CN101586221A - Copper-zirconium base amorphous alloy and preparation method thereof - Google Patents
Copper-zirconium base amorphous alloy and preparation method thereof Download PDFInfo
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- CN101586221A CN101586221A CNA2008101001203A CN200810100120A CN101586221A CN 101586221 A CN101586221 A CN 101586221A CN A2008101001203 A CNA2008101001203 A CN A2008101001203A CN 200810100120 A CN200810100120 A CN 200810100120A CN 101586221 A CN101586221 A CN 101586221A
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Abstract
The invention provides a copper-zirconium base amorphous alloy. The copper-zirconium base amorphous alloy comprises the components of the following general formula: CuaZrbTic, wherein a, b and c are all atomic percent, a is not less than 45 but not more than 55, b is not less than 35 but not more than 50, c is not less than 5 but not more than 15, and the summation of a, b and c is 100. The copper-zirconium base amorphous alloy has good plastic nature, large critical dimension, and favorable compression fracture strength and vickers hardness.
Description
Technical field
The present invention relates to a kind of Alloy And Preparation Method, relate in particular to a kind of copper-zirconium-base amorphous alloy and preparation method thereof.
Background technology
Non-crystaline amorphous metal is that the composed atom arrangement is not periodically and a symmetric class novel alloy material.Because its special microtexture, cause them to have superior mechanics, physics, chemistry and magnetic property, as high strength, high rigidity, performance such as wear-resistant, corrosion-resistant.These superior performances make non-crystaline amorphous metal have application potential in a lot of fields.
Since earlier 1990s, headed by the Japan and the U.S., a series of alloying constituents have been found with strong amorphous formation ability, wherein make the most easily with zirconium-base amorphous alloy, its critical cooling rate is in the 1K/s magnitude, can cast and method such as shrend is prepared into three-dimensional block materials with copper mold.Recently, developed multicomponent Cu-based bulk body amorphous alloy abroad again, with respect to non-crystaline amorphous metals such as zirconium base, palladium bases, Cu-based bulk body non-crystaline amorphous metal has cheaper price and more practical value, but the amorphous formation ability of Cu-based bulk body non-crystaline amorphous metal is relatively poor.
For the problem of the amorphous formation ability difference that solves cu-based amorphous alloys and the intensity that further improves cu-based amorphous alloys, CN 1594639A discloses the series bulk amorphous alloy of a kind of Cu base Cu-Zr-Ti, and the general formula of this alloy is (Cu
xZr
1-x)
1-yTi
y, wherein, the span of x is 54at%≤x≤70at%, the span of y is 2at%≤y≤20.And the composition of this alloy amorphous formation ability the best is Cu
64Zr
28.5Ti
7.5And this invention has partly provided the performance measurement parameter of following general formula: Cu at embodiment
64Zr
28.5Ti
7.5, Cu
62.3Zr
27.7Ti
10, Cu
60.6Zr
26.9Ti
12.5, Cu
58.8Zr
26.2Ti
15With general formula as a comparison case be Cu
60Zr
30Ti
10Non-crystaline amorphous metal compare, this invention formula of is Cu
64Zr
28.5Ti
7.5The amorphous formation ability of non-crystaline amorphous metal stronger, Vickers' hardness and yield strength are higher.And be Cu by general formula
62.3Zr
27.7Ti
10, Cu
60.6Zr
26.9Ti
12.5, Cu
58.8Zr
26.2Ti
15The Vickers' hardness and the yield strength of non-crystaline amorphous metal all be lower than Comparative Examples, amorphous formation ability is a little more than Comparative Examples.
But the diameter of disclosed Cu-based bulk body non-crystaline amorphous metal only is 3mm among the embodiment of foregoing invention, and therefore, its amorphous formation ability is still not high enough.In addition, the preparation condition of this Cu-based bulk body non-crystaline amorphous metal is also relatively harsher, for example, needs to be evacuated to 10 before melting
-2Handkerchief.In addition, there is the shortcoming of plasticity difference in the cu-based amorphous alloys in this inventive embodiments, therefore on using limitation is arranged.
Summary of the invention
The objective of the invention is provides strong copper-zirconium-base amorphous alloy of a kind of amorphous formation ability and plasticity and preparation method thereof in order to overcome the shortcoming of the little and plasticity difference of non-crystaline amorphous metal critical size in the prior art.
The invention provides a kind of copper-zirconium-base amorphous alloy, wherein, the composed as follows of this copper-zirconium-base amorphous alloy stated shown in the general formula: Cu
aZr
bTi
cWherein, a, b, c are atomic percent, 45≤a≤55,35≤b≤45,5≤c≤15, and a, b, c sum are 100.
