CN102021501A - Method for improving forming ability and strength of amorphous alloy by controlling solidifying condition - Google Patents
Method for improving forming ability and strength of amorphous alloy by controlling solidifying condition Download PDFInfo
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- CN102021501A CN102021501A CN200910187388XA CN200910187388A CN102021501A CN 102021501 A CN102021501 A CN 102021501A CN 200910187388X A CN200910187388X A CN 200910187388XA CN 200910187388 A CN200910187388 A CN 200910187388A CN 102021501 A CN102021501 A CN 102021501A
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 23
- 239000000956 alloy Substances 0.000 claims abstract description 26
- 239000010949 copper Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 238000005266 casting Methods 0.000 claims abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004512 die casting Methods 0.000 claims abstract description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 25
- 230000015572 biosynthetic process Effects 0.000 claims description 16
- 239000005300 metallic glass Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005275 alloying Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- 238000002083 X-ray spectrum Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910018054 Ni-Cu Inorganic materials 0.000 description 2
- 229910018481 Ni—Cu Inorganic materials 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229910015365 Au—Si Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005339 levitation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a preparation technology of block amorphous alloy, in particular to a method for improving the forming ability and strength of amorphous alloy by controlling solidifying condition. The method has low process cost, is simple and easy, can obviously strengthen the forming ability of block amorphous alloy and improve the material strength and is suitable for a majority of amorphous systems. The casting is carried out when the preheating temperature of a die reaches 353-393K by adjusting the preheating temperature of the die through adopting a copper die casting method and the amorphous forming ability can be improved so that the amorphous alloy in a larger size can be obtained; meanwhile, the strength of an amorphous alloy material is improved by 4-18 percent. The invention develops a novel method for improving the forming ability of the block amorphous alloy, confirms a novel process parameter for producing the block amorphous alloy in larger size and improving the strength and broadens the application field of the block amorphous alloy.
Description
Technical field
The present invention relates to the technology of preparing of block amorphous alloy, be specially a kind of method that improves non-crystaline amorphous metal formation ability and intensity by the control curing condition.
Background technology
People such as nineteen sixty U.S. professor Duwez adopt the melt supercooled method at first to make Au-Si series non-crystalline state alloy, but the preparation of traditional non-crystaline amorphous metal need surpass 10
6The high speed of cooling of K/s, and thickness or diameter generally all be no more than 50 μ m, limited greatly in actual application in engineering.Since 1988, be that the study group of representative takes the lead in developing three-dimensional dimension and all reaches block amorphous alloy more than the 1mm, comprise numerous systems such as La base, Mg base, Zr base, Pd base, Ti base, Fe base and Cu base with Japanese Inoue professor and U.S. professor Johnson.The block amorphous alloy of this class multicomponent has very strong amorphous formation ability, and its critical cooling rate is more much lower than traditional non-crystaline amorphous metal, generally all is no more than 10
3The K/s magnitude.
Because have the atomic arrangement structure of unique unordered short range order of long-range, non-crystaline amorphous metal has some excellent use propertieies, for example: high strength, high elastic limit and excellent corrosion resisting performance or the like.But some application with non-crystaline amorphous metal system of excellent properties still are subjected to the restriction of size, such as Ni base amorphous.Simultaneously, when the amorphous formation ability of alloy hour, the material property stability of preparing is poorer, these are all restricting the practical application of non-crystalline material.Except optimizing the alloy constituent element, another main path that improves amorphous formation ability is exactly the improvement of processing condition, comprise vacuum melting repeatedly and purify melt, the improvement technology is for example utilized magnetic levitation melting and the Manifold technology that falls, and improves casting process and mould or the like.Obviously, compare, improve amorphous formation ability by improvement and seem more simple and easy to do casting process with other approach.
