CN101871061A - Preparation method of massive nanocrystalline nickel aluminum alloy - Google Patents
Preparation method of massive nanocrystalline nickel aluminum alloy Download PDFInfo
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- CN101871061A CN101871061A CN 201010219672 CN201010219672A CN101871061A CN 101871061 A CN101871061 A CN 101871061A CN 201010219672 CN201010219672 CN 201010219672 CN 201010219672 A CN201010219672 A CN 201010219672A CN 101871061 A CN101871061 A CN 101871061A
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Abstract
The invention provides a preparation method of a massive nanocrystalline nickel aluminum alloy, and relates to a preparation method of a nickel aluminum alloy. The method solves the problems that the existing electric sedimentation method for preparing a nanocrystalline material only can prepare a thin-film material; the hot press sintering method has large energy source consumption, low production efficiency and high production cost; and the large plastic deformation method has strict requirements to the mould, the equipment and the deformation technology. The method comprises the following steps of: ball milling nickel powder and aluminum powder in a high-performance ball mill to obtain nickel aluminum alloy powder; filling the nickel aluminum alloy powder into a black lead mould; preheating in a pulse current sintering furnace; pressuring and heating; and keeping the maximum pressure and the highest temperature for 4-6min to obtain the massive nanocrystalline nickel aluminum alloy. The density of the massive nanocrystalline nickel aluminum alloy is larger than or equal to 99.7%, the depth of the massive material is larger than or equal to 10mm, the energy consumption is 10-20% of the hot press sintering method, and the equipment and the technology are simple. The method can be used for preparing the massive nanocrystalline nickel aluminum alloy.
Description
Technical field
The present invention relates to the preparation method of alumel.
Background technology
The NiAl base intermetallic compound has use temperature height, resistance to oxidation, low density advantage, thereby the candidate material that can be used as high-temperature structural material of future generation is widely used in fields such as aerospace and turbine blade.Grain refining is the effective ways that improve the performance of intermetallic compound, and the nanometer of material grains size can significantly improve the mechanical property of material.The method of existing preparation nano material has galvanic deposit, hot pressed sintering, sever Plastic Deformation, and electrodip process wherein can only prepare thin-film material, can't prepare the bulk nanocrystalline material, and the film maximum ga(u)ge of electrodip process preparation at present is the hundreds of micron; And hot pressing sintering method makes energy consumption big because heating-up time and soaking time are longer, and production efficiency is low, and the production cost height is guaranteeing to be unfavorable for the refinement of crystal grain on density and the homogeneous microstructure basis simultaneously.Sever Plastic Deformation has strict demand to mould, equipment, deformation technique, thereby has limited its range of application.So far do not have a kind of low cost, high efficiency bulk preparation of nanomaterials, seriously restricted the range of application of nano material.
Summary of the invention
The present invention is that the hot pressing sintering method energy consumption is big, production efficiency is low, production cost is high for the electrodip process that solves existing nano material can only prepare thin-film material, sever Plastic Deformation is to mould, equipment, the strict shortcoming of deformation technique, and the preparation method of massive nanocrystalline nickel aluminum alloy is provided.
The preparation method of massive nanocrystalline nickel aluminum alloy of the present invention carries out according to the following steps: one, take by weighing nickel powder and aluminium powder and mix by the atomic ratio 1:1 of nickel and aluminium and obtain mixed powder, measure dehydrated alcohol by 3%～5% of mixed powder volume again; Two, will join in the stirring-type high energy ball mill through the mixed powder of step 1 preparation with through the dehydrated alcohol that step 1 is measured, and feed argon shield again, be 10 ℃～40 ℃ in temperature
,Rotating speed is ball milling 20h～24h under 280 rev/mins～320 rev/mins the condition, obtains the alumel powder; Three, will be in the alumel powder of step 2 preparation be packed graphite jig into, in the pulse electric current sintering stove of again graphite jig being packed into, earlier with pulse electric current sintering stove evacuation to 1.0 * 10
-2Pa～1.5 * 10
-2Pa, energising is with power preheating 25min～35min of 450W～550W; Four, feeding intensity is 13A/mm
2～15A/mm
2, dutycycle is that 0.75 pulsed current carries out sintering, when feeding pulsed current, powder is pressurizeed, pressure increases gradually, make pressure and sintering temperature reach maximum value simultaneously, the maximum value of pressure is 45MPa ~ 55MPa, and the maximum value of sintering temperature is 1000 ℃ ~ 1200 ℃, keeps 4min～6min under the condition of peak pressure and top temperature, cool to room temperature then with the furnace, obtain massive nanocrystalline nickel aluminum alloy.