The present invention also provides the preparation method of copper-zirconium-base amorphous alloy, and this method is included under shielding gas atmosphere or the vacuum environment, and the non-crystaline amorphous metal raw material is carried out the melting and the cooling forming of casting, wherein, and described non-crystaline amorphous metal raw material general molecular formula Cu
aZr
bTi
cRatio, in the formula, a, b, c are atomic percent, 45≤a≤55,35≤b≤45,5≤c≤15, and a, b, c sum are 100.
The critical size of the copper-zirconium-base amorphous alloy that the present invention makes is all more than 5mm, and the non-crystaline amorphous metal that the present invention makes has excellent compression fracture strength and Vickers' hardness.Simultaneously, the amorphous alloy plasticity that the present invention obtains is strong, and the plastix strain amount reaches 25%, and the plastix strain amount of the cu-based amorphous alloys that obtains according to prior art only is about 8%.Therefore, the performance of copper-zirconium-base amorphous alloy of the present invention is more good, is with a wide range of applications in fields such as machinery, medicine equipment and biomaterials.In addition, the preparation method's of copper-zirconium-base amorphous alloy of the present invention condition is comparatively gentle, easily preparation.
Description of drawings
The X-ray powder diffraction figure of the sample that Fig. 1 makes for embodiment 1-6 and Comparative Examples 1;
Fig. 2 is the compressive stress strain curve figure of the non-crystaline amorphous metal that makes for embodiment 1 and Comparative Examples 1.
Embodiment
The composed as follows of copper-zirconium-base amorphous alloy of the present invention stated shown in the general formula: Cu
aZr
bTi
cWherein, a, b, c are atomic percent, 45≤a≤55,35≤b≤45,5≤c≤15, and a, b, c sum are 100.
Under the preferable case, 49≤a≤51,35≤b≤45.Under above-mentioned preferable case, can make that critical size is bigger, the better copper-zirconium-base amorphous alloy of plasticity.
The preparation method of copper-zirconium-base amorphous alloy of the present invention, this method are included under shielding gas atmosphere or the vacuum environment, and the non-crystaline amorphous metal raw material is carried out the melting and the cooling forming of casting, wherein, and described non-crystaline amorphous metal raw material general molecular formula Cu
aZr
bTi
cRatio, in the formula, a, b, c are atomic percent, 45≤a≤55,35≤b≤45,5≤c≤15, and a, b, c sum are 100.
Among the preparation method of non-crystaline amorphous metal of the present invention, containing a spot of impurity in the described non-crystaline amorphous metal raw material to not influence of the melting of non-crystaline amorphous metal, is benchmark with the total amount of non-crystaline amorphous metal, and to be that 5 atom % are following get final product the content of described impurity.Therefore, preparation method of the present invention is not high for the requirement of the purity of various raw materials yet, but the material purity height helps the formation of non-crystaline amorphous metal.Therefore, the purity that is used to prepare the various raw materials of copper-zirconium-base amorphous alloy of the present invention is preferably more than the 99 weight %, more preferably 99-99.999 weight %.
Described shielding gas atmosphere or vacuum environment are in order to make alloy raw material obtain protection in fusion process, to avoid oxidized.The antioxidant property of non-crystaline amorphous metal raw material of the present invention is better, and is therefore lower to the requirement of shielding gas atmosphere and vacuum environment.Described shielding gas is one or more in the neutral element gas in the periodic table of elements.The purity of described shielding gas is not less than 95 volume % and gets final product, and for example can be 95-99.9 volume %.Only need be evacuated to vacuum tightness before the feeding shielding gas in the smelting furnace is to get final product below 1000 handkerchiefs.In addition, described vacuum environment is meant that vacuum tightness is no more than 1000 handkerchiefs, is preferably the 0.1-1000 handkerchief.Vacuum tightness of the present invention is represented with absolute pressure.
The method of described melting is the melting method of various routines in this area, as long as with the abundant fusion of non-crystaline amorphous metal raw material, for example can in melting equipment, carry out melting, smelting temperature and smelting time are along with raw-material different some variations that have of institute's non-crystaline amorphous metal, among the present invention, smelting temperature is preferably 1000-2700 ℃, more preferably 1200-2500 ℃; Smelting time is preferably 0.5-5 minute, more preferably 1-3 minute.Described melting equipment can be the melting equipment of routine, for example arc-melting furnace or induction melting.
