CN101423917B - Rare-earth base amorphous alloy and method of preparing the same - Google Patents
Rare-earth base amorphous alloy and method of preparing the same Download PDFInfo
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Abstract
The invention provides a rare earth based non-crystal alloy, wherein the composition of the non-crystal alloy is ReaAlbMcNd of which, Re is at least two of La, Ce, Pr and Nd elements, M is one or more than one of Fe, Co, Ni, Cu, Zn, Ge, As, Zr, Mo, Pd and Ag elements, N is one or more than one of Y, Hf and Nb, a is more than or equal to 30 and less than or equal to 70, b is more than or equal to 5 and less than or equal to 40, c is more than or equal to 15 and less than or equal to 40, d is more than or equal to 0.1 and less than or equal to 10, and a plus b plus c plus d is equal to 100; anda, b, c and d are all mol percentages. The invention also provides a method for preparing the non-crystal alloy. The non-crystal alloy prepared by the method has the advantages of excellent bending strength and hardness, good non-crystal forming capability and large critical dimension.
Description
Technical field
The invention relates to a kind of non-crystaline amorphous metal and preparation method thereof, more particularly about a kind of rare-earth-base amorphous alloy and preparation method thereof.
Background technology
Non-crystaline amorphous metal has as the long-range of glass unordered, the constructional feature of short range order, non-crystaline amorphous metal is compared with crystal alloy, have high intensity, hardness, wear resistance, solidity to corrosion and high resistance, but also show characteristics such as good supraconductivity and low magnetic loss, therefore, have wide practical use in industries such as IT electronics, machinery, chemical industry.
Rare-earth-base amorphous alloy is with the melting at high temperature of non-crystaline amorphous metal raw material, adopts rapid solidification moulding in supercooling liquid phase region such as copper mold casting method to obtain then.
CN 1664155A discloses a kind of cerium base large amorphous alloy, and this alloy is main component with the cerium, and it is formed available following formula and represents: Ce
aAl
bNi
cCu
dM
e, wherein 50≤a≤80,5≤b≤20,5≤c≤20,5≤d≤20,0＜e≤10, and a+b+c+d+e=100.Described M is Sc, Nb, Ti, V, Cr, Mn, Fe, Co, Y, Zr, Mo, La, Pr, Nd or Hf.
The non-crystaline amorphous metal that this invention provides has improved non-crystaline amorphous metal cost height in the conventional art, oxidation-resistance difference and the high shortcoming of elastic performance.But the critical size of this non-crystaline amorphous metal is 5mm to the maximum, so critical size is still less, can't be as the amorphous alloy material of preparation large size product.
In addition, in the prior art, rare-earth-base amorphous alloy does not have good binding on intensity and amorphous formation ability.The rare-earth-base amorphous alloy that amorphous formation ability is good, intensity are often very low; And the high non-crystaline amorphous metal of intensity does not have the good amorphous formation ability of row, that is to say that intensity is higher, but critical size is less, can't form bulk rare-earth based amorphous alloy.This makes the application of rare-earth-base amorphous material be subjected to greatly restriction.
Summary of the invention
The objective of the invention is the shortcoming that can't obtain intensity height, rare-earth-base amorphous alloy that amorphous formation ability is strong in the prior art, a kind of intensity height, rare-earth-base amorphous alloy that amorphous formation ability is strong and preparation method thereof are provided in order to overcome.
The invention provides a kind of rare-earth-base amorphous alloy, wherein, this non-crystaline amorphous metal consist of Re
aAl
bM
cN
d, in the formula, Re is at least two kinds among La, Ce, Pr and the Nd, M is one or more among Fe, Co, Ni, Cu, Zn, Ge, As, Zr, Mo, Pd and the Ag, N is Y, one or more among Hf and the Nb, 30≤a≤70,5≤b≤40,15≤c≤40,0.1≤d≤10, and a+b+c+d=100; A, b, c, d are molecular fraction.
The present invention also provides a kind of preparation method of rare-earth-base amorphous alloy, and this method comprises, under shielding gas, the non-crystaline amorphous metal raw material is carried out melting and cooling forming, and wherein, described non-crystaline amorphous metal raw material is according to general formula R e
aAl
bM
cN
dRatio add, in the formula, Re is at least two kinds among La, Ce, Pr and the Nd, and M is one or more among Fe, Co, Ni, Cu, Zn, Ge, As, Zr, Mo, Pd and the Ag, and N is Y, among Hf and the Nb one or more, 30≤a≤70,5≤b≤40,15≤c≤40,0.1≤d≤10, and a+b+c+d=100; A, b, c, d are molecular fraction.
