CN105568072A - Preparation method for Al-Pd-Mn quasicrystal - Google Patents

Preparation method for Al-Pd-Mn quasicrystal Download PDF

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CN105568072A
CN105568072A CN201610008752.1A CN201610008752A CN105568072A CN 105568072 A CN105568072 A CN 105568072A CN 201610008752 A CN201610008752 A CN 201610008752A CN 105568072 A CN105568072 A CN 105568072A
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boron nitride
powder
sheet
graphite
preparation
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CN105568072B (en
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范长增
何璞
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Yanshan University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium

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  • Engineering & Computer Science (AREA)
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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

The accurate brilliant preparation method of a kind of Al-Pd-Mn
Technical field
The invention belongs to technical field of metal, a kind of especially accurate brilliant preparation method.
Background technology
Found a kind of peculiar phase-icosahedral phase with metalline in the Al-Mn binary alloy of the Israel scientist D.Shechtman worked in National Bureau of Standards for 1984 at rapid solidification, this is a kind of new crystallographic structure.The electron diffraction spot of this cenotype is quite bright and sharp, and demonstrates unallowed five rotational symmetries of crystalline structure, therefore cannot go to demarcate with any one Bravais lattice.This cenotype is a kind of solid-state ordered phase with long-range translational order quasi-periodicity and non-crystallographic rotational symmetry, is referred to as Icosahedral phases very soon.Accurate brilliant special structure causes people's keen interest, and it is accurate brilliant to impel investigator to find in related system.Initial several years, research system mainly concentrated on binary system and finds that these accurate crystalline substances are all metastable phases very soon.Very fast research system expands to ternary system, and has found some stable Icosahedral phases, and wherein Al-Pd-Mn is exactly one of typical system.At first, icosahedron Al-Pd-Mn system Icosahedral phases melts quenching device (singlerollermeltspinningapparatus) flash set technology realization (abbreviation gets rid of band method) by single roller.Up to now, the additive method obtaining Al-Pd-Mn system Icosahedral phases has: crystal pulling method (Czochralskimethod), Bridgman method (Bridgmanmethod), self-service flux method (self-fluxmethod) and float-zone method (Floatingzonemethod).Not fine and close by the quasicrystal getting rid of the acquisition of band method, easily there is the defects such as hole.Rear several method can obtain high-quality monocrystalline, but needs extremely strict sample pretreatment and accurately will control acid extraction etc.
Summary of the invention
The object of the invention is to provide the accurate brilliant preparation method of the Al-Pd-Mn that a kind of technique is simple, efficient, Icosahedral phases content is high.It is accurate brilliant that the present invention mainly adopts high-pressure process to prepare Al-Pd-Mn, directly pressure is acted on Homogeneous phase mixing and on Al, Pd, Mn mixing raw material being in heating and melting state, according to design temperature, pressure, reaction duration start six-plane piercer can directly obtain single-phase, containing the accurate crystal block body of large size crystal grain.
Technical scheme of the present invention is as follows:
(1) atom ratio of the accurate brilliant chemical composition of Al-Pd-Mn is: Al70-72%, Pd18-21%, Mn7-12%, and described Al, Pd, Mn are high pure metal powder; Be optimized and be divided into Al 71pd 20mn 9.
(2) high-purity Al powder, Pd powder, the abundant ground and mixed of Mn powder are evenly loaded in sintered-carbide die afterwards, pressurize under 2-4MPa 100-300s in hydraulic pressure tabletting machine, obtained preparation block;
(3) graphite furnace tubulose body of heater two ends agalmatolite sheet is sealed, boron nitride crucible is set with in graphite furnace, crucible two ends boron nitride sheet seals, simultaneously graphite furnace two ends graphite flake is as parcel and conduction, the agalmatolite square then above described tubular graphite body of heater, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake used together with six-plane piercer and Conducting steel bowl be put in the drying baker that temperature is 100-200 DEG C dry more than 2-4 hour for subsequent use.
