send the flow of argon gas.The present invention's
The confirmation for carrying out non crystalline structure in embodiment using Bruker D8 X-ray diffractometers, Cu targets K is used when testα, power
1.6Kw.The observation of the linkage interface for the large-size bulk amorphous alloy being prepared by small size block amorphous alloy uses FEI
Quanta 250F Flied emission environmental scanning electronic microscopes.
The preparation of 1. large scale Zr65Al10Ni10Cu15 block amorphous alloys of embodiment
Pass through the full-size of Zr65Al10Ni10Cu15 block amorphous alloys prepared by traditional fusion casting（Critical dimension）Generally
It is apparently higher than this in the size of 10mm or so, and the block amorphous alloy that the present invention prepares, the present invention prepares large scale
The step of Zr65Al10Ni10Cu15 block amorphous alloys, is as follows：
（1）The preparation of amorphous thin ribbon：High-purity Zr, Al, Ni, Cu bulk metal is converted to quality percentage according to atomic percent
Than carrying out dispensing, high vacuum arc-melting furnace melting is put into after ultrasonic cleaning.Break into melted master alloy ingot into pieces fritter,
It after polishing cleaning, weighs certain mass and is put into the quartz ampoule of certain specification, quartz ampoule, which is then put into copper roller, revolves vacuum of quenching
In furnace chamber, after the position for regulating quartz ampoule and induction coil, starts to take out low vacuum and high vacuum successively, wait for that vacuum degree reaches
3.5╳10-3When Pa, high-purity argon gas to the air pressure that 99.999% is filled with into vacuum container reaches 0.05MPa, then proceeds by
Get rid of band.The rotating speed of copper roller is 1900rpm when getting rid of band, and quartz ampoule nozzle is 2 ~ 3mm apart from roll surface distance.First under low induced current
It is preheated, then quickly heats up to high current, after waiting for that melt is completely melt, reduced induced current and keep the temperature a period of time,
When melt flows are steady, start to get rid of band, XRD tests is carried out to obtained Tape samples, the results are shown in Figure 1, it was demonstrated that it is really
For full amorphous, DSC tests are carried out to obtained Tape samples, the results are shown in Figure 2, measures its Tg=375 DEG C, Tx=466 DEG C, Δ T
=91℃；
（2）Prepare large scale Zr65Al10Ni10Cu15 block amorphous alloys：The amorphous thin ribbon prepared is weighed into cleaning drying
It is put into ready mold, mold is put into high vacuum sintering furnace later then, 200MPa is applied to amorphous thin ribbon
Pressure, and start to vacuumize.Wait for that vacuum degree reaches 10-3It when Pa magnitudes, begins to warm up, is first heated to 370 DEG C with 30 DEG C/min
Left and right heat preservation 30 minutes, keeps mold and amorphous thin ribbon temperature uniform, is then heated to 450 DEG C or so heat preservations with 20 DEG C/min rates
40 minutes, make the sufficient viscous flow of non-crystaline amorphous metal, after cooling and demolding, that is, blocks of large alloy sample is prepared, to obtaining
Sample carry out XRD tests, as a result as indicated at 3, it was demonstrated that it is really non crystalline structure, and DSC tests are carried out to obtained block sample,
The results are shown in Figure 4, measures its Tg=373 DEG C, Tx=456 DEG C, Δ T=83 DEG C, maintain that former amorphous thin ribbon has substantially is wider than
The characteristic in cold liquid phase section, obtained sample are 20mm in the minimum dimension of three-dimensional, hence it is evident that have been more than its critical dimension.