Experiment showed, that the non-crystaline amorphous metal that the present invention makes has good bending strength and hardness, and have good amorphous formation ability, the critical size of the non-crystaline amorphous metal that makes is big.For example, the critical size of the non-crystaline amorphous metal that the present invention makes is all more than 6mm, and the critical size of the non-crystaline amorphous metal that prior art makes is all below 5mm.
Description of drawings
The X-ray powder diffraction figure of the sample that Fig. 1 makes for embodiment 1-4 and Comparative Examples 1-2.
Embodiment
Rare-earth-base amorphous alloy of the present invention consist of Re
aAl
bM
cN
d, in the formula, Re is at least two kinds among La, Ce, Pr and the Nd, M is one or more among Fe, Co, Ni, Cu, Zn, Ge, As, Zr, Mo, Pd and the Ag, N is Y, one or more among Hf and the Nb, 30≤a≤70,5≤b≤40,15≤c≤40,0.1≤d≤10, and a+b+c+d=100; A, b, c, d are molecular fraction.
Under the preferable case, described RE is an at least a mixture among La and Ce, Pr and the Nd.Wherein, La can be any ratio with the mol ratio of the total amount of Ce, Pr and Nd, and the mol ratio of the total amount of La and Ce, Pr and Nd is preferably 0.5-3, more preferably 1-2.Under above-mentioned preferable case, the non-crystaline amorphous metal that the present invention makes has better bending strength and hardness, and has good amorphous formation ability, and the critical size of the non-crystaline amorphous metal that makes is big.
Under the preferable case, 60≤a≤65,5≤b≤15,20≤c≤25,0.1≤d≤10, and a+b+c+d=100.
The preparation method of rare-earth-base amorphous alloy of the present invention comprises, under shielding gas, the non-crystaline amorphous metal raw material is carried out melting and cooling forming, it is characterized in that, described non-crystaline amorphous metal raw material is according to general formula R e
aAl
bM
cN
dRatio add, in the formula, Re is at least two kinds among La, Ce, Pr and the Nd, and M is one or more among Fe, Co, Ni, Cu, Zn, Ge, As, Zr, Mo, Pd and the Ag, and N is Y, among Hf and the Nb one or more, 30≤a≤70,5≤b≤40,15≤c≤40,0.1≤d≤10, and a+b+c+d=100; A, b, c, d are molecular fraction.
Under the preferable case, described RE is an at least a mixture among La and Ce, Pr and the Nd.Wherein, La can be any ratio with the mol ratio of the total amount of Ce, Pr and Nd, and the mol ratio of the total amount of La and Ce, Pr and Nd is preferably 0.5-3, more preferably 1-2.Under above-mentioned preferable case, the non-crystaline amorphous metal that the present invention makes has better bending strength and hardness, and has good amorphous formation ability, and the critical size of the non-crystaline amorphous metal that makes is big.
Under the preferable case, 60≤a≤65,5≤b≤15,20≤c≤25,0.1≤d≤10, and a+b+c+d=100.
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 arc-melting furnace, 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 800-1100 ℃, and smelting time is preferably 3-5 minute.
Described cooling can be adopted the method for cooling of various routines in this area, for example, water cooled copper mould cooling or the cooling of oil cooling copper mold, 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.
Because the rare earth composition that the present invention added plays synergies such as anti-oxidant in the non-crystaline amorphous metal forming process, make non-crystaline amorphous metal less demanding to material purity in preparation process, so among the present invention, the purity of each used raw material is 97-99.9 volume %, more preferably 98-99.9 volume %.In addition, not high to shielding gas and purity requirement thereof in preparation process, shielding gas can be neutral element gas or N in the periodic table of elements
2, SF
6In one or more, the purity of gas can be 98-99.9 volume %; Also can contain O in the shielding gas
2, CO, CO
2, H
2O, SO
2, NO, NO
2And H
2The foreign gas of one or more in the gas.Contain a spot of foreign gas to not influence of the melting of non-crystaline amorphous metal, in the time of can also reducing melting to the requirement of shielding gas.Generally, in shielding gas, the volume content of described foreign gas is 1000-10000ppm.In non-crystaline amorphous metal raw material fusion process, the purpose that adds shielding gas all is in order to make alloy raw material obtain protection in fusion process, to avoid oxidized.
