CN108913926B - Method for preparing Al-Pd-Fe two-dimensional quasicrystal particles - Google Patents

Method for preparing Al-Pd-Fe two-dimensional quasicrystal particles Download PDF

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CN108913926B
CN108913926B CN201810607925.0A CN201810607925A CN108913926B CN 108913926 B CN108913926 B CN 108913926B CN 201810607925 A CN201810607925 A CN 201810607925A CN 108913926 B CN108913926 B CN 108913926B
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carbon paper
powder
cushion block
pressure
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CN108913926A (en
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范长增
李豪
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Yanshan University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • C22C1/0416Aluminium-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0466Alloys based on noble metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/04Alloys based on a platinum group metal
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C2200/00Crystalline structure
    • C22C2200/06Quasicrystalline

Abstract

A method for preparing Al-Pd-Fe two-dimensional quasicrystal particles comprises the following chemical components in atomic ratio: 70-75% of Al, 10-25% of Pd and 5-15% of Fe, fully and uniformly mixing high-purity Al powder, Pd powder and Fe powder by using a mortar, uniformly distributing the uniformly mixed metal powder in a graphite grinding tool cavity, prepressing on a mould tablet press, keeping the pressure at 1-2MPa for 60-100s, wrapping a layer of carbon felt outside a graphite crucible, then placing the carbon paper, a large graphite cushion block, carbon paper, a small graphite cushion block, the prepared graphite crucible, a small graphite cushion block, the carbon paper, a large graphite cushion block and the carbon paper in a pressing cavity of the SPS in sequence and pressing, wherein the sintering pressure is 50MPa, heating to 1000-inch 1100 ℃, keeping the temperature for 10-20min, and then cooling to room temperature along with a furnace. The method has the advantages of simple process, strong operability, conventional equipment and less time consumption, and can directly use the mixed raw materials to synthesize the two-dimensional quasicrystal phase by reducing the treatment of the raw materials.