The present invention is earlier with nickel powder and aluminium powder high-energy ball milling, obtain the alumel powder of complete alloying and grain refining, and then with powder sintering that heats up gradually in pressurization gradually, heat up and pressurize synchronously, can guarantee in the temperature-rise period discharge of the gas that adsorbs in the powder, improve density, avoid because pressure is excessive at the beginning, the passage that causes gas to be discharged is blocked, and last gas forms the cavity.Simultaneously, because the volumetric shrinkage of powder in the sintering process, progressively pressurization can guarantee that push-down head contacts all the time with powder, has guaranteed the carrying out of discharge.Density 〉=99.7% of the massive nanocrystalline nickel aluminum alloy of method preparation of the present invention, thickness 〉=the 10mm of block materials, this method energy consumption is little, is 10% ~ 20% of hot pressing sintering method only, makes production efficiency improve production cost and reduces, do not need complex apparatus and technology simple.The massive nanocrystalline nickel aluminum alloy of this method preparation has the characteristics of density height, homogeneous microstructure, it is when room temperature, dependent variable is up to 17%, and compressive strength is up to 2400MPa, more than 300 ℃, material is no longer cracked, be uniform viscous deformation, in the time of 900 ℃, compressive strength is up to 400MPa, in the time of 1200 ℃, its compressive strength is up to 150MPa.
Description of drawings
Fig. 1 is the nano-crystal nickel aluminium alloy block material X-ray diffraction spectrogram of embodiment 18 preparations; Fig. 2 is the transmission electron microscope photo of the nano-crystal nickel aluminium alloy block material of embodiment 18 preparations; Fig. 3 is the hardness point optical photograph of the nano-crystal nickel aluminium alloy block material of embodiment 18 preparations; Fig. 4 is the relation curve of stress and strain of the nano-crystal nickel aluminium alloy block material of embodiment 18 preparation.
Embodiment
Embodiment one: the preparation method of the massive nanocrystalline nickel aluminum alloy of present embodiment carries out according to the following steps: one, take by weighing nickel powder and aluminium powder and mix by the atomic ratio 1:1 of nickel and aluminium and obtain mixed powder, measure dehydrated alcohol by 3%～5% of mixed powder volume again; Two, will join in the stirring-type high energy ball mill through the mixed powder of step 1 preparation with through the dehydrated alcohol that step 1 is measured, and feed argon shield again, be 10 ℃～40 ℃ in temperature
,Rotating speed is ball milling 20h～24h under 280 rev/mins～320 rev/mins the condition, obtains the alumel powder; Three, will be in the alumel powder of step 2 preparation be packed graphite jig into, in the pulse electric current sintering stove of again graphite jig being packed into, earlier with pulse electric current sintering stove evacuation to 1.0 * 10
-2Pa～1.5 * 10
-2Pa, energising is with power preheating 25min～35min of 450W～550W; Four, feeding strength of current is 13A/mm
2～15A/mm
2, dutycycle is that 0.75 pulsed current carries out sintering, when feeding pulsed current, powder is pressurizeed, pressure increases gradually, make pressure and sintering temperature reach maximum value simultaneously, the maximum value of pressure is 45MPa ~ 55MPa, and the maximum value of sintering temperature is 1000 ℃ ~ 1200 ℃, keeps 4min～6min under the condition of peak pressure and top temperature, cool to room temperature then with the furnace, obtain massive nanocrystalline nickel aluminum alloy.
Present embodiment is earlier with nickel powder and aluminium powder high-energy ball milling, obtain the alumel powder of complete alloying and grain refining, and then with powder sintering that heats up gradually in pressurization gradually, (heat up and pressurize synchronously, can guarantee in the temperature-rise period discharge of the gas that adsorbs in the powder, improve density, avoid because pressure is excessive at the beginning, the passage that causes gas to be discharged is blocked, and last gas forms the cavity.Simultaneously, because the volumetric shrinkage of powder in the sintering process, progressively pressurization can guarantee that push-down head contacts all the time with powder, has guaranteed the carrying out of discharge.Density 〉=99.7% of the massive nanocrystalline nickel aluminum alloy of the method preparation of present embodiment, thickness 〉=the 10mm of block materials, this method energy consumption is little, is 10% ~ 20% of hot pressing sintering method only, makes production efficiency improve production cost and reduces, do not need complex apparatus and technology simple.The massive nanocrystalline nickel aluminum alloy of this method preparation has the characteristics of density height, homogeneous microstructure, it is when room temperature, dependent variable is up to 17%, and compressive strength is up to 2400MPa, more than 300 ℃, material is no longer cracked, be uniform viscous deformation, in the time of 900 ℃, compressive strength is up to 400MPa, in the time of 1200 ℃, its compressive strength is up to 150MPa.