The crystallized ability of non-crystaline amorphous metal of the present invention is strong, and therefore described cooling forming can adopt the casting cooling forming method of various routines in this area, for example, fused alloy material (melt) is cast in the mould, then cooling.Described casting process can be for gravity casting, inhale in casting, spray to cast, the die casting any one.Gravity casting is meant and utilizes the action of gravity of melt itself to be cast in the mould.Gravity casting realize easily, and cost is low, so the present invention preferably uses because method is simple.The concrete operation method of described casting is conventionally known to one of skill in the art.Moulding stock can be the material of 30-400W/mK (being preferably 50-200W/mK) for copper alloy, stainless steel and thermal conductivity.Mould can carry out water-cooled, oil cooling or cooled with liquid nitrogen.Refrigerative speed can be more than the 10K/s, to be preferably 10-10
4K/s.The refrigerative degree there are not special requirement, as long as can be shaped to non-crystaline amorphous metal of the present invention.
In addition, preferably when adding raw material, make a, b in the above-mentioned general formula in following scope: 49≤a≤51,35≤b≤45.Under above-mentioned preferable case, the amorphous formation ability of non-crystaline amorphous metal is stronger, can obtain the better copper-zirconium-base amorphous alloy of plasticity.
Describe the present invention in detail below by embodiment.
Embodiment 1
Present embodiment illustrates copper-zirconium-base amorphous alloy provided by the invention and preparation method thereof.
With purity is that the various copper-zirconium-base amorphous alloy raw materials of 99.96 weight % drop in the arc-melting furnaces (Shenyang scientific instrument factory); with arc melting stove evacuation (vacuum tightness is 5 handkerchiefs); the argon gas that feeds purity then and be 99.9 volume % is as shielding gas; under 1300 ℃ of conditions; melting 3 minutes makes the abundant fusion of copper-zirconium-base amorphous alloy raw material.The kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 42 atom % of 50 atom %, the Ti of 8 atom %.
Then the method for fused alloy sample by gravity casting is cast in the copper mold, and with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, forms the copper-zirconium-base amorphous alloy sample A1 that is of a size of 2 millimeters of Φ, 20 millimeters of length.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample A1 consists of Cu
50Zr
42Ti
8
Comparative Examples 1
Method according to embodiment 1 prepares copper-zirconium-base amorphous alloy, and different is that the kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 28.5 atom % of 64 atom %, the Ti of 7.5 atom %.
Finally obtain non-crystaline amorphous metal sample D1.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample D1 consists of Cu
64Zr
28.5Ti
7.5
Embodiment 2
Method according to embodiment 1 prepares copper-zirconium-base amorphous alloy, and different is that the kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 43 atom % of 51 atom %, the Ti of 8 atom %.
Finally obtain non-crystaline amorphous metal sample A2.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample A2 consists of Cu
51Zr
43Ti
8
Embodiment 3
Method according to embodiment 1 prepares copper-zirconium-base amorphous alloy, and different is that the kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 36 atom % of 49 atom %, the Ti of 15 atom %.
Finally obtain non-crystaline amorphous metal sample A3.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample A3 consists of Cu
49Zr
36Ti
15
Embodiment 4
Method according to embodiment 1 prepares copper-zirconium-base amorphous alloy, and different is that the kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 40 atom % of 55 atom %, the Ti of 5 atom %.
Finally obtain non-crystaline amorphous metal sample A4.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample A4 consists of Cu
55Zr
40Ti
5
Method according to embodiment 1 prepares copper-zirconium-base amorphous alloy, and different is that the kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 41 atom % of 45 atom %, the Ti of 14 atom %.
Finally obtain non-crystaline amorphous metal sample A5.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample A5 consists of Cu
45Zr
41Ti
14
Embodiment 6
Present embodiment illustrates copper-zirconium-base amorphous alloy provided by the invention and preparation method thereof.
With purity is that the various copper-zirconium-base amorphous alloy raw materials of 99.96 weight % drop in the arc-melting furnaces (Shenyang scientific instrument factory); with arc melting stove evacuation (vacuum tightness is 10 handkerchiefs); the argon gas that feeds purity then and be 99.9 volume % is as shielding gas; under 1300 ℃ of conditions; melting 3 minutes makes the abundant fusion of copper-zirconium-base amorphous alloy raw material.The kind of each copper-zirconium-base amorphous alloy raw material and consumption are the Zr of Cu, the 39 atom % of 50 atom %, the Ti of 11 atom %.
Then the method for fused alloy sample by gravity casting is cast in the copper mold, and with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, forms the copper-zirconium-base amorphous alloy sample A6 that is of a size of 2 millimeters of Φ, 20 millimeters of length.Ultimate analysis shows, this copper-zirconium-base amorphous alloy sample A6 consists of Cu
50Zr
39Ti
11
Embodiment 7-12
These embodiment illustrate the performance of the copper-zirconium-base amorphous alloy sample that the present invention makes.