Describe the present invention in detail below by embodiment.
Embodiment 1
Present embodiment illustrates rare-earth-base amorphous alloy provided by the invention and preparation method thereof.
200 gram non-crystaline amorphous metal raw materials are dropped in the arc-melting furnace (Shenyang scientific instrument factory); with the arc melting stove evacuation; adopting purity is that the argon gas of 98 volume % is as shielding gas (volume content of foreign gas is 2000ppm); under 1000 ℃ of conditions; melting 5 minutes makes the abundant fusion of non-crystaline amorphous metal raw material.The Fe of the Ni of the Al of the La that consists of 20 moles of % of described non-crystaline amorphous metal raw material, the Ce of 10 moles of %, 26 moles of %, the Cu of 10 moles of %, 15 moles of %, the Co of 11 moles of %, 1 mole of % and the Nb of 7 moles of %.
Then with the fused alloy sample, with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, and fusion and cooling once more according to the method described above pours into the non-crystaline amorphous metal sample Al that is of a size of 3mm * 10mm * 100mm then.Ultimate analysis shows, this non-crystaline amorphous metal sample Al consists of La
20Ce
10Al
26Cu
10Ni
15Co
11Fe
1Nb
7
Embodiment 2
Present embodiment illustrates rare-earth-base amorphous alloy provided by the invention and preparation method thereof.
200 gram non-crystaline amorphous metal raw materials are dropped in the arc-melting furnace (Shenyang scientific instrument factory); with the arc melting stove evacuation; adopting purity is that the argon gas of 98 volume % is as shielding gas (volume content of foreign gas is 2000ppm); under 900 ℃ of conditions; melting 4 minutes makes the abundant fusion of non-crystaline amorphous metal raw material.The Zr of the Al of the La that consists of 30 moles of % of described non-crystaline amorphous metal raw material, the Pr of 30 moles of %, 15 moles of %, the Ge of 10 moles of %, 10 moles of %, the Y of 5 moles of %.
Then with the fused alloy sample, with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, and fusion and cooling once more according to the method described above pours into the non-crystaline amorphous metal sample A2 that is of a size of 3mm * 10mm * 100mm then.Ultimate analysis shows, this non-crystaline amorphous metal sample A2 consists of La
30Pr
30Al
15Ge
10Zr
10Y
5
Embodiment 3
Present embodiment illustrates rare-earth-base amorphous alloy provided by the invention and preparation method thereof.
200 gram non-crystaline amorphous metal raw materials are dropped in the arc-melting furnace (Shenyang scientific instrument factory); with the arc melting stove evacuation; adopting purity is that the argon gas of 98 volume % is as shielding gas (volume content of foreign gas is 2000ppm); under 1000 ℃ of conditions; melting 5 minutes makes the abundant fusion of non-crystaline amorphous metal raw material.The Y of the Co of the As of the Nd of the La that consists of 25 moles of % of described non-crystaline amorphous metal raw material, the Ce of 25 moles of %, 15 moles of %, the Al of 8.9 moles of %, 10 moles of %, the Zn of 12 moles of %, 2 moles of %, the Fe of 1 mole of %, 1 mole of % and the Nb of 0.1 mole of %.
With the fused alloy sample, carry out the water cooled copper mould cooling with the speed of cooling of 100K/s then, fusion and cooling once more according to the method described above pours into the non-crystaline amorphous metal sample A3 that is of a size of 3mm * 10mm * 100mm then.Ultimate analysis shows, this non-crystaline amorphous metal sample A3 consists of La
25Ce
25Nd
15A
L8.9As
10Zn
12Co
2Fe
1Y
1Nb
0.1
Embodiment 4
Present embodiment illustrates rare-earth-base amorphous alloy provided by the invention and preparation method thereof.
200 gram non-crystaline amorphous metal raw materials are dropped in the arc-melting furnace (Shenyang scientific instrument factory); with the arc melting stove evacuation; adopting purity is that the argon gas of 98 volume % is as shielding gas (volume content of foreign gas is 2000ppm); under 1000 ℃ of conditions; melting 5 minutes makes the abundant fusion of non-crystaline amorphous metal raw material.The Fe of the Ni of the Al of the La that consists of 40 moles of % of described non-crystaline amorphous metal raw material, the Ce of 20 moles of %, 15 moles of %, the Cu of 10 moles of %, 10 moles of %, the Co of 3 moles of %, 1.5 moles of % and the Hf of 0.5 mole of %.