Description

Method for preparing Al-Pd-Fe two-dimensional quasicrystal particles
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to preparation of quasicrystal particles.
Background
The Al-Pd-TM (TM is transition metal element) series quasicrystal phase has high hardness, low friction coefficient and strong brittleness, and the main research on the application of the quasicrystal phase at present is as a reinforcing phase of an Al-based composite material. It was found that the phase structure of the Al-Pd-TM alloy remains unchanged even in the fully annealed state in the quasicrystal phase formed in the rapidly solidified Al-Pd-TM alloy, indicating that the Al-Pd-TM series quasicrystal has a stable structure. In previous experimental studies, researchers have conducted arc melting of appropriate amounts of high purity Al, Pd, Fe and quenched them to room temperature in an argon atmosphere, or rapidly quenched them by melt rotation using a high speed rotating copper roll, and separated two-dimensional quasicrystal samples by X-ray diffraction measurement of the pulverized samples or confirmed the diffraction pattern of very small samples by transmission electron microscopy. The preparation cost of the prior experimental quasicrystal material is high, the process is complex, the operation requirement is high, and more equipment is needed.
Disclosure of Invention
The invention aims to provide a method for preparing Al-Pd-Fe two-dimensional quasicrystal particles, which has the advantages of simple process, strong operability, use of conventional equipment and low time consumption.
The invention mainly utilizes an SPS sintering system to directly sinter mixed metal powder, fully and uniformly mixes pure Al powder, Pd powder and Fe powder, then prepresses and prepares a sample, and then directly prepares an alloy block after the SPS sintering system heats, pressurizes and cools.
The technical scheme of the invention is as follows:
(1) the Al-Pd-Fe two-dimensional quasicrystal particle comprises the following chemical components in atomic ratio: 70-75% of Al, 10-25% of Pd and 5-15% of Fe; al, Pd and Fe are high-purity metal powder;
(2) fully and uniformly mixing high-purity Al powder, Pd powder and Fe powder by using a mortar, placing carbon paper on the inner side and the bottom of a graphite cavity prepared in advance, pouring the uniformly mixed metal powder into a graphite crucible for tamping, placing the carbon paper on the top end, placing a small pressure head, and rotating the small pressure head back and forth to uniformly distribute the powder in the graphite grinding cavity, finally performing prepressing on a die tablet press, and slightly lifting a pressure gauge pointer of the tablet press by 1-2MPa for keeping 60-100 s;
(3) because the sintering temperature is higher than 1000 ℃, a layer of carbon felt is wrapped outside the graphite crucible, a square opening is formed in the position of the temperature measuring hole of the mold when the carbon felt is wrapped, the temperature measuring hole of the mold is exposed, the vacuum meter is closed, the air release valve is opened, after the vacuum conversion indicator lamp is turned on, the air release valve is closed, the cavity is opened, and the pressure knob is adjusted to 16.5 MPa;
(4) preparing a large graphite cushion block and a small graphite cushion block according to the following steps: the carbon paper, the large graphite cushion block, the carbon paper, the small graphite cushion block, the prepared graphite crucible, the small graphite cushion block, the carbon paper, the large graphite cushion block and the carbon paper are sequentially placed in a pressure cavity of the SPS sintering system, and the graphite cushion block and the mold are tightly pressed by an upper pressure head and a lower pressure head.
(5) After confirming that the deflation valve is in a closed state, adjusting the sintering pressure to be 50MPa, opening the vacuum meter and the mechanical pump, when the vacuum degree of the cavity is lower than 4Pa, heating to 1000-1100 ℃ at the heating rate of 50-100 ℃/min, preserving the temperature for 10-20min, cooling the sample to room temperature along with the furnace, and taking out the block to directly obtain the block containing the two-dimensional quasicrystal particles.
Compared with the prior art, the invention has the following advantages:
the method has the advantages of simple process operation, strong operability, conventional equipment and less time consumption, simultaneously reduces the treatment of raw materials, can directly use the mixed raw materials to synthesize the two-dimensional quasicrystal phase, is an efficient one-step synthesis method, can quickly and accurately select the quasicrystal by matching with a single crystal X-ray diffractometer and related software, and provides support for further structure analysis.
Drawings
FIG. 1 shows Al obtained in example 1 of the present invention75Pd15Fe10And (3) a crystal grain morphology graph under a quasi-crystal grain polarization microscope.
FIG. 2 shows Al obtained in example 1 of the present invention75Pd15Fe10And (3) a reciprocal space lattice diagram of quasicrystalline particles.
FIG. 3 shows Al obtained in example 2 of the present invention70Pd25Fe5And (3) a crystal grain morphology graph under a quasi-crystal grain polarization microscope.
FIG. 4 shows Al obtained in example 2 of the present invention70Pd25Fe5And (3) a reciprocal space lattice diagram of quasicrystalline particles.
FIG. 5 shows Al obtained in example 3 of the present invention75Pd10Fe15And (3) a crystal grain morphology graph under a quasi-crystal grain polarization microscope.
FIG. 6 shows Al obtained in example 3 of the present invention75Pd10Fe15And (3) a reciprocal space lattice diagram of quasicrystalline particles.
Detailed Description
Example 1
(1) Weighing high-purity Al powder, Pd powder and Fe powder raw materials according to the atomic ratio, wherein the weight of the raw materials is 0.9701g, 0.7617g and 0.2683g (according to the weight of Al75Pd15Fe10Weighing), placing the powder into a mortar, fully grinding and uniformly mixing the powder, placing the powder into a graphite crucible with the inner diameter of phi 20mm, and pressurizing the graphite crucible in a hydraulic tablet press for 100s under the pressure of 1MPa to obtain a sheet prepressing sample with the diameter of phi 20 mm;
(2) the graphite crucible is a tubular furnace body with the height of 40mm, the outer diameter phi of 50mm and the inner diameter phi of 20mm, two ends of the tubular furnace body are sealed by graphite plugs with the thickness of 20mm, the carbon paper is sleeved in the graphite furnace, the carbon paper is 63mm long and 40mm wide and is rolled into a barrel shape to be sleeved on the inner side of the graphite furnace, two ends of the tubular furnace body are respectively separated from the graphite plugs by the carbon paper with the diameter phi of 20mm, and the sample is prevented from reacting with the graphite furnace under high temperature and high. Because the sintering temperature is higher than 1000 ℃, a layer of carbon felt is wrapped outside the graphite mould, and a square opening is formed at the position of the temperature measuring hole of the mould to expose the temperature measuring hole of the mould when the carbon felt is wrapped. Closing the vacuum meter and opening the air release valve, closing the air release valve to open the cavity after the vacuum conversion indicator lamp is turned on, and adjusting the pressure knob to 16.5 MPa;