1, XRD analysis
The copper-zirconium-base amorphous alloy sample that the foregoing description 1-6 is made carries out the XRD powder diffraction analysis respectively on model is the x-ray powder diffraction instrument of D-MAX2200PC, to judge whether alloy is amorphous.The condition of X-ray powder diffraction comprises with copper target emanation, incident wavelength
Acceleration voltage is 40 kilovolts, and electric current is 20 milliamperes, adopts step-scan, and scanning step is 0.04 °, and the result as shown in Figure 1.
Non-crystaline amorphous metal sample A1 from Fig. 1 disperses peak A, non-crystaline amorphous metal sample A2 and disperses peak B, non-crystaline amorphous metal sample A3 and disperse peak C, non-crystaline amorphous metal sample A4 and disperse that peak D, non-crystaline amorphous metal sample A5 disperse peak E, non-crystaline amorphous metal sample A6 disperses peak F, and the sample A1-A6 that embodiment of the invention 1-6 makes is non-crystalline state.
2, critical size test
Method according to embodiment 1-6 prepares non-crystaline amorphous metal, different is, pour into wedge shape, carry out following test then respectively: the sample of the wedge shape thickness with 1mm from the angle of this wedge shape is cut, then aforesaid XRD analysis is carried out in the cross section of cutting this sample formation, measure structure type, if structure type is a non-crystaline amorphous metal, then continue cutting, till structure type is not non-crystaline amorphous metal, record cutting total thickness, described critical size is the thickness after this total thickness deducts 1mm.The result is as shown in table 1.
3, the mensuration of compressed rupture strength and compressive stress strain curve
The copper-zirconium-base amorphous alloy that the foregoing description 1-6 is made carries out following test: the bar that the non-crystaline amorphous metal sample that makes is intercepted into Φ 1mm * 2mm, utilize the compressed rupture strength and the compressive stress strain curve of CMT5105 electronic universal tester specimen, obtain the plastix strain amount (ε of non-crystaline amorphous metal then according to corresponding compressive stress strain curve
p).Plastix strain amount (the ε of described compressed rupture strength and non-crystaline amorphous metal
p) the result as shown in table 1.In addition, the compressive stress strain curve of the non-crystaline amorphous metal sample A1 of embodiment 1 as shown in Figure 2.
4, Vickers' hardness test
The copper-zirconium-base amorphous alloy that the foregoing description 1-6 is made carries out the Vickers' hardness test on Micro Hardness Text Hv1000 Vickers' hardness test machine, pressure head weight is 200 grams, loading time is 10 seconds, every kind of sample is got three numerical value, get its arithmetical av at last, the result is as shown in table 1.
Comparative Examples 2
The performance of the copper-zirconium-base amorphous alloy sample of this Comparative Examples explanation prior art.
According to embodiment 7 described methods the copper-zirconium-base amorphous alloy sample D1 that Comparative Examples 1 makes is carried out above-mentioned performance test, wherein the XRD analysis result as shown in Figure 1, critical size test, compressed rupture strength test, plastix strain amount (ε
p) and the result of Vickers' hardness test as shown in table 1.The compressive stress strain curve of the non-crystaline amorphous metal sample D1 that Comparative Examples 1 makes as shown in Figure 2.
Non-crystaline amorphous metal sample D1 from Fig. 1 disperses peak G as can be seen, and the non-crystaline amorphous metal sample D1 that is made by Comparative Examples 1 is a non-crystalline state.
Table 1
| Sample number into spectrum | Critical size (mm) | Compressed rupture strength (MPa) | Vickers' hardness (Hv) | Plastix strain amount ε p (％) | |
| Embodiment 1 | |
5 | 1842 | 561 | 25 |
| Comparative Examples 1 | D1 | 3 | 1987 | 539 | 8 |
| Embodiment 2 | |
5 | 1815 | 556 | 22 |
| Embodiment 3 | A3 | 6 | 1804 | 547 | 23 |
| Embodiment 4 | |
5 | 1760 | 545 | 22 |
| |
|
5 | 1771 | 543 | 20 |
| Embodiment 6 | A6 | 7 | 1857 | 568 | 26 |
As can be seen from Table 1, the critical size of the non-crystaline amorphous metal that embodiment of the invention 1-6 makes is all more than 5mm, and the critical size of the non-crystaline amorphous metal D1 that Comparative Examples 1 makes only is 3mm, and the non-crystaline amorphous metal that the present invention makes has excellent compression fracture strength and Vickers' hardness.