(4) the preparation block of step (2) to be loaded in boron nitride crucible and the tubular graphene body of heater of step (3) prebake, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake are assembled, be positioned in six-plane piercer, setting pressure controls at 3-6GPa isostatic pressed, control temperature is heated between 850 DEG C-950 DEG C, insulation 30-60min; Treat that temperature is down to 650-850 DEG C, insulation 2-6h.
The present invention compared with prior art tool has the following advantages:
1, technique is simple, energy consumption is low, efficiency is high, settles at one go, only need adopt conventional high-pressure equipment from raw material to accurate crystalline substance.
2, obtained Icosahedral phases content is high, superior in quality.
Figure of description
Fig. 1 is obtained accurate brilliant XRD figure by the embodiment of the present invention 1.
Fig. 2 is Al in the embodiment of the present invention 1 71pd 20mn 9accurate brilliant 2 heavy symmetry axis direction diffraction pattern figure.
Fig. 3 is Al in the embodiment of the present invention 1 71pd 20mn 9accurate brilliant 3 heavy symmetry axis direction diffraction pattern figure.
Fig. 4 is Al in the embodiment of the present invention 1 71pd 20mn 9accurate brilliant 5 heavy symmetry axis direction diffraction pattern figure.
Fig. 5 obtains by the embodiment of the present invention 2 High-Resolution Map of accurate brilliant TEM.
Fig. 6 is schemed by the embodiment of the present invention 2 obtains accurate brilliant SEM.
Fig. 7 is schemed by the embodiment of the present invention 3 obtains accurate brilliant SEM.
Embodiment
Embodiment 1
(1) take high-purity Al powder, Pd powder, Mn powder raw material by atom ratio calculating, its weight is respectively 1.0076g, 1.1194g, 0.2601g (according to Al 71pd 20mn 9take), above-mentioned powder being positioned in mortar that abundant ground and mixed is evenly loaded on internal diameter is in the sintered-carbide die of Φ 10.6mm, and 120s when the 4Mpa that pressurizes in hydraulic pressure tabletting machine is, obtains the simple and mechanical pressing high pressure preparation block of diameter of phi 10.6mm thickness 7.6mm.
(2) graphite furnace is high 16.6mm external diameter Φ 14mm internal diameter Φ 12.1mm tubulose body of heater, two ends Φ 12.06mm thick 3.3mm agalmatolite sheet seals, boron nitride crucible is set with in graphite furnace, crucible height 10mm external diameter Φ 12mm internal diameter Φ 10.8mm, two ends diameter of phi 10.75mm thick 1.2mm boron nitride sheet seals, and graphite furnace two ends parcel and conduction graphite flake specification are the thick 1.6mm of diameter of phi 14 simultaneously.The agalmatolite square that above described tubular graphite body of heater, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake are used together with six-plane piercer and Conducting steel bowl be put in temperature be dry in the drying baker of 180 DEG C more than 3 hours for subsequent use.
(3) preparation block obtained for step (1) to be loaded in boron nitride crucible and the tubular graphene body of heater of step (2) prebake, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake are assembled, be positioned in six-plane piercer, setting pressure is 5GPa isostatic pressed; Heating temperatures to 900 DEG C, insulation 30min; Treat that temperature is down to 750 DEG C, insulation 2h.
(4) insulation terminates rear direct turn-off current and stops heating.
(5) take out block, careful peel sample is residual BN outward, and clean surface obtains Al 71pd 20mn 9accurate brilliant.
Aim at brilliant in row XRD sweep test, determine composition, as shown in Figure 1, obvious Al can be seen 71pd 20mn 9diffraction peak, and it is leading to judge that Icosahedral phases accounts for.
Be as the criterion 2 brilliant heavy symmetry axis direction diffraction spots as shown in Figure 2; Accurate 3 brilliant heavy symmetry axis direction diffraction spots as shown in Figure 3; Accurate 5 brilliant heavy symmetry axis direction diffraction spots as shown in Figure 4.Can prove that the electron diffraction of crystal grain has icosahedron symmetry by Fig. 2-4, crystal grain is icosahedral quasicrystal.
The Atomic Arrangement that the brilliant five heavy symmetry directions that are as the criterion as shown in Figure 5 are observed, from the real space, this confirms that observed crystal grain is quasicrystal particle.