In conventional cast, improving die temperature is to improve casting quality, improves the method a kind of commonly used of cast properties.Do not go but it is applied in the preparation of non-crystaline amorphous metal, because non-crystaline amorphous metal prepares the quick or inferior rapid solidification of general requirement, cooling time is extremely short, and the time that influences each other between mould and foundry goods is also extremely short.In fact, in utmost point short period of time rapid solidification, generally have air film as thin as a wafer between melt that is molded into cold mould and mould, it can influence the interface heat transfer between melt and the mould.The raising of die temperature helps improving the wettability between liquid alloy and the mould inner wall, lowers thermal contact resistance, improves heat exchanger effectiveness.
In recent years, people are obtaining numerous achievements aspect the larger sized block amorphous alloy of preparation, but much all are based on the optimization of alloying constituent, and the experimental summary by a large amount of heterogeneity points comes, and tests consume significant; Not only be simple and easy to implement and improve amorphous formation ability, and can be referred from the non-crystaline amorphous metal suitability for industrialized production in future by improvement to the traditional preparation process method.Therefore, a kind of raising block amorphous alloy with certain ubiquity of development forms the significant and practical value of method of ability.
Summary of the invention
The object of the present invention is to provide and a kind ofly improve the method that block amorphous alloy forms ability by the control curing condition, this method technology cost is low and simple and easy to do, can obviously improve the formation ability of block amorphous alloy.Can also improve simultaneously the intensity of non-crystaline amorphous metal, its compressed rupture strength improves 4%～18%.
Technical scheme of the present invention is:
A kind of method that improves block amorphous alloy formation ability and intensity by the control curing condition, adopt copper mold to cast and prepare the block amorphous alloy sample, mould and die preheating to 353K between the 393K, improve heat exchange and the wettability of alloy liquid between mould inner wall by the control curing condition, form the non-crystal structure of the homogeneous that no crystalline state separates out mutually.The concrete processing parameter of copper mold casting is as follows: vacuum tightness 10
-2～10
-4Pa, the alloy melt temperature is that liquidus temperature adds 300K, speed of cooling 1～10
2K/s.
The mechanical performance index of prepared block amorphous alloy is as follows:
Compare with the sample of the same composition of room temperature die casting preparation, compressed rupture strength improves 4%～18%.
The mechanism of improving non-crystaline amorphous metal formation ability and intensity method provided by the invention is:
The present invention can improve heat transfer and the wettability between mould and the alloy.When the copper mold preheating temperature when 353K is between 393K; gas on the copper mold inwall (such as protective gas such as argon gas) adsorptive capacity reduces significantly; help the discharge of the gas blanket between alloy liquation and the inner chamber; cause thermal contact resistance between the two to reduce; heat conducting efficient improves; the speed of cooling of alloy liquid improves, and helps amorphous and forms.In the non-crystaline amorphous metal that makes under the higher speed of cooling, do not have the formation that can easily bring out multiple shear bands and hinder the microstructure of shear zone expansion, such as even dispersion distribute nanocrystalline, not yielding, thereby intensity is higher.Simultaneously, the minimizing of the adsorptive capacity of argon gas and the rapid condition of surface that helps improving the non-crystaline amorphous metal foundry goods of discharging on the copper mold inwall.In addition, along with the raising of die temperature, the surface free energy of mould inner surface improves, and helps wetting between alloy liquid and the mould, and is can be apace wetting and sprawl at mould inner wall.Alloy melt fill type more rapidly and closely knit, casting flaw obviously reduces, this also is one of reason of improving of sample compressed rupture strength.
The present invention has the following advantages:
1. the present invention has adopted the copper mold casting process by the control die temperature, and cost is low and simple and easy to do.
2. the present invention can be suitable for most of block amorphous alloy systems, as Zr base, Cu base, Ti base etc., can suppress the generation of crystal phase in the process of setting by the inventive method, form the non-crystal structure of homogeneous, improve the formation ability of block amorphous alloy, promoted the application of the alloy system that some amorphous formation abilities are weak.
3. the inventive method can also more obviously improve the intensity of material when improving amorphous formation ability.