(3) preparing a large graphite gasket and a small graphite gasket according to the following steps: sequentially placing carbon paper, a large graphite cushion block, carbon paper, a small graphite cushion block, a prepared graphite mold, a small graphite cushion block, carbon paper, a large graphite cushion block and carbon paper in a pressure cavity of an SPS sintering system, and tightly pressing the graphite cushion block and the mold by using an upper pressing head and a lower pressing head;
(4) and after confirming that the air release valve is in a closed state, adjusting the sintering pressure to be 50MPa, opening the vacuum meter and the mechanical pump, when the vacuum degree of the cavity is lower than 4Pa, heating to 1100 ℃ at the heating rate of 100 ℃/min, preserving the temperature for 10min, cooling the sample to room temperature along with the furnace, and taking out the block to directly obtain the block containing the two-dimensional quasicrystal particles.
The morphology of the crystal particles in the sample was observed under a polarizing microscope, as shown in FIG. 1.
And carrying out single crystal X-ray diffraction experiments on the selected crystal particles, and converting the crystal particles into reciprocal space lattices. As shown in fig. 2, the diffraction points can determine that the crystal particles are two-dimensional quasicrystal particles, and the crystal particles are relatively complete quasicrystal phases.
Example 2
(1) Weighing high-purity Al powder, Pd powder and Fe powder raw materials according to the atomic ratio, wherein the weight of the raw materials is 0.7820g, 1.1018g and 0.1157g (according to the weight of Al70Pd25Fe5Weighing), placing the powder into a mortar, fully grinding and uniformly mixing the powder, placing the powder into a graphite crucible with the inner diameter of phi 20mm, and pressurizing the graphite crucible for 80s under the condition of 1.5Mpa in a hydraulic tablet press to obtain a sheet prepressing sample with the diameter of phi 20 mm;
(2) the graphite crucible is a tubular furnace body with the height of 40mm, the outer diameter phi of 50mm and the inner diameter phi of 20mm, two ends of the tubular furnace body are sealed by graphite plugs with the thickness of 20mm, the carbon paper is sleeved in the graphite furnace, the carbon paper is 63mm long and 40mm wide and is rolled into a barrel shape to be sleeved on the inner side of the graphite furnace, two ends of the tubular furnace body are respectively separated from the graphite plugs by the carbon paper with the diameter phi of 20mm, and the sample is prevented from reacting with the graphite furnace under high temperature and high. Because the sintering temperature is higher than 1000 ℃, a layer of carbon felt is wrapped outside the graphite mould, and a square opening is formed at the position of the temperature measuring hole of the mould to expose the temperature measuring hole of the mould when the carbon felt is wrapped. Closing the vacuum meter and opening the air release valve, closing the air release valve to open the cavity after the vacuum conversion indicator lamp is turned on, and adjusting the pressure knob to 16.5 MPa;
(3) preparing a large graphite gasket and a small graphite gasket according to the following steps: sequentially placing carbon paper, a large graphite cushion block, carbon paper, a small graphite cushion block, a prepared graphite mold, a small graphite cushion block, carbon paper, a large graphite cushion block and carbon paper in a pressure cavity of an SPS sintering system, and tightly pressing the graphite cushion block and the mold by using an upper pressing head and a lower pressing head;
(4) and after confirming that the air release valve is in a closed state, adjusting the sintering pressure to be 50MPa, opening a vacuum meter and a mechanical pump, when the vacuum degree of a cavity is lower than 4Pa, heating to 1000 ℃ at the heating rate of 75 ℃/min, preserving the temperature for 15min, cooling the sample to room temperature along with the furnace, and taking out the block to directly obtain the block containing the two-dimensional quasicrystal particles.
The morphology of the crystal particles in the sample was observed under a polarizing microscope, as shown in FIG. 3.
And carrying out single crystal X-ray diffraction experiments on the selected crystal particles, and converting the crystal particles into reciprocal space lattices. As shown in fig. 4, the diffraction points can determine that the crystal particles are two-dimensional quasicrystal particles, and the crystal particles are relatively complete quasicrystal phases.
Example 3
(1) Weighing high-purity Al powder, Pd powder and Fe powder raw materials according to the atomic ratio, wherein the weight of the raw materials is 1.0310g, 0.5422g and 0.4268g (according to the weight of Al75Pd10Fe15Weighing), placing the powder into a mortar, fully grinding and uniformly mixing the powder, placing the powder into a graphite crucible with the inner diameter of phi 20mm, and pressurizing the graphite crucible in a hydraulic tablet press for 60s under 2Mpa to obtain a sheet prepressing sample with the diameter of phi 20 mm;
(2) the graphite crucible is a tubular furnace body with the height of 40mm, the outer diameter phi of 50mm and the inner diameter phi of 20mm, two ends of the tubular furnace body are sealed by graphite plugs with the thickness of 20mm, the carbon paper is sleeved in the graphite furnace, the carbon paper is 63mm long and 40mm wide and is rolled into a barrel shape to be sleeved on the inner side of the graphite furnace, two ends of the tubular furnace body are respectively separated from the graphite plugs by the carbon paper with the diameter phi of 20mm, and the sample is prevented from reacting with the graphite furnace under high temperature and high. Because the sintering temperature is higher than 1000 ℃, a layer of carbon felt is wrapped outside the graphite mould, and a square opening is formed at the position of the temperature measuring hole of the mould to expose the temperature measuring hole of the mould when the carbon felt is wrapped. Closing the vacuum meter and opening the air release valve, closing the air release valve to open the cavity after the vacuum conversion indicator lamp is turned on, and adjusting the pressure knob to 16.5 MPa;
(3) preparing a large graphite gasket and a small graphite gasket according to the following steps: sequentially placing carbon paper, a large graphite cushion block, carbon paper, a small graphite cushion block, a prepared graphite mold, a small graphite cushion block, carbon paper, a large graphite cushion block and carbon paper in a pressure cavity of an SPS sintering system, and tightly pressing the graphite cushion block and the mold by using an upper pressing head and a lower pressing head;
(4) and after confirming that the air release valve is in a closed state, adjusting the sintering pressure to be 50MPa, opening a vacuum meter and a mechanical pump, when the vacuum degree of a cavity is lower than 4Pa, heating to 1050 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 20min, cooling the sample to room temperature along with the furnace, and taking out the block to directly obtain the block containing the two-dimensional quasicrystal particles.
The morphology of the crystal particles in the sample was observed under a polarizing microscope, as shown in FIG. 5.
And carrying out single crystal X-ray diffraction experiments on the selected crystal particles, and converting the crystal particles into reciprocal space lattices. As shown in fig. 6, it can be determined from the diffraction points that the crystal particles are two-dimensional quasicrystal particles, and the crystal particles are relatively intact quasicrystal phases.