Then with the fused alloy sample, with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, and fusion and cooling once more according to the method described above pours into the non-crystaline amorphous metal sample A4 that is of a size of 3mm * 10mm * 100mm then.Ultimate analysis shows, this non-crystaline amorphous metal sample A4 consists of La
40Ce
20Al
15Cu
10Ni
10Co
3Fe
1.5Hf
0.5
Comparative Examples 1
200 gram non-crystaline amorphous metal raw materials are dropped in the arc-melting furnace (Shenyang scientific instrument factory); with the arc melting stove evacuation; adopting purity is that the argon gas of 98 volume % is as shielding gas (volume content of foreign gas is 2000ppm); under 1000 ℃ of conditions; melting 5 minutes makes the abundant fusion of non-crystaline amorphous metal raw material.The Nb of the Ni of the Ce that consists of 65 moles of % of described non-crystaline amorphous metal raw material, the Al of 10 moles of %, 10 moles of %, the Cu of 10 moles of %, 5 moles of %.
Then with the fused alloy sample, with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, and fusion and cooling once more according to the method described above pours into the non-crystaline amorphous metal sample D1 that is of a size of 3mm * 10mm * 100mm then.Ultimate analysis shows, this non-crystaline amorphous metal sample D1 consists of Ce
65Al
10Cu
10Ni
10Nb
5
Comparative Examples 2
200 gram non-crystaline amorphous metal raw materials are dropped in the arc-melting furnace (Shenyang scientific instrument factory); with the arc melting stove evacuation; adopting purity is that the argon gas of 98 volume % is as shielding gas (volume content of foreign gas is 2000ppm); under 1000 ℃ of conditions; melting 5 minutes makes the abundant fusion of non-crystaline amorphous metal raw material.The Cu of the Al of the La that consists of 5 moles of % of described non-crystaline amorphous metal raw material, the Ce of 57 moles of %, 10 moles of %, the Ni of 12.5 moles of %, 15.5 moles of %.
Then with the fused alloy sample, with 10
3The speed of cooling of K/s is carried out the water cooled copper mould cooling, and fusion and cooling once more according to the method described above pours into the non-crystaline amorphous metal sample D2 that is of a size of 3mm * 10mm * 100mm then.Ultimate analysis shows, this non-crystaline amorphous metal sample D2 consists of La
5Ce
57Al
10Cu
15.5Ni
12.5
Embodiment 5
The performance of the non-crystaline amorphous metal Al that present embodiment explanation the present invention makes.
1, XRD analysis
Be to carry out the XRD powder diffraction analysis on the X ray powder art diffractometer of D-MAX2200PC with sample Al, to judge whether alloy is amorphous in model.The condition of X-ray powder diffraction comprises with the copper target emanation, incident wavelength λ=1.54060
, acceleration voltage is 40 kilovolts, and electric current is 20 milliamperes, adopts step-scan, and scanning step is 0.04 °, and the result is as shown in Figure 1.
2, critical size test
The sample Al of the wedge shape that forms in the copper mold 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 Al 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, bending strength test
The sample Al that embodiment 1 is obtained according to the method for GB/T14452-93 tests on 1 ton the trier (newly thinking carefully company), 50 millimeters of spans, and loading velocity is 0.5 mm/min, the result is as shown in table 1.
4, hardness test
Measure the hardness of the sample Al that embodiment 1 obtains by Vickers' hardness experimental machine (Shanghai safe Mingguang City learn the HVS-10Z of Instr Ltd.), wherein, the pressure head of Vickers' hardness experimental machine is 100g, loading time is 15 seconds, the hardness of three the different points on the difference working sample, averaging then is the hardness of sample Al.The result is as shown in table 1.
Embodiment 6-8
Method according to embodiment 5 is carried out performance test to the sample A2-A4 that embodiment 2-4 makes.The result is shown in Fig. 1 and table 1.
Comparative Examples 3-4
Method according to embodiment 5 is carried out performance test to sample D1 and the D2 that Comparative Examples 1-2 makes.The result is shown in Fig. 1 and table 1.