The preparation of 2. large scale Zr35Ti30Be27.5Cu7.5 block amorphous alloys of embodiment
Pass through the full-size of Zr35Ti30Be27.5Cu7.5 block amorphous alloys prepared by traditional fusion casting（Critical dimension）One
As in 15mm, and the size for the block amorphous alloy that the present invention prepares is apparently higher than this, and the present invention prepares large scale
The step of Zr35Ti30Be27.5Cu7.5 block amorphous alloys, is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Zr, Ti, Cu, Be equal to 99.9% or more.According to
Zr35Ti30Be27.5Cu7.5 nominal composition dispensings, the melting in high vacuum arc-melting furnace under argon gas protection.Copper is used later
The block Bar samples that enough specifications are Ф 6mm ╳ 67mm are prepared in mould spray to cast method.When copper mold spray to cast, mechanical pump is used respectively
Low vacuum is taken out to 10-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump and is filled with into stove
The high purity argon of 0.05MPa starts Supersonic frequency power and carries out induction melting, first in low current when molecule pump frequency is down to 0
Lower preheating, preheating time should be slightly longer, then adjust electric current, to be seen to be completely melt to alloy pig and liquid flowing is uniform,
After bubble effusion completely, spray to cast valve button is pressed, the metal liquid of high-temperature fusion is sprayed onto cooling forming in copper mold, is prepared into
To small size block amorphous alloy sample, surface has apparent metallic luster, and XRD surveys are carried out to obtained block sample
Examination, the results are shown in Figure 5, it was demonstrated that it is really full amorphous, DSC tests is carried out to obtained bulk amorphous alloy sample, as a result such as Fig. 6 institutes
Show, measures its Tg=315 DEG C, Tx=458 DEG C, Δ T=143 DEG C；
（2）Prepare large scale Zr35Ti30Be27.5Cu7.5 block amorphous alloys：Before experiment, copper mold will be used using wire cutting
Spray to cast method is prepared the block Bar samples that enough specifications are Ф 6mm ╳ 67mm and cuts into the several small of Ф 6mm ╳ 12mm
Section.Then polylith cylinder small size block amorphous alloy stacking is put into fixture.By two parts up and down of fixture to phase
The movement of negative direction prepares large-size bulk amorphous alloy to achieve the purpose that compress block amorphous alloy, this experiment is chosen
390℃（This temperature is heated to from room temperature and keep the temperature 10min with the heating speed of 20 DEG C/min）, 2MPa is as experiment condition, pressure
It is taken out after sample cooling and demolding after contracting, that is, prepares blocks of large alloy sample, XRD surveys are carried out to obtained sample
Examination, the results are shown in Figure 7, it was demonstrated that it is really non crystalline structure, DSC tests is carried out to obtained block sample, as a result such as Fig. 8 institutes
Show, measures its Tg=316 DEG C, Tx=454 DEG C, Δ T=138 DEG C maintain the wide supercooled liquid that former small size bulk amorphous alloy has substantially
The characteristic in phase section, obtained sample are 25mm in the minimum dimension of three-dimensional, have also exceeded the critical dimension of its 15mm.It is right
Obtained large-size bulk amorphous linkage interface carries out SEM scannings, as shown in Figure 9, the results showed that：Interface cohesion is close, sees
Less than gap.
The preparation of 3. large scale Zr59.1Ti1.5Cu19.7Ni9.85Al9.85 block amorphous alloys of embodiment
Pass through the full-size one of Zr59.1Ti1.5Cu19.7Ni9.85Al9.85 block amorphous alloys prepared by traditional fusion casting
As be no more than 15mm, and the size for the block amorphous alloy that the present invention prepares is apparently higher than this, and the present invention prepares large scale
The step of Zr59.1Ti1.5Cu19.7Ni9.85Al9.85 block amorphous alloys, is as follows：
（1）The preparation of amorphous powder：By high-purity powder Zr, Ti, Cu, Ni, Al according to the atomic percent in design ingredient, conversion
Dispensing is carried out at weight percent later.The raw material being mixed to get is added in ball grinder and carries out ball milling, ball material mass ratio is 2:
1, ball grinder is filled with high pure nitrogen after vacuumizing and is protected, drum's speed of rotation 600r/min, Ball-milling Time 150h.Finally
Obtain the uniform Zr59.1Ti1.5Cu19.7Ni9.85Al9.85 powder of ingredient.XRD tests and group are carried out to gained alloy powder
Knit observation, it was demonstrated that it is really non-crystaline amorphous metal, as shown in Figure 10.DSC tests are carried out to obtained amorphous sample powder, measure its Tg
=400 DEG C, Tx=492 DEG C, Δ T=92 DEG C, as shown in Figure 11；
（2）Prepare large scale Zr59.1Ti1.5Cu19.7Ni9.85Al9.85 block amorphous alloys：The amorphous powder that will be prepared
It is put into mold after weighing, then mold is put into high vacuum sintering furnace, apply the pressure of 120MPa to amorphous powder
Power, and start to vacuumize.Wait for that vacuum degree reaches 10-3It when Pa magnitudes, begins to warm up, is first heated to 390 DEG C or so with 30 DEG C/min
Heat preservation 40 minutes, keeps mold and amorphous powder temperature uniform, and being then heated to 470 degree or so with 20 DEG C/min rates keeps the temperature 60 points
Clock makes the sufficient viscous flow of non-crystaline amorphous metal, is taken out after cooling and demolding, that is, large-size bulk amorphous alloy is prepared, to obtaining
Sample carry out XRD tests, it was demonstrated that its really be non crystalline structure, as shown in figure 12.DSC tests are carried out to obtained block sample,
Measure its Tg=402 DEG C, Tx=491 DEG C, Δ T=89 DEG C, as shown in Figure 11, being wider than of maintaining that former amorphous powder has substantially are cold
The characteristic in liquid phase section, obtained sample are 20mm in the minimum dimension of three-dimensional, hence it is evident that have been more than its critical dimension.