As shown in Figure 6, be the particle growth pattern observed under SEM scanning electron microscope, regular geometric shape particularly pentagonal profile gives the dynamic information of quasicrystal particle growth.
Embodiment 2
(1) take high-purity Al powder, Pd powder, Mn powder raw material by atom ratio calculating, its weight is respectively 1.0700g, 1.0551g, 0.3631g (according to Al 72pd 18mn 12take), above-mentioned powder being positioned in mortar that abundant ground and mixed is evenly loaded on internal diameter is in the sintered-carbide die of Φ 10.6mm, the 300s when 2Mpa that pressurizes in hydraulic pressure tabletting machine is, obtains the simple and mechanical pressing high pressure preparation block of diameter of phi 10.6mm thickness 7.6mm.
(2) graphite furnace is high 16.6mm external diameter Φ 14mm internal diameter Φ 12.1mm tubulose body of heater, two ends Φ 12.06mm thick 3.3mm agalmatolite sheet seals, boron nitride crucible is set with in graphite furnace, crucible height 10mm external diameter Φ 12mm internal diameter Φ 10.8mm, two ends diameter of phi 10.75mm thick 1.2mm boron nitride sheet seals, and graphite furnace two ends parcel and conduction graphite flake specification are the thick 1.6mm of diameter of phi 14 simultaneously.The agalmatolite square that above-mentioned tubular graphene body of heater, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake for testing is used together with six-plane piercer and Conducting steel bowl be put in temperature be dry in the drying baker of 100 DEG C more than 4 hours for subsequent use.
(3) preparation block obtained for step (1) to be loaded in boron nitride crucible and the tubular graphene body of heater of step (2) prebake, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake are assembled, be positioned in six-plane piercer, setting pressure is 3GPa isostatic pressed; Heating temperatures to 950 DEG C, insulation 60min; Treat that temperature is down to 650 DEG C, insulation 6h.
(4) insulation terminates rear direct turn-off current and stops heating.
(5) take out block, careful peel sample is residual BN outward, and clean surface obtains Al 72pd 18mn 12accurate brilliant.
As shown in Figure 5, can find out that obvious five is heavy symmetrical, therefore can determine to have synthesized Icosahedral phases.As shown in Figure 6, in figure, the geometric shape of rule also can judge the crystalline substance that is as the criterion synthesized.
Embodiment 3
(1) take high-purity Al powder, Pd powder, Mn powder raw material by atom ratio calculating, its weight is respectively 0.9826g, 1.1626g, 0.2001g (according to Al 70pd 21mn 7take), above-mentioned powder being positioned in mortar that abundant ground and mixed is evenly loaded on internal diameter is in the sintered-carbide die of Φ 10.6mm, the 100s when 3Mpa that pressurizes in hydraulic pressure tabletting machine is, obtains the simple and mechanical pressing high pressure preparation block of diameter of phi 10.6mm thickness 7.6mm.
(2) graphite furnace is high 16.6mm external diameter Φ 14mm internal diameter Φ 12.1mm tubulose body of heater, two ends Φ 12.06mm thick 3.3mm agalmatolite sheet seals, boron nitride crucible is set with in graphite furnace, crucible height 10mm external diameter Φ 12mm internal diameter Φ 10.8mm, two ends diameter of phi 10.75mm thick 1.2mm boron nitride sheet seals, and graphite furnace two ends parcel and conduction graphite flake specification are the thick 1.6mm of diameter of phi 14 simultaneously.The agalmatolite square that above-mentioned tubular graphene body of heater, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake for testing is used together with six-plane piercer and Conducting steel bowl be put in temperature be dry in the drying baker of 200 DEG C more than 2 hours for subsequent use.
(3) preparation block obtained for step (1) to be loaded in boron nitride crucible and the tubular graphene body of heater of step (2) prebake, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake are assembled, be positioned in six-plane piercer, setting pressure is 6GPa isostatic pressed; Heating temperatures to 850 DEG C, insulation 45min; Treat that temperature is down to 850 DEG C, insulation 4h.
(4) insulation terminates rear direct turn-off current and stops heating.
(5) take out block, careful peel sample is residual BN outward, and clean surface obtains Al 70pd 21mn 7accurate brilliant.
As shown in Figure 7, from figure, the geometric shape of rule can judge the brilliant sample that is as the criterion synthesized.

