CN105568072B - Preparation method for Al-Pd-Mn quasicrystal - Google Patents
Preparation method for Al-Pd-Mn quasicrystal Download PDFInfo
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- CN105568072B CN105568072B CN201610008752.1A CN201610008752A CN105568072B CN 105568072 B CN105568072 B CN 105568072B CN 201610008752 A CN201610008752 A CN 201610008752A CN 105568072 B CN105568072 B CN 105568072B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention relates to a preparation method for a Al-Pd-Mn quasicrystal. The Al-Pd-Mn quasicrystal includes, by atomic ratio, 70%-72% of Al, 18%-21% of Pd and 7%-12% of Mn. The method includes the steps that high-purity Al powder, high-purity Pd powder and high-purity Mn powder are evenly mixed, injected into a hard alloy mould, and pressed in a hydraulic tablet press under 2-4 MPa for 100-300 seconds to obtain a reserved block; the reserved block is mounted into a boron nitride crucible, a pre-dried tubular graphite oven body, the boron nitride crucible, a boron nitride piece, a pyrophyllite piece and a graphite piece are assembled and placed in a six-surface diamond presser, setting pressure is controlled to be isostatic pressure ranging from 3 GPa to 6 GPa, and the temperature is controlled to rise to 850-950 DEG C and kept for 30-60 minutes; and the temperature is decreased to 650-850 DEG C and is kept for two to six hours. The preparation method is simple in process, low in energy consumption and high in efficiency; the quasicrystal is prepared from the raw materials at a time only with conventional equipment; the prepared quasicrystal has excellent quality performance and good mechanical performance and can be widely applied.
Description
Technical field
The invention belongs to technical field of metal, especially a kind of preparation method of quasi-crystalline substance.
Background technology
Al-Mns of the Israel scientist D.Shechtman in NBS's work in 1984 in rapid solidification
A kind of peculiar phase-icosahedral phase with metalline is found that in bianry alloy, this is a kind of new crystallography knot
Structure.The electron diffraction spot of this cenotype is quite bright and sharp, and shows five rotational symmetries not permitted in crystal structure,
Therefore cannot be gone to demarcate with any Bravais lattice.This cenotype is that one kind has long-range translational order paracycle and amorphous
The solid-state ordered phase of body rotational symmetry, is referred to as quickly Icosahedral phases.It is dense that the special structure of quasi-crystalline substance causes people
Interest, and promote researcher that quasi-crystalline substance is found in related system.Initially several years, research system was concentrated mainly on binary system and very
Find that these quasi-crystalline substances are all metastable phases soon.Quickly research system expands to ternary system, and is found that some stable Icosahedral phases,
Wherein Al-Pd-Mn is exactly one of typical system.Initially, icosahedron Al-Pd-Mn systems Icosahedral phases are by the molten dress of quenching of single roller
Put (referred to as the getting rid of band method) of the realization of (single roller melt spinning apparatus) flash set technology.Cut-off
At present, obtaining the additive method of Al-Pd-Mn system Icosahedral phases has：Czochralski method (Czochralski method), Bridgman method
(Bridgman method), from flux growth metrhod (self-flux method) and float-zone method (Floating zone method).
It is not fine and close by getting rid of the quasicrystal with method acquisition, easily there are the defects such as hole.Afterwards several method can obtain high-quality monocrystalline,
However it is necessary that extremely strict sample pretreatment and will be to precise controls such as acid extractions.
The content of the invention
Present invention aim at providing a kind of preparation of the high Al-Pd-Mn quasi-crystalline substances of process is simple, efficient, Icosahedral phases content
Method.The present invention mainly prepares Al-Pd-Mn quasi-crystalline substances using high-pressure process, directly by pressure act on uniform mixing and in plus
On Al, Pd, Mn mixed material of hot melt state, according to design temperature, pressure, reaction duration starts cubic hinge press can be straight
Connect prepared single-phase, the quasi-crystalline substance block containing large scale crystal grain.