Description of drawings
Fig. 1 a b is the Zr of preparation under the different mold preheating temperatures
64.9Al
7.9Ni
10.7Cu
16.5(Fig. 1 a) and DSC curve (Fig. 1 b) for the X-ray spectrum of sample.
Fig. 2 is the Zr of preparation under the different mold preheating temperatures
64.9Al
7.9Ni
10.7Cu
16.5The scanning of sample and transmission electron microscope photo.
Fig. 3 is the Zr of preparation under the different mold preheating temperatures
64.9Al
7.9Ni
10.7Cu
16.5The sample compressive stress strain curve.
Fig. 4 is the Zr of preparation under the different mold preheating temperatures
47Cu
37.5Ag
7.5Al
8The X-ray spectrum of sample.
Embodiment
The present invention is described in detail in detail by the following examples.
Embodiment 1
The alloy of selecting is Zr-Al-Ni-Cu, and concrete composition is: 64.9%Zr, 7.9%Al, 10.7%Ni, 16.5%Cu (atomic percent).
The smelting process of Zr-Al-Ni-Cu mother alloy is a routine techniques among the present invention, the present embodiment mother alloy smelt concrete processing parameter and process as follows: used starting material are respectively Zr, Al, Ni, Cu high pure metal (purity is not less than 99.9wt.%); Master alloy ingot adopts arc melting, at first working chamber is evacuated to 10-2～10-4Pa, and then feeding high-purity argon gas (purity is 99.99wt.%) carries out melting; Before the molten alloy,, form the dividing potential drop that titanium oxide further reduces oxygen in the working chamber by oxidizing reaction at first with Ti ingot metal fusing, for the composition that guarantees alloy cast ingot even as far as possible, melting 3～5 times that all need to overturn of each alloy pig; Master alloy ingot is broken into fritter, has aperture below the mother alloy of certain mass is put into and (behind the silica tube in aperture 1～1.5mm), working chamber is evacuated to 10
-2～10
-4Pa carries out induction melting again.Control alloy melt temperature adds 300K to liquidus temperature, and the copper mold under with high-purity argon gas the alloy melt in the silica tube being sprayed into obtains different diameter cylinder shape sample, speed of cooling 1～10
2K/s.Before casting, the temperature of control mould keeps treating in 10～15 minutes can casting after die temperature is stablized to the experiment assigned temperature earlier.Sample structure with X ray, differential scanning calorimetric analysis, scanning electron microscope and the different die temperatures of TEM (transmission electron microscope) analysis, as can be known when die temperature is lower than 353K and is higher than 393K, though in the X ray accuracy rating, be characterized by complete amorphous, the contrast of also not having obvious crystalline state phase in scanned photograph, but under transmission electron microscope, can find the crystalline state phase of 100nm magnitude in the noncrystal substrate part, the crystallization enthalpy of the DSC curve calculation of comparing simultaneously, the crystallization enthalpy of sample that die temperature is controlled at 353K casting is higher, has shown that the crystalline state phase content of material is few.The room temperature compression testing shows that the amorphous sample that this alloying constituent obtains all shows the brittle rupture feature of typical block amorphous alloy, and plastix strain is very little.The inventive method is little to the influence of compression plasticity, but is to a certain degree all strengthening compressive strength, and enhancing amplitude from 4% to 18% does not wait.
Fig. 1 a-b is the Zr of preparation under the different mold preheating temperatures
64.9Al
7.9Ni
10.7Cu
16.5(Fig. 1 a) and DSC curve (Fig. 1 b) for the X-ray spectrum of sample.When preparing diameter as can be seen and being the sample of 5mm, only the die temperature sample that is controlled at 353K and 393K preparation shows as complete amorphous.The DSC curve has typical non-crystal structure feature, and by calculating the crystallization enthalpy, the crystallization enthalpy of sample that die temperature is controlled at the 353K casting is higher, and the crystalline state phase content that has shown material still less.