Claims (1)

1. A method for preparing Al-Pd-Fe two-dimensional quasicrystal particles is characterized by comprising the following steps:
(1) the Al-Pd-Fe two-dimensional quasicrystal particle comprises the following chemical components in atomic ratio: 70-75% of Al, 10-25% of Pd and 5-15% of Fe; al, Pd and Fe are high-purity metal powder;
(2) fully and uniformly mixing high-purity Al powder, Pd powder and Fe powder by using a mortar, placing carbon paper on the inner side and the bottom of a prepared graphite crucible cavity, pouring the uniformly mixed metal powder into the graphite crucible for compaction, placing the carbon paper on the top end, placing a small pressure head, and rotating the small pressure head back and forth to uniformly distribute the powder in the graphite crucible cavity, finally performing prepressing on a die tablet press, and slightly lifting a pressure gauge pointer of the tablet press to 1-2MPa to keep the pressure for 60-100 s;
(3) because the sintering temperature is higher than 1000 ℃, a layer of carbon felt is wrapped outside the graphite crucible, a square opening is formed in the position of the temperature measuring hole of the mold when the carbon felt is wrapped, the temperature measuring hole of the mold is exposed, the vacuum meter is closed, the air release valve is opened, after the vacuum conversion indicator lamp is turned on, the air release valve is closed, the cavity is opened, and the pressure knob is adjusted to 16.5 MPa;
(4) preparing a large graphite gasket and a small graphite gasket according to the following steps: placing carbon paper, a large graphite cushion block, carbon paper, a small graphite cushion block, a prepared graphite crucible, a small graphite cushion block, carbon paper, a large graphite cushion block and carbon paper in a pressure cavity of an SPS sintering system in sequence, and tightly pressing the graphite cushion block and the graphite crucible by using an upper pressure head and a lower pressure head;
(5) after confirming that the deflation valve is in a closed state, adjusting the sintering pressure to be 50MPa, opening the vacuum meter and the mechanical pump, when the vacuum degree of the cavity is lower than 4Pa, heating to 1000-1100 ℃ at the heating rate of 50-100 ℃/min, preserving the temperature for 10-20min, cooling the sample to room temperature along with the furnace, and taking out the block to directly obtain the block containing the two-dimensional quasicrystal particles.
CN201810607925.0A 2018-06-13 2018-06-13 Method for preparing Al-Pd-Fe two-dimensional quasicrystal particles Active CN108913926B (en)

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CN103938014A (en) * 2014-04-28 2014-07-23 大连理工大学 Nano-porous Pd material prepared through quasi-crystal de-alloying and preparation process of nano-porous Pd material
CN105648298B (en) * 2016-01-07 2017-08-04 燕山大学 A kind of preparation method with dodecahedron profile Al Cu Fe quasi-crystalline substance blocks
CN105568072B (en) * 2016-01-07 2017-04-26 燕山大学 Preparation method for Al-Pd-Mn quasicrystal
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