Technical scheme is as follows：
(1) atom ratio of the chemical composition of Al-Pd-Mn quasi-crystalline substances is：Al 70-72%, Pd 18-21%, Mn 7-
12%, described Al, Pd, Mn are high pure metal powder；It is optimized and is divided into Al71Pd20Mn9。
(2) high-purity Al powder, Pd powder, Mn powder is fully ground after being well mixed and is fitted in sintered-carbide die, in hydraulic pressure
Pressurize 100-300s in tablet press machine under 2-4MPa, and preparation block is obtained；
(3) graphite furnace tubulose body of heater two ends are sealed with pyrophillite piece, boron nitride crucible, crucible two ends is set with graphite furnace
Sealed with boron nitride piece, while graphite furnace two ends graphite flake is used as parcel and conduction, then by above described tubular graphite body of heater, nitrogen
Pyrophillite square and conductive steel that change boron crucible, boron nitride piece, pyrophillite piece and graphite flake are used together with cubic hinge press
Bowl is put in more than drying 2-4 hours standby in the drying baker that temperature is 100-200 DEG C.
(4) the prepared block of step (2) is fitted in boron nitride crucible and by the tubular graphene stove of step (3) prebake
The assembling of body, boron nitride crucible, boron nitride piece, pyrophillite piece and graphite flake, in being positioned over cubic hinge press, sets Stress control
In 3-6GPa isostatic presseds, control temperature is heated between 850 DEG C -950 DEG C, is incubated 30-60min；Treat that temperature is down to 650-850
DEG C, it is incubated 2-6h.
The present invention has the advantage that compared with prior art：
1st, process is simple, energy consumption be low, efficiency high, settles at one go from raw material to quasi-crystalline substance, only need to adopt conventional high-pressure equipment.
2nd, obtained Icosahedral phases content is high, superior in quality.
Figure of description
Fig. 1 is quasi-crystalline substance XRD obtained by the embodiment of the present invention 1.
Fig. 2 is Al in the embodiment of the present invention 171Pd20Mn9The weight symmetry direction of principal axis diffraction pattern figure of quasi-crystalline substance 2.
Fig. 3 is Al in the embodiment of the present invention 171Pd20Mn9The weight symmetry direction of principal axis diffraction pattern figure of quasi-crystalline substance 3.
Fig. 4 is Al in the embodiment of the present invention 171Pd20Mn9The weight symmetry direction of principal axis diffraction pattern figure of quasi-crystalline substance 5.
Fig. 5 is the High-Resolution Map of quasi-crystalline substance TEM obtained by the embodiment of the present invention 2.
Fig. 6 is quasi-crystalline substance SEM figure obtained by the embodiment of the present invention 2.
Fig. 7 is quasi-crystalline substance SEM figure obtained by the embodiment of the present invention 3.
Specific embodiment
Embodiment 1
(1) calculate by atom ratio and weigh high-purity Al powder, Pd powder, Mn powder raw materials, its weight be respectively 1.0076g,
1.1194g, 0.2601g are (according to Al71Pd20Mn9Weigh), above-mentioned powder is positioned in mortar to be fully ground it is well mixed dress
In internal diameter is for the sintered-carbide die of Φ 10.6mm, the 120s when 4Mpa that pressurizes in hydraulic pressure tablet press machine is obtains diameter of phi
The simple and mechanical pressing high pressure preparation block of 10.6mm thickness 7.6mm.
(2) graphite furnace is high 16.6mm external diameters Φ 14mm internal diameters Φ 12.1mm tubulose bodies of heater, and two ends are thick with Φ 12.06mm
3.3mm pyrophillites piece is sealed, and is set with boron nitride crucible in graphite furnace, the high 10mm external diameters Φ 12mm internal diameters Φ 10.8mm of crucible, and two
End is sealed with diameter of phi 10.75mm thickness 1.2mm boron nitride piece, while graphite furnace two ends parcel and conduction graphite flake specification are straight
The thickness 1.6mm of footpath Φ 14.By above described tubular graphite body of heater, boron nitride crucible, boron nitride piece, pyrophillite piece and graphite flake together with six
The pyrophillite square and Conducting steel bowl that face high pressure apparatus is used be put in the drying baker that temperature is 180 DEG C dry more than 3 hours it is standby
With.