The preparation of 4. large scale Zr41.2Ti13.8Cu12.5Ni10Be22.5 block amorphous alloys of embodiment
Pass through the full-size one of Zr41.2Ti13.8Cu12.5Ni10Be22.5 block amorphous alloys prepared by traditional fusion casting
As in 60mm, and the size for the block amorphous alloy that the present invention prepares is apparently higher than this, and the present invention prepares large scale
The step of Zr41.2Ti13.8Cu12.5Ni10Be22.5 block amorphous alloys, is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Zr, Ti, Cu, Ni, Be equal to 99.9% or more.
According to Zr41.2Ti13.8Cu12.5Ni10Be22.5 nominal composition dispensings, melted in high vacuum arc-melting furnace under argon gas protection
Refining.Use copper mold spray to cast method that enough specifications are prepared as the block Bar samples of Ф 30mm ╳ 67mm later.Copper mold spray to cast
When, use mechanical pumping low vacuum to 10 respectively-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump
And the high purity argon of 0.05MPa is filled with into stove, when molecule pump frequency is down to 0, it is molten that startup Supersonic frequency power carries out induction
Refining first preheats under low current, and preheating time should be slightly longer, then adjusts electric current, it is to be seen be completely melt to alloy pig and
Liquid flowing is uniform, after bubble effusion completely, presses spray to cast valve button, the metal liquid of high-temperature fusion is sprayed onto cold in copper mold
But it shapes, small size block amorphous alloy sample is prepared, surface has apparent metallic luster, to obtained block sample
Product carry out XRD tests, it was demonstrated that it is really full amorphous, carries out DSC tests to obtained bulk amorphous alloy sample, measures its Tg=374
DEG C, Tx=448 DEG C, Δ T=74 DEG C；
（2）Prepare large scale Zr41.2Ti13.8Cu12.5Ni10Be22.5 block amorphous alloys：It, will using wire cutting before experiment
It uses copper mold spray to cast method that enough specifications are prepared and cuts into Ф 30mm ╳ for the block Bar samples of Ф 30mm ╳ 67mm
Several segments of 60mm.Then polylith cylinder small size block amorphous alloy stacking is put into fixture.Pass through the upper of fixture
The movement of lower two parts round about, to reach the mesh that compression block amorphous alloy prepares large-size bulk amorphous alloy
, this experiment chooses 410 DEG C（This temperature is heated to from room temperature and keep the temperature 15min with the heating speed of 20 DEG C/min）, 30MPa works
For experiment condition, is taken out after the sample furnace cooling demoulding after compressing, that is, blocks of large alloy sample is prepared, to obtaining
Sample carry out XRD tests, it was demonstrated that it is really non crystalline structure, carries out DSC tests to obtained block sample, measures its Tg=376
DEG C, Tx=446 DEG C, Δ T=70 DEG C maintain the characteristic between the wide supercooling liquid phase region that former small size bulk amorphous alloy has, obtain substantially
The sample arrived is 70mm in the minimum dimension of three-dimensional, hence it is evident that has been more than its critical dimension.
The preparation of 5. large scale Ti50Ni15Cu32Sn3 block amorphous alloys of embodiment
The full-size of the Ti50Ni15Cu32Sn3 block amorphous alloys prepared by traditional fusion casting is generally in 1mm, and this hair
The size of the bright block amorphous alloy prepared is apparently higher than this, and it is non-that the present invention prepares large scale Ti50Ni15Cu32Sn3 blocks
The step of peritectic alloy, is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Ti, Cu, Ni, Sn equal to 99.9% or more.According to
Ti50Ni15Cu32Sn3 nominal composition dispensings, the melting in high vacuum arc-melting furnace under argon gas protection.Copper mold is used to spray later
The block Bar samples that enough specifications are Ф 1mm ╳ 67mm are prepared in casting.When copper mold spray to cast, use mechanical pumping low respectively
Vacuum is to 10-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump and is filled with 0.05MPa into stove
High purity argon, when molecule pump frequency is down to 0, start Supersonic frequency power carry out induction melting, first preheated under low current,
Preheating time should be slightly longer, then adjusts electric current, to be seen to be completely melt to alloy pig and liquid flowing is uniform, bubble effusion
After completely, spray to cast valve button is pressed, the metal liquid of high-temperature fusion is sprayed onto cooling forming in copper mold, small size is prepared