Claims (9)
1, a kind of copper-zirconium-base amorphous alloy is characterized in that, the composed as follows of this copper-zirconium-base amorphous alloy stated shown in the general formula: Cu
aZr
bTi
cWherein, a, b, c are atomic percent, 45≤a≤55,35≤b≤50,5≤c≤15, and a, b, c sum are 100.
2, alloy according to claim 1, wherein, 49≤a≤51,35≤b≤45.
3, the preparation method of the described copper-zirconium-base amorphous alloy of claim 1, this method are included under shielding gas atmosphere or the vacuum environment, and the non-crystaline amorphous metal raw material is carried out the melting and the cooling forming of casting, and it is characterized in that, described non-crystaline amorphous metal raw material general molecular formula Cu
aZr
bTi
cRatio, in the formula, a, b, c are atomic percent, 45≤a≤55,35≤b≤45,5≤c≤15, and a, b, c sum are 100.
4, method according to claim 3, wherein, 49≤a≤51,35≤b≤45.
5, method according to claim 3, wherein, the condition of described melting comprises that smelting temperature is 1000-2700 ℃, smelting time is 0.5-5 minute.
6, method according to claim 3, wherein, during described cooling forming, rate of cooling is more than the 10K/s.
7, method according to claim 3, wherein, described shielding gas is one or more in the neutral element gas in the periodic table of elements.
8, method according to claim 3, wherein, the vacuum tightness of described vacuum environment is the 0.1-1000 handkerchief.
9, method according to claim 3, wherein, the method for described casting is a gravity casting.
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|---|---|---|---|---|
| CN102242324A (en) * | 2011-07-07 | 2011-11-16 | 湖南理工学院 | Hot-press molding process of Cu50Zr40Ti10 amorphous alloy powder |
| CN102534439A (en) * | 2012-02-12 | 2012-07-04 | 北京航空航天大学 | Nickel-free low-copper zirconium-based bulk amorphous alloy and preparation method thereof |
| CN104645423A (en) * | 2015-02-11 | 2015-05-27 | 东莞台一盈拓科技股份有限公司 | Amorphous alloy scalpel and manufacture method thereof |
| CN107760913A (en) * | 2017-11-08 | 2018-03-06 | 湖南理工学院 | A series of Cu Zr Ti block amorphous alloys and its preparation technology |
| CN107829046A (en) * | 2017-11-08 | 2018-03-23 | 湖南理工学院 | The Cu base bulk metallic glass and its preparation technology of a kind of iron content |
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| CN113564579A (en) * | 2021-07-06 | 2021-10-29 | 燕山大学 | Method for preparing copper-based amorphous composite coating by laser cladding |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102242324A (en) * | 2011-07-07 | 2011-11-16 | 湖南理工学院 | Hot-press molding process of Cu50Zr40Ti10 amorphous alloy powder |
| CN102242324B (en) * | 2011-07-07 | 2012-12-26 | 湖南理工学院 | Hot-press molding process of Cu50Zr40Ti10 amorphous alloy powder |
| CN102534439A (en) * | 2012-02-12 | 2012-07-04 | 北京航空航天大学 | Nickel-free low-copper zirconium-based bulk amorphous alloy and preparation method thereof |
| CN102534439B (en) * | 2012-02-12 | 2014-07-30 | 北京航空航天大学 | Nickel-free low-copper zirconium-based bulk amorphous alloy and preparation method thereof |
| CN104645423A (en) * | 2015-02-11 | 2015-05-27 | 东莞台一盈拓科技股份有限公司 | Amorphous alloy scalpel and manufacture method thereof |
| CN104645423B (en) * | 2015-02-11 | 2017-11-14 | 东莞帕姆蒂昊宇液态金属有限公司 | A kind of non-crystaline amorphous metal scalpel and its manufacture method |
| CN107760913A (en) * | 2017-11-08 | 2018-03-06 | 湖南理工学院 | A series of Cu Zr Ti block amorphous alloys and its preparation technology |
| CN107829046A (en) * | 2017-11-08 | 2018-03-23 | 湖南理工学院 | The Cu base bulk metallic glass and its preparation technology of a kind of iron content |
| CN107829046B (en) * | 2017-11-08 | 2020-01-31 | 湖南理工学院 | Fe-containing copper-based bulk amorphous alloy and preparation process thereof |
| CN109722559A (en) * | 2019-03-14 | 2019-05-07 | 北京科技大学 | A kind of copper zirconium/hafnium base noncrystal alloy of oxygen alloy and preparation method thereof |
| CN113564579A (en) * | 2021-07-06 | 2021-10-29 | 燕山大学 | Method for preparing copper-based amorphous composite coating by laser cladding |
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