(3) preparation block will be fitted in boron nitride crucible and by the tubular graphene of step (2) prebake obtained in step (1)
Body of heater, boron nitride crucible, boron nitride piece, pyrophillite piece and graphite flake assembling, in being positioned over cubic hinge press, set pressure as
5GPa isostatic presseds；Temperature is heated to 900 DEG C, is incubated 30min；Treat that temperature is down to 750 DEG C, be incubated 2h.
(4) directly turn-off current stops heating after insulation terminates.
(5) block is taken out, BN is remained outside careful peel sample, clean surface obtains Al71Pd20Mn9Quasi-crystalline substance.
To the row XRD sweep tests of quasi-crystalline substance Jing, composition is determined, as shown in Figure 1, it can be seen that significantly Al71Pd20Mn9Diffraction
Peak, and it is leading to may determine that Icosahedral phases are accounted for.
It is illustrated in figure 22 weight symmetry direction of principal axis diffraction spots of quasi-crystalline substance；As shown in Figure 33 weight symmetry direction of principal axis of quasi-crystalline substance spread out
Penetrate spot；5 weight symmetry direction of principal axis diffraction spots of quasi-crystalline substance as shown in Figure 4.The electronic diffraction tool of crystal grain may certify that by Fig. 2-4
There is icosahedron symmetry, crystal grain is icosahedral quasicrystal.
The Atomic Arrangement that the weight symmetry direction of quasi-crystalline substance five is observed is illustrated in figure 5, this confirms observed crystal grain from the real space
For quasicrystal particle.
As shown in fig. 6, being the granular grows pattern observed under SEM ESEMs, the geometric shape of rule is particularly
Pentagonal profile gives the dynamic information of quasicrystal particle growth.
Embodiment 2
(1) calculate by atom ratio and weigh high-purity Al powder, Pd powder, Mn powder raw materials, its weight be respectively 1.0700g,
1.0551g, 0.3631g are (according to Al72Pd18Mn12Weigh), above-mentioned powder is positioned in mortar to be fully ground it is well mixed dress
In internal diameter is for the sintered-carbide die of Φ 10.6mm, the 300s when 2Mpa that pressurizes in hydraulic pressure tablet press machine is obtains diameter of phi
The simple and mechanical pressing high pressure preparation block of 10.6mm thickness 7.6mm.
(2) graphite furnace is high 16.6mm external diameters Φ 14mm internal diameters Φ 12.1mm tubulose bodies of heater, and two ends are thick with Φ 12.06mm
3.3mm pyrophillites piece is sealed, and is set with boron nitride crucible in graphite furnace, the high 10mm external diameters Φ 12mm internal diameters Φ 10.8mm of crucible, and two
End is sealed with diameter of phi 10.75mm thickness 1.2mm boron nitride piece, while graphite furnace two ends parcel and conduction graphite flake specification are straight
The thickness 1.6mm of footpath Φ 14.By above-mentioned tubular graphene body of heater, boron nitride crucible, boron nitride piece, pyrophillite piece and stone for testing
The pyrophillite square and Conducting steel bowl that ink sheet is used together with cubic hinge press is put in the drying baker that temperature is 100 DEG C dries 4
It is standby more than hour.
(3) preparation block will be fitted in boron nitride crucible and by the tubular graphene of step (2) prebake obtained in step (1)
Body of heater, boron nitride crucible, boron nitride piece, pyrophillite piece and graphite flake assembling, in being positioned over cubic hinge press, set pressure as
3GPa isostatic presseds；Temperature is heated to 950 DEG C, is incubated 60min；Treat that temperature is down to 650 DEG C, be incubated 6h.
(4) directly turn-off current stops heating after insulation terminates.
(5) block is taken out, BN is remained outside careful peel sample, clean surface obtains Al72Pd18Mn12Quasi-crystalline substance.
As shown in Figure 5, it can be seen that obvious five weight symmetry, thus may determine that having synthesized Icosahedral phases.As shown in fig. 6,
In figure rule geometric shape can also judge synthesize for quasi-crystalline substance.