Block amorphous alloy sample, surface have apparent metallic luster, and XRD tests are carried out to obtained block sample, it was demonstrated that its
It is really full amorphous, DSC tests is carried out to obtained bulk amorphous alloy sample, measure its Tg=413 DEG C, Tx=486 DEG C, Δ T=73 DEG C；
（2）Prepare large scale Ti50Ni15Cu32Sn3 block amorphous alloys：Before experiment, copper mold spray to cast will be used using wire cutting
Several segments that the block Bar samples that enough specifications are Ф 1mm ╳ 67mm cut into Ф 1mm ╳ 12mm are prepared in method.So
Polylith cylinder small size block amorphous alloy stacking is put into fixture afterwards.Round about by two parts up and down of fixture
Movement, prepare large-size bulk amorphous alloy to achieve the purpose that compress block amorphous alloy, 450 DEG C of this experiment selection
（This temperature is heated to from room temperature and keep the temperature 20min with the heating speed of 20 DEG C/min）, 20MPa compresses it as experiment condition
It is taken out after sample furnace cooling demoulding afterwards, that is, prepares blocks of large alloy sample, XRD surveys are carried out to obtained sample
Examination, it was demonstrated that it is really non crystalline structure, carries out DSC tests to obtained block sample, measures its Tg=415 DEG C, Tx=484 DEG C, Δ T=
69 DEG C, the characteristic between the wide supercooling liquid phase region that former small size bulk amorphous alloy has is maintained substantially, obtained sample is in three-dimensional side
To minimum dimension be 5mm, hence it is evident that be more than its critical dimension.
The preparation of 6. large scale Cu60Hf25Ti15 block amorphous alloys of embodiment
Pass through the full-size of Cu60Hf25Ti15 block amorphous alloys prepared by traditional fusion casting（Critical dimension）Generally in 4mm
Left and right, and the size for the block amorphous alloy that the present invention prepares is apparently higher than this, the present invention prepares large scale
The step of Cu60Hf25Ti15 block amorphous alloys, is as follows：
（1）The preparation of amorphous thin ribbon：High-purity Hf, Ti, Cu bulk metal is converted to mass percent according to atomic percent
Dispensing is carried out, high vacuum arc-melting furnace melting is put into after ultrasonic cleaning.It breaks into melted master alloy ingot into pieces fritter, beats
It after mill cleaning, weighs certain mass and is put into the quartz ampoule of certain specification, quartz ampoule, which is then put into copper roller, revolves quenching vacuum furnace
In room, after the position for regulating quartz ampoule and induction coil, starts to take out low vacuum and high vacuum successively, wait for that vacuum degree reaches
3.5╳10-3When Pa, high-purity argon gas to the air pressure that 99.999% is filled with into vacuum container reaches 0.05MPa, then proceeds by
Get rid of band.The rotating speed of copper roller is 1900rpm when getting rid of band, and quartz ampoule nozzle is 2 ~ 3mm apart from roll surface distance.First under low induced current
It is preheated, then quickly heats up to high current, after waiting for that melt is completely melt, reduced induced current and keep the temperature a period of time,
When melt flows are steady, start to get rid of band, XRD tests is carried out to obtained Tape samples, it was demonstrated that it is really full amorphous, to obtaining
Tape samples carry out DSC tests, measure its Tg=472 DEG C, Tx=532 DEG C, Δ T=60 DEG C；
（2）Prepare large scale Cu60Hf25Ti15 block amorphous alloys：Ready amorphous thin ribbon is weighed and is cleaned after drying
It is put into mold, then mold is put into high vacuum soldering oven, apply the pressure of 110MPa to amorphous thin ribbon, and start to take out
Vacuum.Wait for that vacuum degree reaches 10-3When Pa magnitudes, begin to warm up, being first heated to 465 DEG C or so with 30 DEG C/min keeps the temperature 30 minutes,
Keep mold and amorphous thin ribbon temperature uniform, then 20 DEG C/min rates are heated to 500 DEG C or so and keep the temperature 40 minutes, make non-crystaline amorphous metal
Sufficient viscous flow, takes out after furnace cooling, that is, prepares blocks of large alloy sample, and XRD is carried out to obtained sample
Test, it was demonstrated that it is really non crystalline structure, carries out DSC tests to obtained block sample, measures its Tg=473 DEG C, Tx=530 DEG C, Δ
T=57 DEG C maintain the characteristic between the wide supercooling liquid phase region that former amorphous thin ribbon has substantially, and obtained sample is in three-dimensional
Minimum dimension is 10mm, hence it is evident that has been more than its critical dimension.