Embodiment two: what present embodiment and embodiment one were different is: the amount of dehydrated alcohol is 3.5%～4.5% of nickel powder and an aluminium powder mixed powder volume in the step 1.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: the amount of dehydrated alcohol is 4.0% of nickel powder and an aluminium powder mixed powder volume in the step 1.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different with one of embodiment one to three is: the temperature of high energy ball mill is 15 ℃～35 ℃ in the step 2
,Rotating speed is that 290 rev/mins～310 rev/mins, ball milling time are 21h～23h.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one to four is: the temperature of high energy ball mill is 20 ℃ in the step 2
,Rotating speed is that 300 rev/mins, ball milling time are 22h.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to five is: the vacuum tightness of pulse electric current sintering stove is 1.1 * 10 in the step 3
-2Pa～1.4 * 10
-2Pa.Other is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: the vacuum tightness of pulse electric current sintering stove is 1.3 * 10 in the step 3
-2Pa.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different with one of embodiment one to seven is: electric power is that 460W～530W, warm up time are 28min～33min in the step 3.Other is identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different with one of embodiment one to eight is: electric power is that 500W, warm up time are 30min in the step 3.Other is identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different with one of embodiment one to nine is: the strength of current of pulsed current is 13.5A/mm in the step 4
2～14.5A/mm
2Other is identical with one of embodiment one to nine.
Embodiment 11: what present embodiment was different with one of embodiment one to ten is: the strength of current of pulsed current is 14A/mm in the step 4
2Other is identical with one of embodiment one to ten.
Embodiment 12: what present embodiment was different with one of embodiment one to 11 is: the maximum value of pressure is 47MPa ~ 53MPa in the step 4.Other is identical with one of embodiment one to 11.
Embodiment 13: what present embodiment was different with one of embodiment one to 12 is: the maximum value of pressure is 50MPa in the step 4.Other is identical with one of embodiment one to 12.
Embodiment 14: what present embodiment was different with one of embodiment one to 13 is: the maximum value of sintering temperature is 1030 ℃ ~ 1180 ℃ in the step 4.Other is identical with one of embodiment one to 13.
Embodiment 15: what present embodiment was different with one of embodiment one to 14 is: the maximum value of sintering temperature is 1100 ℃ in the step 4.Other is identical with one of embodiment one to 14.
Embodiment 16: what present embodiment was different with one of embodiment one to 15 is: keep 4.5min～5.5min in the step 4 under the condition of peak pressure and top temperature.Other is identical with one of embodiment one to 15.
Embodiment 17: what present embodiment was different with one of embodiment one to 16 is: keep 5min in the step 4 under the condition of peak pressure and top temperature.Other is identical with one of embodiment one to 16.
Embodiment 18: what present embodiment was different with one of embodiment one to 17 is: the fineness of nickel powder and aluminium powder is 200 orders ~ 400 orders in the step 1.Other is identical with one of embodiment one to 17.
Embodiment 19: what present embodiment was different with one of embodiment one to 18 is: the fineness of nickel powder and aluminium powder is 325 orders in the step 1.Other is identical with one of embodiment one to 18.
Embodiment 20: the preparation method of the massive nanocrystalline nickel aluminum alloy of present embodiment carries out according to the following steps: one, take by weighing 300 purpose nickel powders and 300 purpose aluminium powders and mix by the atomic ratio 1:1 of nickel and aluminium and obtain mixed powder, measure dehydrated alcohol by 4% of mixed powder volume again; Two, will join in the stirring-type high energy ball mill through the mixed powder of step preparation with through the dehydrated alcohol that step 1 takes by weighing, again by accounting for the feeding argon shield, in temperature is that 20 ℃, rotating speed are ball milling 22h under 300 rev/mins the condition, obtains the nickel ferroaluminium powder of complete alloying and grain refining; Three, will be in the nickel ferroaluminium powder of step 2 preparation to be packed graphite jig into, in the pulse electric current sintering stove of again graphite jig being packed into, the pulsed current of setting the pulse electric current sintering stove earlier is 14A/mm
2, the dutycycle of pulsed current is 0.75; Four, earlier with pulse electric current sintering stove evacuation to 1.3 * 10
-2Pa, energising is with the power preheating 30min of 500W; And then the pulse electric current sintering that feeds, in the pulsed current that feeds, powder is pressurizeed, pressure increases gradually, make pressure and sintering temperature reach maximum value simultaneously, the maximum value of pressure is 50MPa, and the maximum value of sintering temperature is 1100 ℃, keeps 5min under the condition of peak pressure and top temperature, cool to room temperature then with the furnace, obtain massive nanocrystalline nickel aluminum alloy.