Embodiment 3
(1) calculate by atom ratio and weigh high-purity Al powder, Pd powder, Mn powder raw materials, its weight be respectively 0.9826g,
1.1626g, 0.2001g are (according to Al70Pd21Mn7Weigh), above-mentioned powder is positioned in mortar to be fully ground to be well mixed it is loaded on
During internal diameter is for the sintered-carbide die of Φ 10.6mm, the 100s when 3Mpa that pressurizes in hydraulic pressure tablet press machine is obtains diameter of phi
The simple and mechanical pressing high pressure preparation block of 10.6mm thickness 7.6mm.
(2) graphite furnace is high 16.6mm external diameters Φ 14mm internal diameters Φ 12.1mm tubulose bodies of heater, and two ends are thick with Φ 12.06mm
3.3mm pyrophillites piece is sealed, and is set with boron nitride crucible in graphite furnace, the high 10mm external diameters Φ 12mm internal diameters Φ 10.8mm of crucible, and two
End is sealed with diameter of phi 10.75mm thickness 1.2mm boron nitride piece, while graphite furnace two ends parcel and conduction graphite flake specification are straight
The thickness 1.6mm of footpath Φ 14.By above-mentioned tubular graphene body of heater, boron nitride crucible, boron nitride piece, pyrophillite piece and stone for testing
The pyrophillite square and Conducting steel bowl that ink sheet is used together with cubic hinge press is put in the drying baker that temperature is 200 DEG C dries 2
It is standby more than hour.
(3) preparation block will be fitted in boron nitride crucible and by the tubular graphene of step (2) prebake obtained in step (1)
Body of heater, boron nitride crucible, boron nitride piece, pyrophillite piece and graphite flake assembling, in being positioned over cubic hinge press, set pressure as
6GPa isostatic presseds；Temperature is heated to 850 DEG C, is incubated 45min；Treat that temperature is down to 850 DEG C, be incubated 4h.
(4) directly turn-off current stops heating after insulation terminates.
(5) block is taken out, BN is remained outside careful peel sample, clean surface obtains Al70Pd21Mn7Quasi-crystalline substance.
As shown in fig. 7, from figure the geometric shape of rule may determine that synthesis for quasi-crystalline substance sample.
Claims (2)
1. a kind of preparation method of Al-Pd-Mn quasi-crystalline substances, it is characterised in that：
(1) atom ratio of the chemical composition of Al-Pd-Mn quasi-crystalline substances is：Al 70-72%, Pd 18-21%, Mn 7-12%；
(2) high-purity Al powder, Pd powder, Mn powder is fully ground after being well mixed and is fitted in sintered-carbide die, in hydraulic pressure compressing tablet
Pressurize 100-300s in machine under 2-4MPa, and preparation block is obtained；
(3) graphite furnace tubulose body of heater two ends are sealed with pyrophillite piece, boron nitride crucible, crucible two ends nitrogen is set with graphite furnace
Change the sealing of boron piece, while graphite furnace two ends graphite flake is used as parcel and conduction, then by above described tubular graphite body of heater, boron nitride
The pyrophillite square and Conducting steel bowl that crucible, boron nitride piece, pyrophillite piece and graphite flake are used together with cubic hinge press is put
It is standby 2-4 hours to be dried in temperature is for 100-200 DEG C of drying baker；
(4) the prepared block of step (2) is fitted in boron nitride crucible and by tubular graphene body of heater, the nitrogen of step (3) prebake
Change the assembling of boron crucible, boron nitride piece, pyrophillite piece and graphite flake, in being positioned over cubic hinge press, setting Stress control is in 3-
6GPa isostatic presseds, control temperature is heated between 850 DEG C -950 DEG C, is incubated 30-60min；Treat that temperature is down to 650-850 DEG C, protect
Warm 2-6h.
2. the preparation method of Al-Pd-Mn quasi-crystalline substances according to claim 1, it is characterised in that：The chemistry of Al-Pd-Mn quasi-crystalline substances
Component atoms proportioning is：Al 71%, Pd 20%, Mn 9%.
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| CN108913926B (en) * | 2018-06-13 | 2021-05-18 | 燕山大学 | Method for preparing Al-Pd-Fe two-dimensional quasicrystal particles |
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