The preparation of 7. large scale Ni45Ti20Zr23Al12 block amorphous alloys of embodiment
The full-size of the Ni45Ti20Zr23Al12 block amorphous alloys prepared by traditional fusion casting is generally less than 0.5mm,
And the size for the block amorphous alloy that the present invention prepares is apparently higher than this, the present invention prepares large scale Ni45Ti20Zr23Al12
The step of block amorphous alloy, is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Ti, Zr, Ni, Al equal to 99.9% or more.According to
Ni45Ti20Zr23Al12 nominal composition dispensings, the melting in high vacuum arc-melting furnace under argon gas protection.Copper mold is used later
The block Bar samples that enough specifications are Ф 0.3mm ╳ 67mm are prepared in spray to cast method.When copper mold spray to cast, mechanical pump is used respectively
Low vacuum is taken out to 10-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump and is filled with into stove
The high purity argon of 0.05MPa starts Supersonic frequency power and carries out induction melting, first in low current when molecule pump frequency is down to 0
Lower preheating, preheating time should be slightly longer, then adjust electric current, to be seen to be completely melt to alloy pig and liquid flowing is uniform,
After bubble effusion completely, spray to cast valve button is pressed, the metal liquid of high-temperature fusion is sprayed onto cooling forming in copper mold, is prepared into
To small size block amorphous alloy sample, surface has apparent metallic luster, and XRD surveys are carried out to obtained block sample
Examination, it was demonstrated that it is really full amorphous, carries out DSC tests to obtained bulk amorphous alloy sample, measures its Tg=510 DEG C, Tx=559 DEG C, Δ
T=49℃；
（2）Prepare large scale Ni45Ti20Zr23Al12 block amorphous alloys：Before experiment, copper mold spray to cast will be used using wire cutting
Method is prepared the block Bar samples that enough specifications are Ф 0.3mm ╳ 67mm and cuts into the several small of Ф 0.3mm ╳ 12mm
Section.Then polylith cylinder small size block amorphous alloy stacking is put into fixture.By two parts up and down of fixture to phase
The movement of negative direction prepares large-size bulk amorphous alloy to achieve the purpose that compress block amorphous alloy, this experiment is chosen
530℃（This temperature is heated to from room temperature and keep the temperature 0.5min with the heating speed of 20 DEG C/min）, 15MPa as experiment condition,
It is taken out after sample furnace cooling demoulding after compression, that is, prepares blocks of large alloy sample, obtained sample is carried out
XRD is tested, it was demonstrated that it is really non crystalline structure, carries out DSC tests to obtained block sample, measures its Tg=511 DEG C, Tx=558
DEG C, Δ T=47 DEG C maintain the characteristic between the wide supercooling liquid phase region that former small size bulk amorphous alloy has substantially, and obtained sample exists
The minimum dimension of three-dimensional is 2mm, hence it is evident that has been more than its critical dimension.
The preparation of 8. large scale Fe60Ni7.5Mo7.5P10C10B5 block amorphous alloys of embodiment
The full-size of the Fe60Ni7.5Mo7.5P10C10B5 block amorphous alloys prepared by traditional fusion casting is generally 4mm
, and the size for the block amorphous alloy that the present invention prepares is apparently higher than this, the present invention prepares large scale
The step of Fe60Ni7.5Mo7.5P10C10B5 block amorphous alloys, is as follows：
（1）The preparation of amorphous powder：By required high-purity powder according to the atomic percent in design ingredient, it is converted to weight percent
Dispensing is carried out than later.The raw material being mixed to get is added in ball grinder and carries out ball milling, ball material mass ratio is 2:1, ball grinder is taken out
It is filled with high pure nitrogen after vacuum to be protected, drum's speed of rotation 600r/min, Ball-milling Time 150h.It is equal to finally obtain ingredient
Even Fe60Ni7.5Mo7.5P10C10B5 powder.XRD tests and structure observation are carried out to gained alloy powder, it was demonstrated that it is really
Non-crystaline amorphous metal.DSC tests are carried out to obtained amorphous sample powder, measure its Tg=454 DEG C, Tx=551 DEG C, Δ T=97 DEG C；
（2）Prepare large scale Fe60Ni7.5Mo7.5P10C10B5 block amorphous alloys：The amorphous powder prepared is weighed it
After be put into mold, then mold is put into high vacuum soldering oven, applies the pressure of 90MPa to amorphous powder, and opens
Beginning vacuumizes.Wait for that vacuum degree reaches 10-3It when Pa magnitudes, begins to warm up, being first heated to 449 DEG C or so with 30 DEG C/min keeps the temperature 40 points
Clock keeps mold and amorphous powder temperature uniform, and being then heated to 500 DEG C or so with 20 DEG C/min rates keeps the temperature 45 minutes, makes non-
The sufficient viscous flow of peritectic alloy, takes out after furnace cooling, that is, prepares large-size bulk amorphous alloy, to obtained sample into
Row XRD tests, it was demonstrated that it is really non crystalline structure.DSC tests are carried out to obtained block sample, measure its Tg=456 DEG C, Tx=550
DEG C, Δ T=94 DEG C maintain the characteristic between the wide supercooling liquid phase region that former amorphous powder has substantially, and obtained sample is in three-dimensional side
To minimum dimension be 8mm, hence it is evident that be more than its critical dimension.