Claims (3)

1. the accurate brilliant preparation method of Al-Pd-Mn, is characterized in that:
(1) atom ratio of the accurate brilliant chemical composition of Al-Pd-Mn is: Al70-72%, Pd18-21%, Mn7-12%;
(2) high-purity Al powder, Pd powder, the abundant ground and mixed of Mn powder are evenly loaded in sintered-carbide die afterwards, pressurize under 2-4MPa 100-300s in hydraulic pressure tabletting machine, obtained preparation block;
(3) graphite furnace tubulose body of heater two ends agalmatolite sheet is sealed, boron nitride crucible is set with in graphite furnace, crucible two ends boron nitride sheet seals, simultaneously graphite furnace two ends graphite flake is as parcel and conduction, the agalmatolite square then above described tubular graphite body of heater, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake used together with six-plane piercer and Conducting steel bowl be put in the drying baker that temperature is 100-200 DEG C dry more than 2-4 hour for subsequent use;
(4) the preparation block of step (2) to be loaded in boron nitride crucible and the tubular graphene body of heater of step (3) prebake, boron nitride crucible, boron nitride sheet, agalmatolite sheet and graphite flake are assembled, be positioned in six-plane piercer, setting pressure controls at 3-6GPa isostatic pressed, control temperature is heated between 850 DEG C-950 DEG C, insulation 30-60min; Treat that temperature is down to 650-850 DEG C, insulation 2-6h.
2. the accurate brilliant preparation method of Al-Pd-Mn according to claim 1, is characterized in that: Al-Pd-Mn is accurate, and brilliant chemical composition atom ratio is: Al71%, Pd20%, Mn9%.
3. the accurate brilliant preparation method of Al-Pd-Mn according to claim 1 and 2, is characterized in that: described Al, Pd, Mn are high pure metal powder.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107338471A (en) * 2017-07-27 2017-11-10 燕山大学 A kind of preparation method of high pressure metastable phase Al21Pd8 single crystal grains
CN108913926A (en) * 2018-06-13 2018-11-30 燕山大学 A method of preparing Al-Pd-Fe two dimensional quasicrystal particle
CN109226767A (en) * 2018-07-27 2019-01-18 常州大学 Prepare the high pressure high temperature synthetic method of second phase particles simulation material in aluminium alloy

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07238336A (en) * 1994-02-25 1995-09-12 Takeshi Masumoto High strength aluminum-base alloy
JPH09260125A (en) * 1996-03-26 1997-10-03 Akihisa Inoue Magnetic material
CN102641890B (en) * 2012-04-28 2014-04-02 中南大学 Preparation method of powder metallurgy superfine crystal titanium aluminum base alloy panel

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07238336A (en) * 1994-02-25 1995-09-12 Takeshi Masumoto High strength aluminum-base alloy
JPH09260125A (en) * 1996-03-26 1997-10-03 Akihisa Inoue Magnetic material
CN102641890B (en) * 2012-04-28 2014-04-02 中南大学 Preparation method of powder metallurgy superfine crystal titanium aluminum base alloy panel

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107338471A (en) * 2017-07-27 2017-11-10 燕山大学 A kind of preparation method of high pressure metastable phase Al21Pd8 single crystal grains
CN107338471B (en) * 2017-07-27 2019-10-15 燕山大学 A kind of preparation method of high pressure metastable phase Al21Pd8 single crystal grain
CN108913926A (en) * 2018-06-13 2018-11-30 燕山大学 A method of preparing Al-Pd-Fe two dimensional quasicrystal particle
CN109226767A (en) * 2018-07-27 2019-01-18 常州大学 Prepare the high pressure high temperature synthetic method of second phase particles simulation material in aluminium alloy

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