The massive nanocrystalline nickel aluminum alloy that present embodiment obtains utilizes the X-ray diffraction analysis instrument of RigakuD type to analyze, the X-ray diffraction spectrogram that obtains as shown in Figure 1, as can be seen from Figure 1, massive nanocrystalline nickel aluminum alloy is made of mutually β-NiAl fully;
The massive nanocrystalline nickel aluminum alloy that present embodiment obtains utilizes FEITECNHIG2F30 TEM (transmission electron microscope) analysis instrument to analyze, the transmission electron microscope photo of gained as shown in Figure 2, as can be seen from Figure 2, the transmission light field mutually in, crystal grain is nearly equiax crystal, and average grain size is about 100nm;
The massive nanocrystalline nickel aluminum alloy that present embodiment obtains utilizes model to be HVS-5 hardness test machine, load is 1000g, dwell time is 10s, measuring 5 points averages, obtaining its Vickers' hardness mean value is HV=627.20, wherein the hardness point optical photograph of hardness test as shown in Figure 3, as can be seen from Figure 3, the diagonal position of hardness point, flawless produces.
The massive nanocrystalline nickel aluminum alloy utilization that present embodiment obtains is tested its compressive strength at the Gleeble1500D hot modeling test machine, and specimen size is 4mm * 4mm * 6mm, and specimen surface is handled with 400 order sand paperings.The heat-up rate of hot modeling test machine is 10 ℃/s, soaking time 10s.Range of measuring temp is a room temperature to 1200 ℃.Obtain in room temperature, 300 ℃, 750 ℃, 900 ℃, 1000 ℃, the relation curve of stress and strain as shown in Figure 4 under 1200 ℃ the condition, as can be seen from Figure 4, massive nanocrystalline nickel aluminum alloy is when room temperature, dependent variable reaches 17%, compressive strength reaches 2400MPa, more than 300 ℃, material is no longer cracked, is uniform viscous deformation, in the time of 900 ℃, compressive strength is 400MPa, and in the time of 1200 ℃, its compressive strength is 150MPa, the intensity of material is greatly improved, compare with the as cast condition coarse-grain, room temperature strength has improved about 1400MPa, and the room temperature dependent variable has also brought up to 12%.
Density 〉=99.7% of the nano-crystal nickel aluminium alloy block material of method preparation of the present invention, the thickness 〉=10mm of block materials, this method institute energy requirement only is a hot pressing sintering method 13.8%.
Claims (10)
1. the preparation method of massive nanocrystalline nickel aluminum alloy, the preparation method who it is characterized in that massive nanocrystalline nickel aluminum alloy carries out according to the following steps: one, take by weighing nickel powder and aluminium powder and mix by the atomic ratio 1:1 of nickel and aluminium and obtain mixed powder, measure dehydrated alcohol by 3%～5% of mixed powder volume again; Two, will join in the stirring-type high energy ball mill through the mixed powder of step 1 preparation with through the dehydrated alcohol that step 1 is measured, and feed argon shield again, be 10 ℃～40 ℃ in temperature
,Rotating speed is ball milling 20h～24h under 280 rev/mins～320 rev/mins the condition, obtains the alumel powder; Three, will be in the alumel powder of step 2 preparation be packed graphite jig into, in the pulse electric current sintering stove of again graphite jig being packed into, earlier with pulse electric current sintering stove evacuation to 1.0 * 10
-2Pa～1.5 * 10
-2Pa, energising is with power preheating 25min～35min of 450W～550W; Four, feeding intensity is 13A/mm
2～15A/mm
2, dutycycle is that 0.75 pulsed current carries out sintering, when feeding pulsed current, powder is pressurizeed, pressure increases gradually, make pressure and sintering temperature reach maximum value simultaneously, the maximum value of pressure is 45MPa ~ 55MPa, and the maximum value of sintering temperature is 1000 ℃ ~ 1200 ℃, keeps 4min～6min under the condition of peak pressure and top temperature, cool to room temperature then with the furnace, obtain massive nanocrystalline nickel aluminum alloy.
2. the preparation method of massive nanocrystalline nickel aluminum alloy according to claim 1, the amount that it is characterized in that dehydrated alcohol in the step 1 is 3.5%～4.5% of nickel powder and an aluminium powder mixed powder volume.