The preparation of 9. large scale Al86Y4.5Ni7Co1La1.5 block amorphous alloys of embodiment
The full-size of the Al86Y4.5Ni7Co1La1.5 block amorphous alloys prepared by traditional fusion casting is 1mm, and this hair
The size of the bright block amorphous alloy prepared is apparently higher than this, and the present invention prepares large scale Al86Y4.5Ni7Co1La1.5 blocks
The step of body non-crystaline amorphous metal, is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Al, Ni, Y, Co, La equal to 99.9% or more.It presses
According to Al86Y4.5Ni7Co1La1.5 nominal composition dispensings, the melting in high vacuum arc-melting furnace under argon gas protection.It uses later
The block Bar samples that enough specifications are Ф 1mm ╳ 67mm are prepared in copper mold spray to cast method.When copper mold spray to cast, machinery is used respectively
Pumping low vacuum is to 10-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump and is filled with into stove
The high purity argon of 0.05MPa starts Supersonic frequency power and carries out induction melting, first in low current when molecule pump frequency is down to 0
Lower preheating, preheating time should be slightly longer, then adjust electric current, to be seen to be completely melt to alloy pig and liquid flowing is uniform,
After bubble effusion completely, spray to cast valve button is pressed, the metal liquid of high-temperature fusion is sprayed onto cooling forming in copper mold, is prepared into
To small size block amorphous alloy sample, surface has apparent metallic luster, and XRD surveys are carried out to obtained block sample
Examination, it was demonstrated that it is really full amorphous, carries out DSC tests to obtained bulk amorphous alloy sample, measures its Tg=231 DEG C, Tx=246 DEG C, Δ
T=15℃；
（2）Prepare large scale Al86Y4.5Ni7Co1La1.5 block amorphous alloys：Before experiment, copper mold will be used using wire cutting
Spray to cast method is prepared the block Bar samples that enough specifications are Ф 1mm ╳ 67mm and cuts into the several small of Ф 1mm ╳ 12mm
Section.Then polylith cylinder small size block amorphous alloy stacking is put into fixture.By two parts up and down of fixture to phase
The movement of negative direction prepares large-size bulk amorphous alloy to achieve the purpose that compress block amorphous alloy, this experiment is chosen
238℃（This temperature is heated to from room temperature and keep the temperature 0.7min with the heating speed of 10 DEG C/min）, 25MPa as experiment condition,
It is taken out after sample furnace cooling demoulding after compression, that is, prepares blocks of large alloy sample, obtained sample is carried out
XRD is tested, it was demonstrated that it is really non crystalline structure, carries out DSC tests to obtained block sample, measures its Tg=233 DEG C, Tx=245
DEG C, Δ T=12 DEG C maintain the characteristic between the wide supercooling liquid phase region that former small size bulk amorphous alloy has substantially, and obtained sample exists
Three-dimensional put to minimum dimension be 2mm, hence it is evident that be more than its critical dimension.
The preparation of 10. large scale Co62Nb8B30 block amorphous alloys of embodiment
The full-size of the Co62Nb8B30 block amorphous alloys prepared by traditional fusion casting is generally 2mm or so, and this hair
The size of the bright block amorphous alloy prepared is apparently higher than this, and the present invention prepares large scale Co62Nb8B30 block amorphous alloys
The step of it is as follows：
（1）The preparation of amorphous powder：By required high-purity powder according to the atomic percent in design ingredient, it is converted to weight percent
Dispensing is carried out than later.The raw material being mixed to get is added in ball grinder and carries out ball milling, ball material mass ratio is 2:1, ball grinder is taken out
It is filled with high pure nitrogen after vacuum to be protected, drum's speed of rotation 600r/min, Ball-milling Time 150h.It is equal to finally obtain ingredient
Even Co62Nb8B30 powder.XRD tests and structure observation are carried out to gained alloy powder, it was demonstrated that it is really non-crystaline amorphous metal.It is right
Obtained amorphous sample powder carries out DSC tests, measures its Tg=622 DEG C, Tx=662 DEG C, Δ T=40 DEG C；
（2）Prepare large scale Co62Nb8B30 block amorphous alloys：It is put into mold after the amorphous powder prepared is weighed
In, then mold is put into high vacuum soldering oven, applies the pressure of 46MPa to amorphous powder, and starts to vacuumize.It waits for true
Reciprocal of duty cycle reaches 10-3It when Pa magnitudes, begins to warm up, being first heated to 610 DEG C or so with 30 DEG C/min keeps the temperature 40 minutes, makes mold and non-
Brilliant powder temperature is uniform, and being then heated to 640 degree or so with 20 DEG C/min rates keeps the temperature 5 minutes, and non-crystaline amorphous metal is made adequately to glue
It remains in a standstill dynamic, is taken out after furnace cooling, that is, prepare large-size bulk amorphous alloy, XRD tests are carried out to obtained sample, it was demonstrated that
It is really non crystalline structure.DSC tests are carried out to obtained block sample, measure its Tg=623 DEG C, Tx=661 DEG C, Δ T=38 DEG C, base
Originally the characteristic between the wide supercooling liquid phase region that former amorphous powder has is maintained, obtained sample is in the minimum dimension of three-dimensional
4mm, hence it is evident that be more than its critical dimension.
