CN104278220B - A kind of high W content Ni base noncrystal alloy and preparation method thereof - Google Patents
A kind of high W content Ni base noncrystal alloy and preparation method thereof Download PDFInfo
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- CN104278220B CN104278220B CN201410514123.7A CN201410514123A CN104278220B CN 104278220 B CN104278220 B CN 104278220B CN 201410514123 A CN201410514123 A CN 201410514123A CN 104278220 B CN104278220 B CN 104278220B
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Abstract
A kind of high W content Ni base noncrystal alloy and preparation method thereof.Amorphous alloy component, by atomic fraction, comprising: Ni? 60 ~ 69%, W? 17 ~ 22%, Nb? 0 ~ 8%, B? 13.5%; Preparation key step is: according to composition proportion and Homogeneous phase mixing starting powder, repressed, pre-burning consolidation, adopts vacuum arc melting to prepare mother alloy ingot, gets rid of the standby AMORPHOUS ALLOY RIBBONS of band mechanism by vacuum.Amorphous alloy component of the present invention is relatively simple, non precious metal composition, cost is lower, and still there is higher crystallization temperature and microhardness, its brilliant crystallization temperature 782 ~ 851K, high 8.5 ~ the 11.2GPa of microhardness, have broad application prospects in friction and corrosion resistant material, the present invention adopts powder pre-burning base substrate arc melting, and energy consumption reduces, and prepared high W content Ni base noncrystal alloy has that crystallization temperature is high, Heat stability is good, hardness is high, composition is simple, controllability good, low cost and other advantages, has broad application prospects.
Description
Technical field
The present invention relates to a kind of high W content Ni base noncrystal alloy and preparation method thereof.Belong to amorphous alloy material preparing technical field.
Background technology
Compared with common crystalline metallic material, non-crystaline amorphous metal has the advantages such as intensity is high, good toughness, solidity to corrosion are high, corrosion resistance superplasticity by force and at a certain temperature, becomes the novel material having application potential.But when temperature exceedes crystallization temperature, non-crystalline state will be transformed into crystalline phases, and amorphous excellent properties will significantly weaken, so just limit the application of non-crystaline amorphous metal under comparatively high temps occasion.Generally, the non-crystaline amorphous metal with high-content high-melting-point element has higher crystallization temperature.The fusing point of tungsten is high, so the non-crystaline amorphous metal of high W content has higher crystallization temperature." FirstWall " material of a new generation's nuclear reaction is operated in (Fusionengineeringanddesign in hot environment, 2011,86:1719-1723), corrosion resistance nature is lower owing to having crystal boundary for most of crystalline material, to such an extent as to do not find suitable " FirstWall " material for a long time, and the non-crystaline amorphous metal of high W content will become desirable " FirstWall " material due to himself feature.Simultaneously, the consistency and elasticity modulus of tungsten is also higher, be Hv=0.06E according to the Young's modulus of non-crystaline amorphous metal and the pass of Vickers' hardness, the non-crystaline amorphous metal of high W content has the feature of high elastic coefficient, high rigidity, this feature can make it under the effect of high speed load, have very high dynamic fracture toughnes, there is high self-sharpening in Penetration, as the non-crystaline amorphous metal of high W content is combined into armour piercing shot material, to " mushroom head " phenomenon of tungsten-alloyed white iron be greatly reduced, improve its penetration property.