Fig. 2 a is the stereoscan photograph of die temperature 353K, forms typical pure amorphous as can be seen, and other die temperatures are more or less the same therewith.Fig. 2 b-d is the transmission electron microscope photo of the sample of preparation under the different mold preheating temperatures, only the no obvious crystalline state phase of die temperature 353K preparation.
Fig. 3 be under the different mold preheating temperatures preparation sample stress under compression strain curve, as can be seen die temperature is brought up to 353K after, to a certain degree strengthening compressive strength, enhancing amplitude from 4% to 18% does not wait.
Embodiment 2
Difference from Example 1 is:
Alloying constituent is 47%Zr, 37.5%Cu, 7.5%Ag, 8%Al (atomic percent).The concrete processing parameter of copper mold casting is as follows: vacuum tightness 10-2～10-4Pa, cooling rate speed 1～10
2K/s, die temperature is preheating to 353K.As can be seen from Figure 4, the X ray crystalline state peak of the sample of die temperature 353K preparation obviously weakens, and is complete amorphous basically, illustrates that amorphous formation ability strengthens.The room temperature compressed rupture strength is 2159～2228MPa simultaneously, than sample (2073MPa) raising 4%～8% of room temperature mould preparation.
Embodiment 3
Difference from Example 1 is:
Alloying constituent is 62%Zr, 15.4%Cu, 12.6%Ni, 10%Al (atomic percent).The concrete processing parameter of copper mold casting is as follows: vacuum tightness 10
-2～10
-4Pa, cooling rate speed 1～10
2K/s, die temperature is preheating to 353K.The amorphous formation ability of the sample of die temperature 353K preparation strengthens.The sample of compressed rupture strength average specific room temperature mould preparation simultaneously improves 7.4%.
Claims (3)
1. one kind is passed through the method that the control curing condition improves non-crystaline amorphous metal formation ability and intensity, it is characterized in that, utilize copper mold casting, improve heat exchange and wettability between alloy liquid and the mould inner wall, form the non-crystal structure of the homogeneous that no crystalline state separates out mutually by the control curing condition; When adopting copper mold casting preparation block amorphous alloy sample, the preheating temperature of its mould remains between the 353K to 393K.
2. in accordance with the method for claim 1, it is characterized in that the copper mold concrete processing parameter of casting is as follows: vacuum tightness 10
-2～10
-4Pa, the alloy melt temperature is that liquidus temperature adds 300K, speed of cooling 1～10
2K/s.
3. in accordance with the method for claim 1, it is characterized in that prepared composite materials property index is as follows: compare compressed rupture strength σ with the sample of the same composition of room temperature die casting preparation
fImprove 4%～18%.
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| CN101314838B (en) * | 2007-05-30 | 2012-05-30 | 中国科学院金属研究所 | Zr-Cu-Ni-Al-Ag alloy with higher amorphous forming ability and production method thereof |
| CN101347830A (en) * | 2007-07-18 | 2009-01-21 | 中国科学院金属研究所 | Method for improving massive amorphous alloy plasticity by controlling solidification condition |
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Effective date of registration: 20160128 Address after: 110013 room 155-5, Chuangxin Road, Dongling District, Liaoning, Shenyang, 619 Patentee after: Liaoning Jinyan liquid metal Technology Co. Ltd. Address before: 110016 Shenyang, Liaoning Province Cultural Road, No. 72, Shenhe Patentee before: Institute of metal research, Chinese Academy of Sciences |
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Effective date of registration: 20180424 Address after: 110013 room 155-5, Chuangxin Road, Dongling District, Liaoning, Shenyang, 619 Co-patentee after: Shenyang new metal material preparation technology Co. Ltd. Patentee after: Liaoning Jinyan liquid metal Technology Co. Ltd. Address before: 110013 room 155-5, Chuangxin Road, Dongling District, Liaoning, Shenyang, 619 Patentee before: Liaoning Jinyan liquid metal Technology Co. Ltd. |
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