The preparation of 11. large scale Mg65Cu20Zn5Y10 block amorphous alloys of embodiment
The full-size of the Mg65Cu20Zn5Y10 block amorphous alloys prepared by traditional fusion casting is 6mm, and system of the present invention
Size for the block amorphous alloy gone out is apparently higher than this, and the present invention prepares large scale Mg65Cu20Zn5Y10 block amorphous alloys
The step of it is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Mg, Cu, Zn, Y equal to 99.9% or more.According to
Mg65Cu20Zn5Y10 nominal composition dispensings, the melting in high vacuum arc-melting furnace under argon gas protection.Copper mold is used to spray later
The block Bar samples that enough specifications are Ф 6mm ╳ 67mm are prepared in casting.When copper mold spray to cast, use mechanical pumping low respectively
Vacuum is to 10-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump and is filled with 0.05MPa into stove
High purity argon, when molecule pump frequency is down to 0, start Supersonic frequency power carry out induction melting, first preheated under low current,
Preheating time should be slightly longer, then adjusts electric current, to be seen to be completely melt to alloy pig and liquid flowing is uniform, bubble effusion
After completely, spray to cast valve button is pressed, the metal liquid of high-temperature fusion is sprayed onto cooling forming in copper mold, small size is prepared
Block amorphous alloy sample, surface have apparent metallic luster, and XRD tests are carried out to obtained block sample, it was demonstrated that its
It is really full amorphous, DSC tests is carried out to obtained bulk amorphous alloy sample, measure its Tg=131 DEG C, Tx=183 DEG C, Δ T=52 DEG C；
（2）Prepare large scale Mg65Cu20Zn5Y10 block amorphous alloys：Before experiment, copper mold spray to cast method will be used using wire cutting
Several segments that the block Bar samples that enough specifications are Ф 6mm ╳ 67mm cut into Ф 6mm ╳ 12mm are prepared.Then
Polylith cylinder small size block amorphous alloy stacking is put into fixture.Round about by two parts up and down of fixture
It is mobile, large-size bulk amorphous alloy is prepared to achieve the purpose that compress block amorphous alloy, this experiment chooses 160 DEG C（With
The heating speed of 10 DEG C/min is heated to this temperature from room temperature and keeps the temperature 0.6min）, 16MPa is as experiment condition, after compression
Sample furnace cooling demoulding after take out, that is, prepare blocks of large alloy sample, XRD tests carried out to obtained sample,
It is non crystalline structure to confirm it really, carries out DSC tests to obtained block sample, its T can be obtainedg=133 DEG C, Tx=182 DEG C, Δ T=
49 DEG C, the characteristic between the wide supercooling liquid phase region that former small size bulk amorphous alloy has is maintained substantially, and obtained sample is put in three-dimensional
To minimum dimension be 9mm, hence it is evident that be more than its critical dimension.
The preparation of 12. large scale Au49Ag5.5Pd2.3Cu26.9Si16.3 block amorphous alloys of embodiment
The full-size of the Au49Ag5.5Pd2.3Cu26.9Si16.3 block amorphous alloys prepared by traditional fusion casting is
5mm, and the size for the block amorphous alloy that the present invention prepares is apparently higher than this, the present invention prepares large scale
The step of Au49Ag5.5Pd2.3Cu26.9Si16.3 block amorphous alloys, is as follows：
（1）The preparation of small size block amorphous alloy：Purity is selected to be all higher than Au, Ag, Pd, Cu, Si equal to 99.9% or more.