At present, few to the research of the non-crystalline material of high W content both at home and abroad.The people such as Inoue (ScriptaMetallurgica, 1980,14 (2): 235-239) once reported W
70si
20b
10get rid of band amorphous, there is the hardness of superelevation.The people such as Ohtsuki (AppliedPhysicsLetters, 2004,14:4911-4913; MaterialsTransactions, 2005,46 (1): 48-53) once utilize copper roller to get rid of band and prepare W
46ru
37b
17non-crystaline amorphous metal, its first crystallization temperature is up to 1174K, and microhardness has 16.8 ± 1GPa, and microhardness during 900K is still higher than 10GPa; And prepare W
54rh
26b
20, W
56ir
23b
21, W
45re
23ru
15b
17, W
37ru
31rh
18b
14, W
38ir
17ru
31b
14, W
46ru
37b
15si
2etc. multiple amorphous alloy ribbon, all there is higher crystallization temperature.Yoshimoto etc. (2007 subsequently, (449-451): 260-263) study further getting rid of band non-crystaline amorphous metal above on the basis of people's researchs such as Ohtsuki, find that its crystallization temperature is between 1049 ~ 1331K, microhardness is in 13 ~ 18GPa scope.Suo etc. (MaterialsScienceandEngineeringA, 2011,528:2912-2916) select once to have made that 2mm is wide, 45 μm of thick W
30fe
38b
32-xc
xserial vacuum such as (x=5,7,10,13,15at.%) gets rid of band, the first crystallization temperature up to 984 ~ 1067K, W under room temperature
30fe
38b
32-xc
x(x=7,10,13,15at.%) gets rid of the microhardness of band amorphous between 11.9 to 12.8GPa.The non-crystaline amorphous metal of visible high W content shows high physical and mechanical properties, has huge application potential.The precious metal such as large more options Ru, Rh, Ir when but above investigator designs amorphous component, cost is higher; And although the research of Suo etc. adopts W, Fe, B and C tetra-kinds of elements, cost of alloy reduces relatively, but B and the C total content of the medium and small atomic radius of its component prescription is higher, cause that to prepare in mother alloy process volatilization at arc melting serious, cause melting difficulty, the Fe of high level makes amorphous thin ribbon with certain magnetic in addition, limits its application in particular circumstances.
CN101353771A discloses " a kind of tungsten based amorphous alloy ", a series of amorphous thin ribbons prepared by the method have comparatively high crystallization temperature, but its its composition comprises W, Fe, Si, Cr, Mn, Mo, B, Co macroelement, composition is very complicated, and it adopts tungsten block to carry out arc melting, as everyone knows, the fusing point of tungsten the highest (3410 DEG C) in all elemental metals, tungsten block need the long period or repeatedly melting number of times could mix in mother alloy, cause energy consumption to improve.
Summary of the invention
Because the above-mentioned defect of existing component prescription and technology, problem to be solved by this invention is to provide a kind of Ni base noncrystal alloy component prescription and preparation method of high W content.
A kind of high W content Ni base noncrystal alloy of the present invention, by atomic fraction, comprises following component composition:
Ni60～69％，
W17～22％，
B13.5％。
A kind of high W content Ni base noncrystal alloy of the present invention, the Nb also containing 0 ~ 8% atomic fraction in alloy compositions.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, comprises the steps:
The first step: by the atomic fraction of the alloy compositions of design, join and get Ni, the powder of W, Nb, B; After mixing in ball mill, be pressed into briquet, then, at 850 ~ 900 DEG C of temperature, reduce pre-burning, make there is certain bonding strength between its powder particle, prevent from being blown by electric arc in fusion process flying;
Second step: the briquet after pre-burning is loaded in vacuum arc melting furnace, is evacuated to 1 × 10
-5pa, then fills high-purity argon gas to 0.05MPa, carries out at least 4 arc meltings, obtain mother alloy after molten titanium oxygen uptake;
3rd step: the mother alloy segmentation obtained by second step loads silica tube, is placed in vacuum and gets rid of band machine, gets rid of the high W content Ni base amorphous ribbon of band preparation.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, W metal powder size is 5 ~ 8 μm, metal W powder size 2.0 μm, and metal Nb powder size is Nb30 ~ 35 μm, and B powder size is 30 ~ 70 μm; Purity >=99.9% of tungsten powder, purity >=99.5% of nickel powder, purity >=99.9% of boron, purity >=99.9% of niobium powder.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, in the first step, drum's speed of rotation 200r/min, ball milling mixing time is 4 ~ 6 hours.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, forming pressure when being pressed into briquet is 150 ~ 200MPa
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, in the first step, described pre-burning atmosphere is hydrogen atmosphere, burn-in time 1 ~ 1.5h.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, in second step, arc melting is vacuum non-consumable arc melting, and arc melting number of times is 4-6 time.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, in the 3rd step, getting rid of band machine copper roller rotating speed is 30m/s, and the high W content Ni base amorphous ribbon width of preparation is 2 ~ 4mm, and thickness is 15 ~ 40 μm.