3. the preparation method of massive nanocrystalline nickel aluminum alloy according to claim 1 and 2, the temperature that it is characterized in that high energy ball mill in the step 2 is 15 ℃～35 ℃
,Rotating speed is that 290 rev/mins～310 rev/mins, ball milling time are 21h～23h.
4. the preparation method of massive nanocrystalline nickel aluminum alloy according to claim 3, the vacuum tightness that it is characterized in that pulse electric current sintering stove in the step 3 is 1.1 * 10
-2Pa～1.4 * 10
-2Pa.
5. according to the preparation method of claim 1,2 or 4 described massive nanocrystalline nickel aluminum alloys, it is characterized in that electric power is that 460W～530W, warm up time are 28min～33min in the step 3.
6. the preparation method of massive nanocrystalline nickel aluminum alloy according to claim 5, the strength of current that it is characterized in that pulsed current in the step 4 is 13.5A/mm
2～14.5A/mm
2
7. according to the preparation method of claim 1,2,4 or 6 described massive nanocrystalline nickel aluminum alloys, the strength of current that it is characterized in that pulsed current in the step 4 is 13.5A/mm
2～14.5A/mm
2
8. the preparation method of massive nanocrystalline nickel aluminum alloy according to claim 7, the maximum value that it is characterized in that pressure in the step 4 is 47MPa ~ 53MPa.
9. according to the preparation method of claim 1,2,4,6 or 8 described massive nanocrystalline nickel aluminum alloys, the maximum value that it is characterized in that sintering temperature in the step 4 is 1030 ℃ ~ 1180 ℃.
10. the preparation method of massive nanocrystalline nickel aluminum alloy according to claim 7 is characterized in that keeping 4.5min～5.5min in the step 4 under the condition of peak pressure and top temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182806A (en) * | 2011-12-30 | 2013-07-03 | 财团法人金属工业研究发展中心 | Working die and plated film layer |
| CN103773984A (en) * | 2014-01-23 | 2014-05-07 | 上海交通大学 | Powder metallurgy method for preparing superfine crystalline alloy by use of micro-nano laminated sheet |
| CN103774149A (en) * | 2014-02-10 | 2014-05-07 | 天津工业大学 | Preparation method of high-strength nano-porous nickel film |
| CN106591629A (en) * | 2016-12-20 | 2017-04-26 | 南京九致信息科技有限公司 | Flame-retardant aluminum-nickel alloy material and preparation method thereof |
| CN109396449A (en) * | 2018-09-30 | 2019-03-01 | 东北大学 | One kind preparing Ni by raw material of Ni-Al mixed-powder3The method of Al intermetallic compound powder |
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| CN1410571A (en) * | 2002-10-22 | 2003-04-16 | 中国科学院兰州化学物理研究所 | Preparation method of large nano crystal nickel aluminium intermetallic compound |
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| CN1410571A (en) * | 2002-10-22 | 2003-04-16 | 中国科学院兰州化学物理研究所 | Preparation method of large nano crystal nickel aluminium intermetallic compound |
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| 《Intermetallics》 20100113 Chunping Zhang et al. Dependence of heating rate in PCAS on microstructures and high temperature deformation properties of -TiAl intermetallic alloys 834-840 1-10 第8卷, 第5期 2 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182806A (en) * | 2011-12-30 | 2013-07-03 | 财团法人金属工业研究发展中心 | Working die and plated film layer |
| CN103182806B (en) * | 2011-12-30 | 2016-01-20 | 财团法人金属工业研究发展中心 | Work mould and film plating layer |
| CN103773984A (en) * | 2014-01-23 | 2014-05-07 | 上海交通大学 | Powder metallurgy method for preparing superfine crystalline alloy by use of micro-nano laminated sheet |
| CN103773984B (en) * | 2014-01-23 | 2015-10-14 | 上海交通大学 | The powder metallurgy process of Ultra-fine Grained alloy prepared by a kind of micro-nano lamination |
| CN103774149A (en) * | 2014-02-10 | 2014-05-07 | 天津工业大学 | Preparation method of high-strength nano-porous nickel film |
| CN106591629A (en) * | 2016-12-20 | 2017-04-26 | 南京九致信息科技有限公司 | Flame-retardant aluminum-nickel alloy material and preparation method thereof |
| CN109396449A (en) * | 2018-09-30 | 2019-03-01 | 东北大学 | One kind preparing Ni by raw material of Ni-Al mixed-powder3The method of Al intermetallic compound powder |
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Open date: 20101027 |