Table 1
| Sample source | Critical size (mm) | Bending strength (MPa) | Hardness (Hv) |
| Embodiment 1 | 8 | 838.7 | 230.9 |
| Embodiment 2 | 8 | 854.5 | 230.3 |
| Embodiment 3 | 8 | 853.6 | 234.6 |
| Embodiment 4 | 8 | 859.1 | 245.4 |
| Comparative Examples 1 | 5 | 792.5 | 219.8 |
| Comparative Examples 2 | 4 | 800.3 | 215.6 |
Non-crystaline amorphous metal sample Al 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 D1 disperse peak E and non-crystaline amorphous metal sample D2 disperses peak F as can be seen, and sample A1-A4 and D1-2 that embodiment of the invention 1-4 and Comparative Examples 1-2 make are non-crystalline state.
As can be seen from Table 1, the critical size of the non-crystaline amorphous metal that embodiment of the invention 1-4 makes is all more than 6mm, and the critical size of the non-crystaline amorphous metal that Comparative Examples makes only is 4mm and 5mm, and the non-crystaline amorphous metal that the present invention makes has good bending strength and hardness.
Claims (6)
1. a rare-earth-base amorphous alloy is characterized in that, this non-crystaline amorphous metal consist of RE
aAl
bM
cN
dIn the formula, RE is an at least a mixture among La and Ce, Pr and the Nd, and the mol ratio of the total amount of La and Ce, Pr and Nd is 0.5-3, and M is one or more among Fe, Co, Ni, Zn, Ge, As, Zr, Mo, Pd and the Ag, N is one or more among Y, Hf and the Nb, 30≤a≤70,5≤b≤40,15≤c≤40,0.1≤d≤10, and a+b+c+d=100; A, b, c, d are molecular fraction.
2. alloy according to claim 1, wherein, 60≤a≤65,5≤b≤15,20≤c≤25,0.1≤d≤5, and a+b+c+d=100.
3. the preparation method of a rare-earth-base amorphous alloy, this method comprises, under shielding gas atmosphere, the non-crystaline amorphous metal raw material is carried out melting and cooling forming, it is characterized in that, described non-crystaline amorphous metal raw material is according to general formula R e
aAl
bM
cN
dRatio add, in the formula, RE is an at least a mixture among La and Ce, Pr and the Nd, and the mol ratio of the total amount of La and Ce, Pr and Nd is 0.5-3, M is one or more among Fe, Co, Ni, Zn, Ge, As, Zr, Mo, Pd and the Ag, N is Y, one or more among Hf and the Nb, 30≤a≤70,5≤b≤40,15≤c≤40,0.1≤d≤10, and a+b+c+d=100; A, b, c, d are molecular fraction.
4. method according to claim 3, wherein, 60≤a≤65,5≤b≤15,20≤c≤25,0.1≤d≤10, and a+b+c+d=100.
5. method according to claim 3, wherein, the condition of described melting comprises that smelting temperature is 800-1100 ℃, smelting time is 3-5 minute; During described cooling forming, rate of cooling is more than the 10K/s.
6. method according to claim 3, wherein, described shielding gas is neutral element gas, N in the periodic table of elements
2And SF
6In one or more.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2667258B2 (en) * | 1989-08-31 | 1997-10-27 | 健 増本 | Rare earth metal base alloy foil or rare earth metal base alloy fine wire and method for producing the same |
| CN1936058A (en) * | 2006-09-30 | 2007-03-28 | 北京航空航天大学 | La-Ce base amorphous alloy |
| CN1952201A (en) * | 2005-10-21 | 2007-04-25 | 中国科学院物理研究所 | Mixed rare earths-based amorphous metal plastic |
-
2007
- 2007-10-31 CN CN2007101820741A patent/CN101423917B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2667258B2 (en) * | 1989-08-31 | 1997-10-27 | 健 増本 | Rare earth metal base alloy foil or rare earth metal base alloy fine wire and method for producing the same |
| CN1952201A (en) * | 2005-10-21 | 2007-04-25 | 中国科学院物理研究所 | Mixed rare earths-based amorphous metal plastic |
| CN1936058A (en) * | 2006-09-30 | 2007-03-28 | 北京航空航天大学 | La-Ce base amorphous alloy |
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| Title |
|---|
| JP第2667258号B2 1997.06.27 |
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