The preparation method of a kind of high W content Ni base noncrystal alloy of the present invention, the high W content Ni base noncrystal alloy crystallization temperature 782 ~ 851K of preparation; Microhardness 8.5 ~ 11.2Gpa.
The advantage of high W content Ni base noncrystal alloy of the present invention is as follows:
1, amorphous component is simple, is convenient to preparation; Non precious metal, cost is lower; The constituent contents such as little atomic radius B are lower, and decrease in arc melting process and volatilize, alloying constituent control accuracy is high;
2, under high temperature, W has higher solubility in Ni, and in arc melting process, tungsten powder Particle Phase is more readily soluble in Ni for larger tungsten metal blocks, overcomes when tungsten block carries out arc melting that smelting time is long, often, power is high, consume energy large shortcoming;
3, under 850 DEG C ~ 900 DEG C hydrogen atmospheres, sinter 1 ~ 1.5h, increase the bonding strength of powder compact, partial oxide and aqueous vapor can be removed simultaneously, prevent powder from easily being blown under arc melting and fly, improve the controllability of alloying constituent further;
4, Heat stability is good, has higher crystallization temperature 782 ~ 851K; Microhardness is high, 8.5 ~ 11.2GPa.
5, the non-crystaline amorphous metal that prepared by the present invention can be applicable to friction and corrosion resistant material field.
In sum, although its crystallization temperature of Ni base noncrystal alloy of a kind of high W content of the present invention and microhardness are a little less than tungsten amorphous alloy, but amorphous alloy component of the present invention is relatively simple, non precious metal composition, cost is lower, and still has higher crystallization temperature and microhardness, its brilliant crystallization temperature 782 ~ 851K, high 8.5 ~ the 11.2Gpa of microhardness, has broad application prospects in friction and corrosion resistant material.Meanwhile, arc melting method of the present invention has positive reference at refractory metal alloy melting fermentation.The present invention adopts arc melting powder pre-burning body preparation mother alloy, overcome smelting time when larger tungsten block carries out arc melting long, often, power is high, consume energy large shortcoming, and prevents from powder from easily being blown under arc melting flying, improve the controllability of alloying constituent.
Accompanying drawing explanation
Accompanying drawing 1 is the XRD curve of high W content Ni base noncrystal alloy in embodiment 1.
Accompanying drawing 2 is TEM and the selected diffraction picture of high W content Ni base noncrystal alloy in embodiment 1.
Accompanying drawing 3 is the DSC curve of high W content Ni base noncrystal alloy in embodiment 1.
Accompanying drawing 4 is the XRD curve of high W content Ni base noncrystal alloy in embodiment 4.
Accompanying drawing 5 is TEM and the selected diffraction picture of high W content Ni base noncrystal alloy in embodiment 4.
Accompanying drawing 6 is the DSC curve of high W content Ni base noncrystal alloy in embodiment 4.
As can be seen from Figure 1, near 2 θ=45 °, there is a wide disperse bag, without obvious Bragg diffraction peak on XRD curve, show that this alloy is non-crystal structure.
As can be seen from high-resolution-ration transmission electric-lens and the selected area electron diffraction picture of Fig. 2, the arrangement of its alloy atom is disorderly and unsystematic, corresponding selected diffraction style only has the ring of disperse and wider dizzy composition, without the diffraction spot feature of crystalline structure, show that it is complete non-crystal structure, consistent with XRD test result.
As can be seen from the DSC curve of Fig. 3, its crystallization temperature Tx, up to 782K, shows that amorphous has higher stability.
Without obviously separating out peak on the XRD curve of accompanying drawing 4, what show prepared by embodiment 4 is non-crystal structure material.
Fig. 5 and Fig. 2 is similar, high resolution transmission picture atomic arrangement chaotic, and selected diffraction style only has the ring of disperse and wider dizzy composition, proves that it is non-crystal structure further.