According to Au49Ag5.5Pd2.3Cu26.9Si16.3 nominal composition dispensings, melted in high vacuum arc-melting furnace under argon gas protection
Refining.Use copper mold spray to cast method that enough specifications are prepared as the block Bar samples of Ф 5mm ╳ 67mm later.Copper mold spray to cast
When, use mechanical pumping low vacuum to 10 respectively-1Pa magnitudes, with molecular pump pumping high vacuum to 3.5 ╳ 10-3Pa closes molecular pump
And the high purity argon of 0.05MPa is filled with into stove, when molecule pump frequency is down to 0, it is molten that startup Supersonic frequency power carries out induction
Refining first preheats under low current, and preheating time should be slightly longer, then adjusts electric current, it is to be seen be completely melt to alloy pig and
Liquid flowing is uniform, after bubble effusion completely, presses spray to cast valve button, the metal liquid of high-temperature fusion is sprayed onto cold in copper mold
But it shapes, small size block amorphous alloy sample is prepared, surface has apparent metallic luster, to obtained block sample
Product carry out XRD tests, it was demonstrated that it is really full amorphous, carries out DSC tests to obtained bulk amorphous alloy sample, measures its Tg=128
DEG C, Tx=186 DEG C, Δ T=58 DEG C；
（2）Prepare large scale Au49Ag5.5Pd2.3Cu26.9Si16.3 block amorphous alloys：Before experiment, it will be adopted using wire cutting
The block Bar samples that enough specifications are Ф 5mm ╳ 67mm are prepared with copper mold spray to cast method and cut into Ф 5mm ╳ 12mm
Several segments.Then polylith cylinder small size block amorphous alloy stacking is put into fixture.Pass through two up and down of fixture
Divide movement round about, large-size bulk amorphous alloy, this reality are prepared to achieve the purpose that compress block amorphous alloy
Test 155 DEG C of selection（This temperature is heated to from room temperature and keep the temperature 0.8min with the heating speed of 10 DEG C/min）, 36MPa is as experiment
Condition is taken out after the sample furnace cooling demoulding after compressing, that is, blocks of large alloy sample is prepared, to obtained sample
Carry out XRD tests, it was demonstrated that it is really non crystalline structure, carries out DSC tests to obtained block sample, its T can be obtainedg=129 DEG C, Tx
=184 DEG C, Δ T=55 DEG C maintain the characteristic between the wide supercooling liquid phase region that former small size bulk amorphous alloy has, obtained sample substantially
Product three-dimensional put to minimum dimension be 8mm, hence it is evident that be more than its critical dimension.
Claims (7)
1. the preparation method of large-size bulk amorphous alloy, which is characterized in that will be placed by getting rid of the amorphous thin ribbon prepared with method
In in mold, it is heated at a certain temperature in supercooled liquid phase section with the heating speed of 10 ~ 30 DEG C/min, heat preservation 0.5min ~
60min carries out thermoplasticity compression, then Slow cooling under the pressure of 2 ~ 200MPa, you can obtains the blocks of large
Non-crystaline amorphous metal.
2. the preparation method of large-size bulk amorphous alloy, which is characterized in that the non-crystalline flour that will be prepared by atomization or ball-milling method
End is positioned in mold, is heated at a certain temperature in supercooled liquid phase section with the heating speed of 10 ~ 30 DEG C/min, heat preservation
0.5min ~ 60min carries out thermoplasticity compression, then Slow cooling under the pressure of 2 ~ 200MPa, you can obtains the big ruler
Very little block amorphous alloy.
3. the preparation method of large-size bulk amorphous alloy, which is characterized in that the small size block prepared by fusion casting is non-
Peritectic alloy is positioned in mold, is heated at a certain temperature in supercooled liquid phase section with the heating speed of 10 ~ 30 DEG C/min, is protected
Warm 0.5min ~ 60min carries out thermoplasticity compression, then Slow cooling under the pressure of 2 ~ 200MPa, you can big described in obtaining
Dimensioned blocks non-crystaline amorphous metal.
4. preparation method as described in claim 1, which is characterized in that amorphous thin ribbon is zirconium base, titanium-based, copper-based, Ni-based, iron
Base, aluminium base, cobalt-based, magnesium-based or auri amorphous any one.
5. preparation method as claimed in claim 2, which is characterized in that amorphous powder is zirconium base, titanium-based, copper-based, Ni-based, iron
Base, aluminium base, cobalt-based, magnesium-based or auri amorphous any one.
6. preparation method as claimed in claim 3, which is characterized in that small size block amorphous alloy system be zirconium base, titanium-based,
Copper-based, Ni-based, iron-based, aluminium base, cobalt-based, magnesium-based or auri amorphous any one.
7. preparation method as described in any one of claims 1-3, which is characterized in that mold uses steel mold or copper mould.
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