The DSC curve of Fig. 6 can be found out, its crystallization temperature Tx is up to 820K, and amorphous has higher stability.
Embodiment
Be intended to further illustrate the present invention below in conjunction with embodiment, and unrestricted the present invention.
The material prepared in the embodiment of the present invention adopts XRD and tem analysis alloying constituent, adopts micro-vickers hardness instrument to measure amorphous microhardness, adopts differential thermal analyzer to measure the crystallization temperature of amorphous ribbon.
Embodiment 1
(1) by atomic fraction, Ni content is 68.6%, W content be 17.9%, B content is 13.5%, preparation 50g material.
(2) batching is placed in roller ball mill mixing 6h, rotating speed 200r/min, then briquetting under 200MPa, blank diameter is 20mm, pre-burning 1.5h under 850 DEG C of hydrogen atmospheres, divides and comes out of the stove for three times, avoids oxidation.
(3) pressed compact after pre-burning is loaded in non-consumable vacuum arc melting furnace, be evacuated to 1 × 10
-5pa, then fills high-purity argon gas to 0.05MPa, carries out 6 arc meltings after molten titanium oxygen uptake.
(4) uniform for 4g melting mother alloy is loaded silica tube, be placed in vacuum and get rid of the amorphous ribbon that band machine prepares high W content, copper roller rotating speed is 30m/s.Adopting micro-vickers hardness instrument to record its microhardness is 8.5GPa, and adopting differential thermal analyzer to record its crystallization temperature is 782K.
Embodiment 2
(1) by atomic fraction, Ni content is 66.6%, W content be 19.9%, B content is 13.5%, preparation 50g material.
(2) batching is placed in roller ball mill mixing 6h, rotating speed 200r/min, then briquetting under 200MPa, blank diameter is 20mm, pre-burning 1.5h under 860 DEG C of hydrogen atmospheres, divides and comes out of the stove for three times, avoids oxidation.
(3) pressed compact after pre-burning is loaded in non-consumable vacuum arc melting furnace, be evacuated to 1 × 10
-5pa, then fills high-purity argon gas to 0.05MPa, carries out 6 arc meltings after molten titanium oxygen uptake.
(4) uniform for 5g melting mother alloy is loaded silica tube, be placed in vacuum and get rid of the amorphous ribbon that band machine prepares high W content, copper roller rotating speed is 30m/s.Adopting micro-vickers hardness instrument to record its microhardness is 10.2GPa, and adopting differential thermal analyzer to record its crystallization temperature is 807K.
Embodiment 3
(1) by atomic fraction, Ni content is 60.6%, W content be 17.9%, Nb content be 8%, B content is 13.5%, preparation 55g material.
(2) batching is placed in roller ball mill mixing 6h, rotating speed 200r/min, then briquetting under 200MPa, blank diameter is 20mm, pre-burning 1.5h under 900 DEG C of hydrogen atmospheres, divides and comes out of the stove for three times, avoids oxidation.
(3) pressed compact after pre-burning is loaded in non-consumable vacuum arc melting furnace, be evacuated to 1 × 10
-5pa, then fills high-purity argon gas to 0.05MPa, carries out 6 arc meltings after molten titanium oxygen uptake.
(4) uniform for 6g melting mother alloy is loaded silica tube, be placed in vacuum and get rid of the amorphous ribbon that band machine prepares high W content, copper roller rotating speed is 30m/s.Adopting micro-vickers hardness instrument to record its microhardness is 10.1GPa, and adopting differential thermal analyzer to record its crystallization temperature is 851K.
Embodiment 4
(1) by atomic fraction, Ni content is 64.6%, W content be 21.9%, B content is 13.5%, preparation 60g material.
(2) batching is placed in roller ball mill mixing 6h, rotating speed 200r/min, then briquetting under 200MPa, blank diameter is 20mm, pre-burning 1.5h under 900 DEG C of hydrogen atmospheres, divides and comes out of the stove for three times, avoids oxidation.
(3) pressed compact after pre-burning is loaded in non-consumable vacuum arc melting furnace, be evacuated to 1 × 10
-5pa, then fills high-purity argon gas to 0.05MPa, carries out 6 arc meltings after molten titanium oxygen uptake.
(4) uniform for 5g melting mother alloy is loaded silica tube, be placed in vacuum and get rid of the amorphous ribbon that band machine prepares high W content, copper roller rotating speed is 30m/s.Adopting micro-vickers hardness instrument to record its microhardness is 11.2GPa, and adopting differential thermal analyzer to record its crystallization temperature is 820K.
Although its crystallization temperature of Ni base noncrystal alloy of a kind of high W content of the present invention and microhardness are a little less than tungsten amorphous alloy, but amorphous alloy component of the present invention is relatively simple, non precious metal composition, cost is lower, and still there is higher crystallization temperature and microhardness, its brilliant crystallization temperature 782 ~ 851K, the high 8.5 ~ 11.2GPa of microhardness, have broad application prospects in friction and corrosion resistant material.Meanwhile, arc melting method of the present invention has positive reference at refractory metal alloy melting fermentation.The present invention adopts arc melting powder pre-burning body preparation mother alloy, overcome smelting time when larger tungsten block carries out arc melting long, often, power is high, consume energy large shortcoming, and prevents from powder from easily being blown under arc melting flying, improve the controllability of alloying constituent.
Claims (8)
1. a preparation method for high W content Ni base noncrystal alloy, comprises the steps:
The first step: by the atomic fraction of the alloy compositions of design, join and get Ni, the powder of W, Nb, B; After mixing in ball mill, be pressed into briquet, then, at 850 ~ 900 DEG C of temperature, reduce pre-burning;
The atomic fraction of alloy compositions is: Ni60 ~ 69%, W17 ~ 22%, B13.5%, Nb0 ~ 8%;
Second step: the briquet after pre-burning is loaded in vacuum arc melting furnace, is evacuated to 1 × 10
-5pa, then fills high-purity argon gas to 0.05MPa, carries out at least 4 arc meltings, obtain mother alloy after molten titanium oxygen uptake;
3rd step: the mother alloy segmentation obtained by second step loads silica tube, is placed in vacuum and gets rid of band machine, gets rid of the high W content Ni base amorphous ribbon of band preparation.
2. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 1, it is characterized in that: W metal powder size is 5 ~ 8 μm, metal W powder size 2.0 μm, metal Nb powder size is 30 ~ 35 μm, and B powder size is 30 ~ 70 μm; Purity >=99.9% of tungsten powder, purity >=99.5% of nickel powder, purity >=99.9% of boron, purity >=99.9% of niobium powder.
3. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 1, it is characterized in that: in the first step, drum's speed of rotation 200r/min, ball milling mixing time is 4 ~ 6 hours.
4. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 3, is characterized in that: forming pressure when being pressed into briquet is 150 ~ 200MPa.
5. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 4, it is characterized in that: in the first step, described pre-burning atmosphere is hydrogen atmosphere, burn-in time 1 ~ 1.5h.
6. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 1, it is characterized in that: in second step, arc melting is vacuum non-consumable arc melting, and arc melting number of times is 4 ~ 6 times.
7. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 1, it is characterized in that: in the 3rd step, getting rid of band machine copper roller rotating speed is 30m/s, and the high W content Ni base amorphous ribbon width of preparation is 2 ~ 4mm, and thickness is 15 ~ 40 μm.
8. the preparation method of a kind of high W content Ni base noncrystal alloy according to claim 1-7 any one, is characterized in that: the high W content Ni base noncrystal alloy crystallization temperature 782 ~ 851K of preparation; Microhardness 8.5 ~ 11.2Gpa.
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| CN109399765B (en) * | 2017-08-16 | 2022-02-01 | 南京理工大学 | Method for electrochemically degrading azo dye wastewater by using amorphous alloy |
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| CN1142313C (en) * | 2000-11-22 | 2004-03-17 | 中国科学院金属研究所 | Nickel base amorphous alloy |
| CN101532153B (en) * | 2009-03-13 | 2011-07-06 | 甘军 | Amorphous nano-alloy plating layer of electrodeposition nickel-based series, electroplating liquid and electroplating process |
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